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Research Article Microencapsulation of -Carotene by Spray Drying: Effect of Wall Material Concentration and Drying Inlet Temperature Luiz C. Corrêa-Filho , Maria M. Lourenço, Margarida Moldão-Martins , and V-tor D. Alves LEAF, Linking Landscape, Environment, Agriculture and Food, Instituto Superior de Agronomia, Universidade de Lisboa, Tapada da Ajuda, 1349-017 Lisboa, Portugal Correspondence should be addressed to Margarida Mold˜ ao-Martins; [email protected] Received 18 August 2018; Revised 24 December 2018; Accepted 3 January 2019; Published 22 January 2019 Academic Editor: Amy Simonne Copyright © 2019 Luiz C. Corrˆ ea-Filho et al. is is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. Carotenoids are a class of natural pigments found mainly in fruits and vegetables. Among them, -carotene is regarded the most potent precursor of vitamin A. However, it is susceptible to oxidation upon exposure to oxygen, light, and heat, which can result in loss of colour, antioxidant activity, and vitamin activity. us, the objective of this work was to study the microencapsulation process of -carotene by spray drying, using arabic gum as wall material, to protect it against adverse environmental conditions. is was carried out using the response surface methodology coupled to a central composite rotatable design, evaluating simultaneously the effect of drying air inlet temperature (110-200 C) and the wall material concentration (5-35%) on the drying yield, encapsulation efficiency, loading capacity, and antioxidant activity. In addition, morphology and particles size distribution were evaluated. Scanning electron microscopy images have shown that the particles were microcapsules with a smooth surface when produced at the higher drying temperatures tested, most of them having a diameter lower than 10 m. e conditions that enabled obtaining simultaneously arabic gum microparticles with higher -carotene content, higher encapsulation efficiency, and higher drying yield were a wall material concentration of 11.9% and a drying inlet temperature of 173 C. e systematic approach used for the study of -carotene microencapsulation process by spray drying using arabic gum may be easily applied for other core and wall materials. 1. Introduction Carotenoids, which are synthesized by fruits and vegeta- bles, are a family of hydrophobic pigmented compounds that structurally exist as hydrocarbons (carotenes) or their oxygenated derivatives (xanthophylls). ey are natural com- pounds responsible for yellow, orange, and red colours in many foods [1–3]. More than 700 different carotenoids have been isolated and identified from natural sources, of which about 50 become constituents of a typical human diet. Approximately 20 are present in human blood and tissues, such as -carotene, -carotene, lycopene, lutein, zeaxanthin, -cryptoxanthin, -cryptoxanthin, -carotene, neurosporene, and -carotene [3–5]. ese carotenoids have been recognised as potent antiox- idants in humans that may play a role in preventing many diseases such as cancer, heart disease, Alzheimer’s disease, Parkinson’s disease, hypertension, and diabetes [6, 7]. In addi- tion to that, other already well-known function of carotenoids (like -carotene, -carotene and cryptoxanthin) in humans is as provitamin A activity. Vitamin A is an essential nutrient for functions such as embryonic development, cell differenti- ation, vision, immunity, and reproduction [8, 9]. Among the provitamin A carotenoids, -carotene is regarded the most potent precursor. In addition, it also has antioxidant action by scavenging oxygen radicals and reducing oxidative stress in the body. -carotene is an orange carotenoid that is abundant in apricots, asparagus, carrots, spinach, broccoli, papaya, grapefruits, sweet potatoes, pumpkin, and paprika [10–13]. However, due to their highly conjugated structure, carotenoids are rather unstable to ther- mal and chemical oxidation and can be easily degraded when exposed to light, oxygen, and heat during food processing and storage [14, 15]. Hindawi International Journal of Food Science Volume 2019, Article ID 8914852, 12 pages https://doi.org/10.1155/2019/8914852
13

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Page 1: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

Research ArticleMicroencapsulation of 120573-Carotene by Spray Drying Effect ofWall Material Concentration and Drying Inlet Temperature

Luiz C Correcirca-Filho Maria M LourenccediloMargarida Moldatildeo-Martins and V-tor D Alves

LEAF Linking Landscape Environment Agriculture and Food Instituto Superior de Agronomia Universidade de LisboaTapada da Ajuda 1349-017 Lisboa Portugal

Correspondence should be addressed to Margarida Moldao-Martins mmoldaoisaulisboapt

Received 18 August 2018 Revised 24 December 2018 Accepted 3 January 2019 Published 22 January 2019

Academic Editor Amy Simonne

Copyright copy 2019 Luiz C Correa-Filho et al This is an open access article distributed under the Creative Commons AttributionLicense which permits unrestricted use distribution and reproduction in any medium provided the original work is properlycited

Carotenoids are a class of natural pigments found mainly in fruits and vegetables Among them 120573-carotene is regarded the mostpotent precursor of vitamin A However it is susceptible to oxidation upon exposure to oxygen light and heat which can result inloss of colour antioxidant activity and vitamin activityThus the objective of this workwas to study themicroencapsulationprocessof 120573-carotene by spray drying using arabic gum as wall material to protect it against adverse environmental conditions This wascarried out using the response surface methodology coupled to a central composite rotatable design evaluating simultaneously theeffect of drying air inlet temperature (110-200∘C) and the wall material concentration (5-35) on the drying yield encapsulationefficiency loading capacity and antioxidant activity In addition morphology and particles size distribution were evaluatedScanning electron microscopy images have shown that the particles were microcapsules with a smooth surface when producedat the higher drying temperatures tested most of them having a diameter lower than 10 120583mThe conditions that enabled obtainingsimultaneously arabic gummicroparticles with higher 120573-carotene content higher encapsulation efficiency and higher drying yieldwere a wall material concentration of 119 and a drying inlet temperature of 173∘CThe systematic approach used for the study of120573-carotene microencapsulation process by spray drying using arabic gum may be easily applied for other core and wall materials

1 Introduction

Carotenoids which are synthesized by fruits and vegeta-bles are a family of hydrophobic pigmented compoundsthat structurally exist as hydrocarbons (carotenes) or theiroxygenated derivatives (xanthophylls) They are natural com-pounds responsible for yellow orange and red colours inmany foods [1ndash3] More than 700 different carotenoidshave been isolated and identified from natural sources ofwhich about 50 become constituents of a typical humandiet Approximately 20 are present in human blood andtissues such as 120573-carotene 120572-carotene lycopene luteinzeaxanthin 120573-cryptoxanthin 120572-cryptoxanthin 120574-caroteneneurosporene and 120577-carotene [3ndash5]

These carotenoids have been recognised as potent antiox-idants in humans that may play a role in preventing manydiseases such as cancer heart disease Alzheimerrsquos disease

Parkinsonrsquos disease hypertension and diabetes [6 7] In addi-tion to that other alreadywell-known function of carotenoids(like 120573-carotene 120572-carotene and cryptoxanthin) in humansis as provitamin A activity Vitamin A is an essential nutrientfor functions such as embryonic development cell differenti-ation vision immunity and reproduction [8 9]

Among the provitamin A carotenoids 120573-carotene isregarded the most potent precursor In addition it alsohas antioxidant action by scavenging oxygen radicals andreducing oxidative stress in the body 120573-carotene is anorange carotenoid that is abundant in apricots asparaguscarrots spinach broccoli papaya grapefruits sweet potatoespumpkin and paprika [10ndash13] However due to their highlyconjugated structure carotenoids are rather unstable to ther-mal and chemical oxidation and can be easily degraded whenexposed to light oxygen and heat during food processing andstorage [14 15]

HindawiInternational Journal of Food ScienceVolume 2019 Article ID 8914852 12 pageshttpsdoiorg10115520198914852

2 International Journal of Food Science

The stability of natural bioactive compounds ie thepreservation of their expected functional properties couldbe improved using encapsulation techniques such as spraydrying spray cooling coacervation extrusion coating influidized bed and polymerization [16] Microencapsulationis described as a technique to entrap tiny particles of solids ordroplets of liquids or gases in a biopolymer to result in smallspheres which are called microcapsules or microparticleswith diameters ranging from 1 to 1000 120583m This techniquecould simplify the manufacture handling and storage offood reducing production costs In addition the microen-capsulated bioactives are protected against environmentalconditions thereby improving its stability [16ndash18]

In the food industry spray drying is one of the oldestand most popular drying technologies used for microen-capsulation of carotenoids due to its low cost flexibilityproduction of good quality powder particles rapid solubilityof the capsules and continuous operation [15 19] Thestructures formed in the encapsulation process are composedby two components the core (bioactive compounds) and theprotective matrix material Core materials are dispersed in apolymer solution (wall material) and subsequently atomizedinto a hot chamber which promotes the rapid removal of thewater [18 20] The properties of the powdered particles (likeparticle size and distribution moisture content and thermalstability) may be affected by the type of wall material usedand by the spray drying operating conditions such as the inletand outlet temperatures feed flow rate inlet air flow rate andatomization speed or pressure [21]

Several wall materials are commonly used such as carbo-hydrates (modified starches maltodextrin pectins sucrosecellulose arabic gum agar and carrageenan) proteins(gelatin casein and milk or soy protein) lipids (stearic acidand mono and diglycerides) and their mixtures [20 22]From these polymers arabic gum is one of the most com-mon wall materials used in microencapsulation due to itsexcellent emulsification properties It is a complex polysac-charide obtained from the branches of acacia trees which iscomposed of approximately 2 protein and high proportionof carbohydrates (D-galactose L-rhamnose L-arabinose andD-glucuronic acid) [21 23 24] It is envisaged that caro-tenoids interact with the hydrophobic region of the arabicgum sample (hydrophobic proteins) via hydrophobic-hydro-phobic interactions In addition arabic gum promotes lowviscosity in aqueous media no colour or smell subtle tastehigh oxidative stability and good retention of volatiles [25]

Several studies regarding the carotenoids encapsulationprocess by spray drying have already been reported in theliterature [26ndash32]Though there is a lack of a systematic studyconcerning the simultaneous effect of process parameters inthe drying operation performance and on the properties ofthe particles obtained As such the aim of this work was togo further and study the encapsulation process of a modelcarotenoid molecule (120573-carotene) by spray drying usingarabic gum as wall material intending to evaluate simul-taneously the effect of drying inlet temperature and the wallmaterial concentration using the response surface method-ology coupled with a central composite rotatable designThe response variables were the drying yield encapsulation

efficiency particles loading morphology and size as wellas the antioxidant activity of the encapsulated 120573-carotenemolecules

2 Material and Methods

21 Materials 120573-carotene was supplied from SigmandashAldrich(Steinheim Germany) Arabic gum (LabChem) was usedto form the protective matrix 221015840-Azinobis (3-ethylbenzo-thiazoline-6-sulphonic acid) diammonium salt (ABTS) waspurchased from SigmandashAldrich (Steinheim Germany)6-Hydroxy-2578-tetramethylchroman-2-carboxylic acid(Trolox) was obtained from Acros Organics (Geel Belgium)Potassium persulfate (K2S2O8) and ethanol were purchasedfrom Panreac AppliChem

22 Spray Drying Process Arabic gum was dissolved indistilled water under stirring overnight at room temperatureat the concentration values indicated in Table 1 After fullhydration of the polymer molecules 120573-carotene (5 drybasis) was added to polymer solution and the emulsionwas produced by stirring with an Ultra-Turrax T25 (IKAGermany) at 13500 rpm for 1 min at ambient temperatureA volume of 25 mL of emulsion was prepared for eachexperimental condition

The resultant emulsions were fed at a rate of 37mLminminus1to a cocurrent spray dryer (Lab-Plant SD-05 HuddersfieldEngland) equipped with a 05 mm diameter nozzle a dryingchamber (500 mm height and 215 mm diameter) and acyclone (300 mm height and a bottom diameter of 90 mm)The drying air flow rate was set at 47 m3h The feedsolution was kept under magnetic stirring The pressure ofthe compressed air set at 17 bar and had a maximum flowrate of 73m3hThe inlet temperature ranged between 110 and200∘C Encapsulation of 120573-carotene with arabic gum (5ndash35)was performed according to an experimental design (Table 1)The ranges of arabic gum and inlet temperature were chosenaccording to preliminary results The dried powders obtainedwere collected and stored under vacuum and protected fromlight

23 Experimental Design Response surface methodology(RSM) coupled with a central composite rotatable design(CCRD) was used to evaluate the effects of arabic gum con-centration (5-35) and drying inlet temperature (110-200∘C)on the response variables drying yield (DY) encapsulationefficiency (EE) morphology of microparticles antioxidantactivity of the encapsulated 120573-carotene (AA) and micropar-ticles 120573-carotene content (LC) A total of 11 experimentswere carried out (Table 1) 4 factorial design points (plusmn 1) 4star points (plusmn1414) and 3 central points (0) The repetitionof the central point is used to determine the experimentalerror which is assumed to be constant along the experimentaldomainThe experiments were performed randomly in orderto avoid systematic errors

The responses data was fitted to second-order polynomialmodels using decoded variables as follows

119884119894 = 1198870 + 11988711198831 + 11988721198832 + 1198871111988321 + 11988722119883

22 + 1198871211988311198832 (1)

International Journal of Food Science 3

Table 1 Experimental design with coded and decoded values of independent variables and spray drying responses

Run Independent variables Responses variablesArabic gum () T LC EE AA DY

1 94 (-1) 1232 (-1) 219 99 053 2252 94 (-1) 1868 (+1) 273 147 011 2693 306 (+1) 1232 (-1) 244 80 078 1634 306 (+1) 1868 (+1) 294 92 024 1595 20 (0) 155 (0) 159 139 022 4396 20 (0) 155 (0) 140 125 027 4027 20 (0) 155 (0) 167 138 017 4138 5 (-120572) 155 (0) 336 160 005 2389 35 (120572) 155 (0) 264 122 030 23210 20 (0) 110 (-120572) 119 62 036 28611 20 (0) 200(+120572) 214 148 012 343T temperature (∘C) LC loading capacity (mg 120573-carotenegminus1particles) EE encapsulation efficiency () AA antioxidant activity (120583mol troloxmgminus1120573-carotene) DY drying yield ()

where Yi corresponds to the response variables X1 and X2represent the coded independent variables (arabic gum con-centration and drying inlet temperature respectively) b0 isthe interception bi bj bij (i j = 1 2) are the linear quadraticand interaction coefficients respectively The adequacy of themodel to the experimental data was verified by applying theanalysis of variance (ANOVA) and coefficient of determina-tion (R2) and adjusted R2 (R2 adj) [33]The statistical analysiswas carried out using the software ldquoStatisticTMrdquo version 7(Statsoft USA)

The optimum conditions for the microencapsulation of120573-carotene were determined considering the results of theresponse variables that were significantly affected by spraydrying conditions using the desirability function

24 AntioxidantActivity beforeMicroencapsulation The totalantioxidant activity of samples was performed by radicalscavenging activity assessment expressed as Trolox Equiva-lentAntioxidantActivity (TEAC) described by do SMRufinoAlves [34] andNenadis Wang [35] with slightmodificationsAn ABTS stock solution was prepared by dissolving ABTSin water at a 7 mM concentration ABTS+ solution wasproduced by reaction of 5 mL of ABTS stock solution and88 120583L of a 140 mM potassium persulfate (K2S2O8) solutionto give a final concentration of 245 mM This solution waskept in a dark room at room temperature for 12-16 h Beforeanalysis ABTS+ solution was diluted with ethanol to obtainan initial absorbance value of 070 plusmn005 at 734 nm

For the evaluation of the antioxidant activity of 120573-carotene itself a volume of 30 120583L of diluted 120573-carotene withethanol was mixed with 3000 120583L of ABTS+ solution followedby incubation for 6min in the darkThen the absorbance wasmeasured in a spectrophotometer (Unicam UVVis Spec-trometer ndash UV4) at a wavelength of 734 nm A calibrationcurve was performed using Trolox as standard antioxidantat the concentration range of 250-2000 120583M in ethanol Allanalytical measurements were carried out in triplicate

25 Spray Drying and Microparticlesrsquo Characterization

251 Drying Yield Drying yield (DY) was determined gravi-metrically as described by Di Battista Constenla [36] as theratio of the mass of microparticles collected at the end of thespray drying process and the mass of solids contained in thefeed solutions

252 Morphological Characterization of Microparticles Themorphology of the particles obtained by spray drying wasobserved by scanning electron microscopy (SEM) The sam-ples were coated with a mixture of gold (80) and palladium(20) in a vacuum chamber and analysed using a HitachiS2400 scanning microscope operated at 15kV with differentmagnifications (500x to 2000x) Particles size was measuredby analysing SEM images using the image processing softwareImageJ (National Institute of Health USA) [37]

253 Loading Capacity and Encapsulation Efficiency For thedetermination of the concentration of the 120573-carotene presentin the microparticles (LC) the method described by RochaFavaro-Trindade [27] was used with some modifications Amass of 10 mg of microparticles was added to 50 ml ofethanol The suspension was homogenized with an Ultra-Turrax T25 (IKA Germany) at 13500 rpm during 3 min inorder to break the particles Aftermixing the suspension wasplaced in amber glass flasks and kept away from light forabout 12 h at 5∘C Afterwards the suspension was centrifuged(HERMLE Labortechnik Z 383 K) at 10000 rpm during10 min at 8∘C in order to recover the supernatant Theconcentration of 120573-carotene in the liquid phase (supernatant)was quantified in a spectrophotometer (Unicam UVVisSpectrometer UV4) at a wavelength of 450 nm A calibrationcurve was performed with 120573-carotene diluted in ethanolwith different concentrations (05-10 mgLminus1) The loadingcapacity (LC) of the particles was expressed as the mass of120573-carotene per mass of particles

4 International Journal of Food Science

(a) (b) (c)

(d) (e) (f)

(g) (h) (i)

Figure 1 Scanning electron microscopy (SEM) images (magnification x500) of arabic gum microparticles with microencapsulated 120573-carotene (a) 94 AG 1232∘C (b) 94 AG 1868∘C (c) 306 AG 1232∘C (d) 306 AG 1868∘C (e) 20 AG 155∘C (f) 5 AG 155∘C(g) 35 AG 155∘C (h) 20 AG 110∘C (i) 20 AG 200∘C

The encapsulation efficiency (EE) was calculated as byRocha Favaro-Trindade [27] quantifying the ratio betweenthe mass of 120573-carotene present in the microparticles and the120573-carotenersquo mass initially present in the feed solution

254 Antioxidant Activity of the Encapsulated Material Forthe measurement of the antioxidant activity (AA) of theencapsulated molecules the microparticles core materialswere previously extracted with ethanol as described in theprevious section Afterwards a volume of 800 120583L of super-natant was mixed with 2200 120583L of ABTS+ solution followedby the steps described in Section 24 for pure 120573-carotene

3 Results and Discussion

31 Microparticle Morphology and Size Distribution Themorphological characteristics of the obtained arabic gummicroparticles with 120573-carotene were investigated using SEMSEM images have shown that the particles maintain a similar

spherical-like shape with a smooth or wrinkled surfacedepending on the drying conditions (Figure 1)

Most of the particles did not present a significant inci-dence of cracks or fissures in the outer surface indicating aresistant external physical structureMicroparticles producedwithout apparent damage have a lower gas permeabilitypresenting a more effective protection of the bioactive com-pounds from oxidation reactions and avoiding their unde-sired release [38]

Higher drying inlet temperatures tend to produce parti-cles with a smoother surface and with a low degree of teethand concavities (Figures 1(a) 1(b) 1(c) 1(d) 1(h) and 1(i))This fact may be attributed to rapid water evaporation andhigher pressure inside the particles during microencapsula-tion at higher temperatures preventing shrinking [39] On theother hand water diffusion is slower at lower temperaturesallowing more time for the particles to deform wrinkleand collapse [40] Similar results were reported by Santiago-Adame Medina-Torres [41] for microparticles of cinnamon

International Journal of Food Science 5

(a) (b)

Figure 2 Scanning electron microscopy (SEM) images (magnification x2000) of the internal surface of Arabic gum microparticles with120573-carotene microencapsulated (a) 20 AG 110∘C (b) 94 AG 1232∘C

infusions with maltodextrin in which the effect of threedifferent drying temperatures (140 160 and 180∘C) wasevaluated They found microparticles morphologically moredefined and smoother without evident cracks or particleagglomerations in the spray drying process both at 160 and180∘C

At the contrary Figures 1(a) and 1(c) 1(b) and 1(d)and 1(e) and 1(f) show that the different values of arabicgum concentration studied did not influence substantially theparticles morphology as mixtures with a similar proportionof smooth and collapsed particles were obtained GoncalvesEstevinho [23] and Tonon Brabet [42] also found no influ-ence of the wall material concentration on the morphology ofthe particles obtained in themicroencapsulation of vitamin Awith arabic gum and acaı pulp with maltodextrin

The internal morphology is shown in Figure 2 Allmicroparticles obtained were shown to be microcapsulesenvisaging that the core material (120573-carotene) was entrappedwithin the wall or in the centre Central void formation acharacteristic of the spray drying process is related to theexpansion of the particles during the latter stages of thedrying process when the temperature exceeds the boilingpoint of the water [43 44] This internal structure of themicroparticles was also observed in microencapsulated soy-bean extract microencapsulated by spray drying in arabicgum or maltodextrin matrix [45] as well as in gelatinarabicgummicroparticles loaded with fish oil [46]

Particle size distribution is a physical parameter of thepowders which may influence their properties involvinghandling transport and storage such as bulk density angleof repose flowability rehydration capacity solubility anddispersibility [17 47] According toOnwulata [48] and Tontuland Topuz [49] the stability of the functional componentssensitive to environmental conditions is also affected by theparticle size

The particle size of 120573-carotene loaded arabic gummicro-capsules ranged from 182 to 4091 120583m In Figure 3 theparticle size distribution of the microcapsules produced atdifferent temperatures is shown (at 1232 and 1868∘C) andwith different arabic gum concentrations (5 and 35) In allcases more than 80 of the particles had a size below 10 120583m

In general a higher frequency of particles with sizesabove 10 120583m was observed with increasing arabic gumconcentration (Figures 3(a) and 3(b))This factmay be relatedto the higher viscosity of the spray drying feed solutionAccording to Tontul and Topuz [49] and Tonon Brabet [42]the liquid droplet size during atomization varies directly withthe liquid viscosity at constant atomizer speed resulting inlarger particles Similar results were obtained for differentpowders produced by spray drying such as blackberry juicein maltodextrin Ferrari Germer [50] and coffee oil in arabicgum Frascareli Silva [51]

The increase in inlet drying temperature also resulted in ahigher frequency of particles with sizes above 10 120583m (Figures3(c) and 3(d)) This can be related to increased swellingthereby preventing contraction of the particle as the dryingtemperature increases [50 52]These results are in agreementwith those obtained by Tonon Brabet [42] who evaluated themicroencapsulated acaı pulp inmaltodextrin by spray dryingAccording to the authors slower drying rate ie when theinlet drying temperature is low the particles shrink evenlymaking their size smaller However when the drying rateis higher the rapid evaporation of the water creates a hardcrust in the particle that prevents its contraction in the dryingprocess resulting in larger particles

32 Response Surface Analysis Response surface methodol-ogy (RSM) was performed to optimize spray drying condi-tions considering linear quadratic and interaction effectsbetween independent variables on the microencapsulationof 120573-carotene with arabic gum A second-order polynomialmodel described by (1) was fitted to the experimental datavalues obtained for each response variable studied which arepresented in Table 1 The determination coefficients (R2 andRAdj2) and the linear and quadratic effects of the factorsas well as their interaction for each response variable arepresented in Table 2

The results show that except for the antioxidant activityresponse the mathematical model used was fitted withgood determination coefficients (R2 gt 070) According toLundstedt Seifert [53] values above 07 represent a good fitof the model In addition ANOVA indicated that the lack of

6 International Journal of Food Science

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(a)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(b)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(c)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(d)

Figure 3 Relative frequency (bars) and cumulative frequency (line) equivalent to the diameter of microparticles (a) 94 AG 1232∘C (b)94 AG 1868∘C (c) 5 AG 155∘C (d) 35 AG 155∘C

Table 2 Second-order polynomial equations for each response variable

Equation R2 RAdj2

EE = minus48699 lowast + 03036AG minus 0001AG2 + 0710T lowast minus 0002T2 lowast minus 0003AGT 087 074DY = minus175962 lowast + 4222AG lowast minus 0097AG2 lowast + 2245T lowast minus 0007T2 lowast minus 0004AGT 085 071LC = 56961ndash2808AG lowast + 0069AG2 lowast minus 0257T + 00025T2 lowast minus 00003AGT 091 082AG arabic gum () T temperature (∘C) EE encapsulation efficiency () DY drying yield () LC loading capacity (mg 120573-carotenegminus1particles)lowastAffectingsignificantly the response variable (pgt005)

fit (p gt 005) relative to pure error was not significant at 95of confidence level The expected errors of the models on theprediction of the responses were estimated to be 76 72and 127 for LC EE and DY respectively Figures 4(a) 4(b)and 5 show the 3-dimensional response surfaces that illustratethe effects of arabic gum concentration (AG ) and dryinginlet temperature (T ∘C) on the responses studied

321 Encapsulation Efficiency and Loading Capacity Theencapsulation efficiency values of 120573-carotenewith arabic gum

ranged between 62 and 160 and the loading capacity valuesranged from 119 to 336mg120573-carotenegminus1particles as shownin Table 1 Similar results were found by Rocha Favaro-Trindade [27] uponmicroencapsulation of lycopene inmodi-fied starch that found an EE around 21 and by Botrel Borges[54] who microencapsulated oregano oil using a mixtureof arabic gum maltodextrin and modified starch as wallmaterial by spray drying found an EE between 51 and 339

As seen in Figures 4(a) and 4(b) the increase in dryingtemperature and decrease in arabic gum concentration lead

International Journal of Food Science 7

18

16

14

12

10

8

6

4

200

180

160

140

1205

1015

2025

3035

EncapsulationEffi

ciency ()

Temperature ( ∘C) Arabic gum ()

(a)

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

45

40

35

30

25

20

15

10

Loading Capacity

(mg-caroteneg - 1particles)

(b)

Figure 4 Response surface fitted to (a) encapsulation efficiency and (b) loading capacity as a function of Arabic gum concentration anddrying inlet temperature

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

50

40

30

20

10

0

Drying yield (

)

Figure 5 Response surface fitted to drying yield as a function ofarabic gum concentration and drying

to an increase in the EE Regarding LC higher values wereobserved at both ends of the arabic gum concentrationthat is when the lowest (5) and the highest concentration(35) of the wall material were used In addition when thedrying temperature increased the loading capacity was alsoincreased The same behaviour was reported by Ferrari Ger-mer [50] in microparticles of blackberry using maltodextrinas wall material

According to Jafari Assadpoor [19] the encapsulationefficiency is influenced by the drying conditions emulsion

and bioactive compound characteristics and the wall materialproperties Low encapsulation efficiency value could be dueto 120573-carotene being extremely sensitive to environmentalfactors such as exposure to heat light and oxygen duringencapsulation processing

The experimental data obtained of the encapsulation effi-ciency and loading capacity of the particles were adjusted tothe second-order polynomialmodelwith a satisfactory coeffi-cient of determination (Table 2) Both independent variableshad a significant effect on these responses Arabic gumconcentration had a positive quadratic effect on the loadingcapacity of the microparticles whereas for the encapsulationefficiency arabic gum concentration showed a linear negativeeffect In relation to the drying inlet temperature a positivelinear and quadratic negative effect on the encapsulation effi-ciency and a positive linear effect on the loading capacitywereobserved However the interaction coefficient was found tobe nonsignificant indicating that there was no interactionbetween the independent variables on the EE of particles

The drying temperature is directly proportional to theevaporation rate and inversely proportional to the finalwater content of the dried microparticles At high dryingtemperatures there is a higher evaporation rate of water onthe droplet surface which leads to the rapid formation of asemipermeable membrane resulting in the protection of therelease of the bioactive compounds during the drying processand consequently in a higher bioactive retention Howeverhigher drying temperatures could cause cracks and fissureson the surface of the particles leading to loss of the bioactivecompound [19 21]

Wall material concentration is also a factor that affectsthe retention of the bioactive compounds due to their vis-cosity properties in the feed solution Some researchers have

8 International Journal of Food Science

reported that the wall material concentration has a positiveeffect on the encapsulation efficiency ie the increase ofsolids content in the feed increases bioactive retention [21 5556] This behaviour could be related to the reduction of thetime required to form a surface crust in the atomized dropletsin the initial drying process when the solids concentration inthe feed solution increases This rapidly formed crust is notpermeable to compounds thereby protecting the bioactivefrom oxidation [57 58]

However too high viscosity of the feed solutions delaysthe formation of discrete particles during spray dryingwhereas a low viscosity in feed delays the formation of asemipermeable surface crust favouring further losses of thebioactive compounds [59] Therefore according to Reinec-cius [60] each wall material has its ideal feed concentrationto obtain higher encapsulation efficiency which is basedon the solubility and viscosity of the feed solution In thiswork an ideal arabic gum concentration of 74 was foundfor higher values of encapsulation efficiency and loadingcapacity Fernandes Marques [57] who evaluated the effectof total solids concentration on the microencapsulation ofrosemary essential oil by spray drying using maltodextrinand modified starch (11) as wall materials found higherencapsulation efficiency when a concentration of the wallmaterial of 22 was used which was reported as the idealconcentration for maltodextrin as wall material

322 Drying Yield Drying yield of the spray drying processis directly related to the cost of production and efficiencythus it is an important indicator that the industry considersin its production line [49 61] According to Nunes andMercadante [62] and Rutz Borges [63] drying yield isinfluenced by both the equipment settings (feed rate feedinlet and outlet temperature and flow rate) and dryingconditions (type and wall material concentration)

In this study a second-order model was fitted to theexperimental data of the drying yield with acceptable coef-ficient of determination and Table 2 shows that both inde-pendent variables arabic gum concentration and the dryinginlet temperature had a significant negative quadratic effecton the drying yield According to Table 1 the drying yields of120573-carotene with arabic gum ranged between 159 and 439Other researchers have found values of drying yield around50 Roccia Martınez [64] who studied the microencapsu-lation of the sunflower oil by spray drying using maltodextrinas a carrier agent found drying yield values that ranged from544 to 3988 and Santana Kurozawa [31] produced arabicgum microparticles with pulp pequi extract by spray dryingand obtained a drying yield values between 258 and 561

Low drying yield in the spray drying process is mostlydue to retention of the powder in the drying chamber wallcyclone inefficient in collecting fine particles and the highviscosity of the feed solution This powder retention problemcauses considerable economic loss and it is not cost-effectivefor industry as there would be frequent interruptions tothe dryer cleaning besides affecting the quality of the finalproduct However drying yield in the microencapsulationtechnique could be improved by modifying the spray dryingconditions in order to decrease the adhesion of particles to

the drying chamber wall [64ndash66] According to Tontul andTopuz [49] and Jayasundera Adhikari [67] the mechanicalscraping of the drying chamber wall introduction of coldair from the bottom and the use of low temperature lowhumidity air are some examples of process-based approachesthat could increase drying yield

As shown in Figure 5 as the drying temperature andthe arabic gum concentration increased the drying yieldalso increased until a maximum value was achieved Afterthis value decreases in the drying yield were observed evenwith the increase of both independent variables The highestdrying yield value was found for the sample with 20 GAdried at 155∘C

Chong and Wong [68] also found an optimum dosageof the wall material concentration (30 maltodextrin) andtemperature value (180∘C) that maximized the drying yield(57) when producing sapodilla puree particles by spraydrying using different maltodextrin concentrations (10-50wv) The authors referred that increasing the wall materialconcentration above the optimum value leads to an increaseviscosity of the feed solution thereby negatively affecting thedrying yield

323 Antioxidant Activity The AA values of encapsulated120573-carotene range from 005 to 078 120583mol troloxmgminus1120573-carotene whereas the commercial 120573-carotene before encap-sulation possessed 235 120583mol troloxmgminus1120573-carotene Thelower antioxidant activity after the encapsulation may berelated not only to the encapsulation process itself but alsoto the incomplete extraction of the encapsulated moleculesbefore antioxidant activity measurement This decrease inantioxidant activity after the spray drying process was alsoobserved for example by Franceschinis Salvatori [69] in themicroencapsulation of blackberry juices with maltodextrinand Hee Tan [70] in virgin coconut oil microparticles in amixture of maltodextrin arabic gum sodium caseinate andwhey protein concentrate

The data obtained for the antioxidant activity did notfit the second-order polynomial model though from theresults of Table 1 the two independent variables studiedarabic gum concentration and drying inlet temperatureaffected antioxidant activity of the encapsulated moleculessince an AA increase was observed when the temperaturedecreased (runs 4-3 2-1 and 11-10) and when the arabic gumconcentration increased (runs 1-3 2-4 8-9)

Other researchers have also studied the influence ofdrying inlet temperature and wall material on AA of theparticles Kha Nguyen [71] studied the effects of varyingmaltodextrin concentrations and spray drying temperatureson the antioxidant activity of Gac fruit powder and theyreported that increasing the drying inlet temperature from120 to 200∘C showed a significant loss of AA Additionallywith increasing maltodextrin concentration from 20 to 30the loss of AA was also observed The authors explainedthat AA loss could be due to loss of antioxidant compoundspresent in Gac powder spray dried at high temperaturesMiravet Alacid [72] who evaluated the antioxidant activityof pomegranate juice powder produced by spray dryingusing prebiotic fibers and maltodextrin as wall material also

International Journal of Food Science 9

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

10

08

06

04

02

00

minus02

Desirability

Figure 6 Desirability surface for optimal conditions

observed that the increase of the drying inlet temperaturefrom 160 to 200∘C had a significant negative effect on theantioxidant activity for both wall materials studied

324 Optimization of Drying Process Conditions The desir-ability function was performed for the simultaneous opti-mization of the responses that fitted to the second-ordermodel (Table 2) and the desirability surface for optimalconditions is depicted in Figure 6 Desirability values higherthan 07 were considered indicating a good optimization ofthe experimental data of each response variable [73] Thebest conditions for the spray drying microencapsulation of 120573-carotene with arabic gum as wall material were determined inorder to obtain higher values for drying yield encapsulationefficiency and loading capacity

The inlet drying temperature of 173∘C and arabic gumconcentration of 119 are recommended as the ideal con-ditions for microencapsulation of 120573-carotene Under theseconditions the predicted EE DY and LC are 1562 3630and 2274 mg 120573-carotenegminus1particles respectively

4 Conclusions

Themicroencapsulation of120573-carotene in arabic gumby spraydrying was investigated The arabic gum concentration anddrying inlet temperature influenced the drying yield encap-sulation efficiency and load capacity responses Regardingthe AA the antioxidant activity of 120573-carotene was reducedwhen microencapsulated at high temperatures (200∘C) inrelation to low temperatures (110∘C)

SEM analysis showed that the microparticles are micro-capsules Most of them presented a similar morphology amixture of smooth and wrinkled particles with a diameterlower than 10 120583m Increases in drying temperature favouredthe formation of smoother and larger particles

From the experimental conditions the drying inlet tem-perature of 173∘C and the arabic gum concentration of 119

were those that allow obtaining higher 120573-carotene contenthigher encapsulation efficiency and higher drying yield

The systematic approach used for the study of 120573-carotenemicroencapsulation process by spray drying may be easilyapplied for other core and wall materials Further studies willfocus on release studies in several aqueous media and even-tually on the encapsulation of natural carotenoid extracts

Data Availability

The data used to support the findings of this study areincluded within the article

Conflicts of Interest

The authors declare that they have no conflicts of interest

Acknowledgments

This work was supported by Conselho Nacional de Desen-volvimento Cientıfico e TecnologicondashCNPq through theCiencia sem Fronteiras program (CSF) (Grant CSF 2062682014-9 to first author)The authors acknowledge the financialsupport from Fundacao para a Ciencia e a TecnologiaPortugal Project UIDAGR041292013

References

[1] M E Rodrıguez-Huezo R Pedroza-Islas L A Prado-Bar-ragan C I Beristain and E J Vernon-Carter ldquoMicroencapsu-lation by spray drying of multiple emulsions containing caro-tenoidsrdquo Journal of Food Science vol 69 no 7 pp 351ndash359 2004

[2] A V Rao and L G Rao ldquoCarotenoids and human healthrdquoPharmacological Research vol 55 no 3 pp 207ndash216 2007

[3] J Fiedor and K Burda ldquoPotential role of carotenoids as anti-oxidants in human health and diseaserdquo Nutrients vol 6 no 2pp 466ndash488 2014

[4] R Arimboor R B Natarajan K R Menon L P Chan-drasekhar and VMoorkoth ldquoRed pepper (Capsicum annuum)carotenoids as a source of natural food colors analysis andstabilitymdasha reviewrdquo Journal of Food Science and Technology vol52 no 3 pp 1258ndash1271 2015

[5] M H Walter and D Strack ldquoCarotenoids and their cleavageproducts Biosynthesis and functionsrdquoNatural Product Reportsvol 28 no 4 pp 663ndash692 2011

[6] A Kaczor M Baranska and K Czamara Carotenoids WileyOnline Library 2016

[7] A F Aissa M L P Bianchi J C Ribeiro et al ldquoComparativestudy of 120573-carotene and microencapsulated 120573-carotene Eval-uation of their genotoxic and antigenotoxic effectsrdquo Food andChemical Toxicology vol 50 no 5 pp 1418ndash1424 2012

[8] Z Al Tanoury A Piskunov and C Rochette-Egly ldquoVitamina and retinoid signaling Genomic and nongenomic effectsrdquoJournal of Lipid Research vol 54 no 7 pp 1761ndash1775 2013

[9] E G Donhowe F P Flores W L Kerr L Wicker and F KongldquoCharacterization and invitro bioavailability of 120573-caroteneEffects of microencapsulation method and food matrixrdquo LWT-Food Science and Technology vol 57 no 1 pp 42ndash48 2014

[10] K Gul A Tak A Singh et al ldquoChemistry encapsulation andhealth benefits of szlig-carotene-A reviewrdquo Cogent Food amp Agri-culture vol 1 no 1 Article ID 1018696 2015

10 International Journal of Food Science

[11] HW Kim J B Kim S Poovan et al ldquoEffect of processing con-ditions on the content of cistrans carotene isomers as provita-min A carotenoids in Korean sweet potato varietiesrdquo Interna-tional Journal of Food Sciences and Nutrition vol 65 no 7 pp821ndash826 2014

[12] C Qian E A Decker H Xiao and D J McClements ldquoNano-emulsion delivery systems Influence of carrier oil on 120573-caro-tene bioaccessibilityrdquo Food Chemistry vol 135 no 3 pp 1440ndash1447 2012

[13] J C Spada L D F Marczak I C Tessaro and C P Z NorenaldquoMicroencapsulation of 120573-carotene using native pinhao starchmodified pinhao starch and gelatin by freeze-dryingrdquo Interna-tional Journal of Food Science amp Technology vol 47 no 1 pp186ndash194 2012

[14] G Zakynthinos and T Varzakas ldquoCarotenoids From plants tofood industryrdquo Current Research in Nutrition and Food Sciencevol 4 no 1 pp 38ndash51 2016

[15] R Liang Q Huang J Ma C F Shoemaker and F ZhongldquoEffect of relative humidity on the store stability of spray-driedbeta-carotene nanoemulsionsrdquo Food Hydrocolloids vol 33 no2 pp 225ndash233 2013

[16] C Saenz S Tapia J Chavez and P Robert ldquoMicroencapsula-tion by spray drying of bioactive compounds from cactus pear(Opuntia ficus-indica)rdquo Food Chemistry vol 114 no 2 pp 616ndash622 2009

[17] S AkhavanMahdavi SM Jafari E Assadpoor andDDehnadldquoMicroencapsulation optimization of natural anthocyaninswith maltodextrin gum Arabic and gelatinrdquo InternationalJournal of Biological Macromolecules vol 85 pp 379ndash385 2016

[18] N V N Jyothi P M Prasanna S N Sakarkar K S PrabhaP S Ramaiah and G Y Srawan ldquoMicroencapsulation tech-niques factors influencing encapsulation efficiencyrdquo Journal ofMicroencapsulation vol 27 no 3 pp 187ndash197 2010

[19] S M Jafari E Assadpoor Y He and B Bhandari ldquoEncapsu-lation efficiency of food flavours and oils during spray dryingrdquoDrying Technology vol 26 no 7 pp 816ndash835 2008

[20] S C Samantha A S Bruna R M Adriana B Fabio A RSandro and R C Aline ldquoDrying by spray drying in the foodindustry Micro-encapsulation process parameters and maincarriers usedrdquo African Journal of Food Science vol 9 no 9 pp462ndash470 2015

[21] T C Kha M H Nguyen P D Roach and C E StathopoulosldquoMicroencapsulation of Gac oil Optimisation of spray dryingconditions using response surface methodologyrdquo Powder Tech-nology vol 264 pp 298ndash309 2014

[22] E Janiszewska-Turak ldquoCarotenoids microencapsulation byspray drying method and supercritical micronizationrdquo FoodResearch International vol 99 pp 891ndash901 2017

[23] A Goncalves B N Estevinho and F Rocha ldquoDesign andcharacterization of controlled-release vitamin A microparticlesprepared by a spray-drying processrdquo Powder Technology vol305 pp 411ndash417 2017

[24] MOrdonez and AHerrera ldquoMorphologic and stability cassavastarch matrices for encapsulating limonene by spray dryingrdquoPowder Technology vol 253 pp 89ndash97 2014

[25] S-M Jafari K Mahdavi-Khazaei and A Hemmati-KakhkildquoMicroencapsulation of saffron petal anthocyanins with cressseed gum compared with Arabic gum through freeze dryingrdquoCarbohydrate Polymers vol 140 pp 20ndash25 2016

[26] M P Rascon C I Beristain H S Garcıa and M A Sal-gado ldquoCarotenoid retention and storage stability of spray-dried encapsulated paprika oleoresin using gum Arabic and

Soy protein isolate as wall materialsrdquo LWT- Food Science andTechnology vol 44 no 2 pp 549ndash557 2011

[27] GA Rocha C S Favaro-Trindade andC R F Grosso ldquoMicro-encapsulation of lycopene by spray drying Characterizationstability and application of microcapsulesrdquo Food and Bioprod-ucts Processing vol 90 no 1 pp 37ndash42 2012

[28] Q Shen and S Y Quek ldquoMicroencapsulation of astaxanthinwith blends of milk protein and fiber by spray dryingrdquo Journalof Food Engineering vol 123 pp 165ndash171 2014

[29] A M Goula and K G Adamopoulos ldquoA new technique forspray-dried encapsulation of lycopenerdquoDrying Technology vol30 no 6 pp 641ndash652 2012

[30] J Loksuwan ldquoCharacteristics of microencapsulated 120573-caroteneformed by spray drying with modified tapioca starch nativetapioca starch andmaltodextrinrdquoFoodHydrocolloids vol 21 no5-6 pp 928ndash935 2007

[31] A A Santana L E Kurozawa R A de Oliveira and K JPark ldquoInfluence of Process Conditions on the PhysicochemicalProperties of Pequi Powder Produced by Spray Dryingrdquo DryingTechnology vol 31 no 7 pp 825ndash836 2013

[32] D Troya D S Tupuna-Yerovi and J Ruales ldquoEffects of WallMaterials and Operating Parameters on Physicochemical Pro-perties Process Efficiency and Total Carotenoid Content ofMicroencapsulated Banana Passionfruit Pulp (Passiflora tri-partita var mollissima) by Spray-Dryingrdquo Food and BioprocessTechnology vol 11 no 10 pp 1828ndash1839 2018

[33] D C Montgomery Design and Analysis of Experiments JohnWiley amp Sons 8th edition 2012

[34] M do S M Rufino R Alves E de Brito et al MetodologiaCientıfica Determinacao da Atividade Antioxidante Total emFrutas pela Captura do Radical Livre ABTS ComunicadoTecnico (Embrapa Agroindustria Tropical Online) 2007

[35] N Nenadis L-F Wang M Tsimidou and H-Y Zhang ldquoEsti-mation of scavenging activity of phenolic compounds using theABTS∙+ assayrdquo Journal of Agricultural and Food Chemistry vol52 no 15 pp 4669ndash4674 2004

[36] C A Di Battista D ConstenlaM V Ramırez-Rigo and J PinaldquoThe use of Arabic gum maltodextrin and surfactants in themicroencapsulation of phytosterols by spray dryingrdquo PowderTechnology vol 286 pp 193ndash201 2015

[37] C A Schneider W S Rasband and K W Eliceiri ldquoNIH Imageto ImageJ 25 years of image analysisrdquo Nature Methods vol 9no 7 pp 671ndash675 2012

[38] S Shamaei S S Seiiedlou M Aghbashlo E Tsotsas and AKharaghani ldquoMicroencapsulation of walnut oil by spray dry-ing effects of wall material and drying conditions on physico-chemical properties of microcapsulesrdquo Innovative Food Scienceand Emerging Technologies vol 39 pp 101ndash112 2017

[39] L Medina-Torres R Santiago-Adame F Calderas et alldquoMicroencapsulation by spray drying of laurel infusions (Litseaglaucescens) with maltodextrinrdquo Industrial Crops and Productsvol 90 pp 1ndash8 2016

[40] S Beirao-da-Costa C Duarte A I Bourbon et al ldquoInulinpotential for encapsulation and controlled delivery of Oreganoessential oilrdquo Food Hydrocolloids vol 33 no 2 pp 199ndash2062013

[41] R Santiago-Adame L Medina-Torres J A Gallegos-Infante etal ldquoSpray drying-microencapsulation of cinnamon infusions(Cinnamomum zeylanicum) with maltodextrinrdquo LWT- FoodScience and Technology vol 64 no 2 pp 571ndash577 2015

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

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Page 2: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

2 International Journal of Food Science

The stability of natural bioactive compounds ie thepreservation of their expected functional properties couldbe improved using encapsulation techniques such as spraydrying spray cooling coacervation extrusion coating influidized bed and polymerization [16] Microencapsulationis described as a technique to entrap tiny particles of solids ordroplets of liquids or gases in a biopolymer to result in smallspheres which are called microcapsules or microparticleswith diameters ranging from 1 to 1000 120583m This techniquecould simplify the manufacture handling and storage offood reducing production costs In addition the microen-capsulated bioactives are protected against environmentalconditions thereby improving its stability [16ndash18]

In the food industry spray drying is one of the oldestand most popular drying technologies used for microen-capsulation of carotenoids due to its low cost flexibilityproduction of good quality powder particles rapid solubilityof the capsules and continuous operation [15 19] Thestructures formed in the encapsulation process are composedby two components the core (bioactive compounds) and theprotective matrix material Core materials are dispersed in apolymer solution (wall material) and subsequently atomizedinto a hot chamber which promotes the rapid removal of thewater [18 20] The properties of the powdered particles (likeparticle size and distribution moisture content and thermalstability) may be affected by the type of wall material usedand by the spray drying operating conditions such as the inletand outlet temperatures feed flow rate inlet air flow rate andatomization speed or pressure [21]

Several wall materials are commonly used such as carbo-hydrates (modified starches maltodextrin pectins sucrosecellulose arabic gum agar and carrageenan) proteins(gelatin casein and milk or soy protein) lipids (stearic acidand mono and diglycerides) and their mixtures [20 22]From these polymers arabic gum is one of the most com-mon wall materials used in microencapsulation due to itsexcellent emulsification properties It is a complex polysac-charide obtained from the branches of acacia trees which iscomposed of approximately 2 protein and high proportionof carbohydrates (D-galactose L-rhamnose L-arabinose andD-glucuronic acid) [21 23 24] It is envisaged that caro-tenoids interact with the hydrophobic region of the arabicgum sample (hydrophobic proteins) via hydrophobic-hydro-phobic interactions In addition arabic gum promotes lowviscosity in aqueous media no colour or smell subtle tastehigh oxidative stability and good retention of volatiles [25]

Several studies regarding the carotenoids encapsulationprocess by spray drying have already been reported in theliterature [26ndash32]Though there is a lack of a systematic studyconcerning the simultaneous effect of process parameters inthe drying operation performance and on the properties ofthe particles obtained As such the aim of this work was togo further and study the encapsulation process of a modelcarotenoid molecule (120573-carotene) by spray drying usingarabic gum as wall material intending to evaluate simul-taneously the effect of drying inlet temperature and the wallmaterial concentration using the response surface method-ology coupled with a central composite rotatable designThe response variables were the drying yield encapsulation

efficiency particles loading morphology and size as wellas the antioxidant activity of the encapsulated 120573-carotenemolecules

2 Material and Methods

21 Materials 120573-carotene was supplied from SigmandashAldrich(Steinheim Germany) Arabic gum (LabChem) was usedto form the protective matrix 221015840-Azinobis (3-ethylbenzo-thiazoline-6-sulphonic acid) diammonium salt (ABTS) waspurchased from SigmandashAldrich (Steinheim Germany)6-Hydroxy-2578-tetramethylchroman-2-carboxylic acid(Trolox) was obtained from Acros Organics (Geel Belgium)Potassium persulfate (K2S2O8) and ethanol were purchasedfrom Panreac AppliChem

22 Spray Drying Process Arabic gum was dissolved indistilled water under stirring overnight at room temperatureat the concentration values indicated in Table 1 After fullhydration of the polymer molecules 120573-carotene (5 drybasis) was added to polymer solution and the emulsionwas produced by stirring with an Ultra-Turrax T25 (IKAGermany) at 13500 rpm for 1 min at ambient temperatureA volume of 25 mL of emulsion was prepared for eachexperimental condition

The resultant emulsions were fed at a rate of 37mLminminus1to a cocurrent spray dryer (Lab-Plant SD-05 HuddersfieldEngland) equipped with a 05 mm diameter nozzle a dryingchamber (500 mm height and 215 mm diameter) and acyclone (300 mm height and a bottom diameter of 90 mm)The drying air flow rate was set at 47 m3h The feedsolution was kept under magnetic stirring The pressure ofthe compressed air set at 17 bar and had a maximum flowrate of 73m3hThe inlet temperature ranged between 110 and200∘C Encapsulation of 120573-carotene with arabic gum (5ndash35)was performed according to an experimental design (Table 1)The ranges of arabic gum and inlet temperature were chosenaccording to preliminary results The dried powders obtainedwere collected and stored under vacuum and protected fromlight

23 Experimental Design Response surface methodology(RSM) coupled with a central composite rotatable design(CCRD) was used to evaluate the effects of arabic gum con-centration (5-35) and drying inlet temperature (110-200∘C)on the response variables drying yield (DY) encapsulationefficiency (EE) morphology of microparticles antioxidantactivity of the encapsulated 120573-carotene (AA) and micropar-ticles 120573-carotene content (LC) A total of 11 experimentswere carried out (Table 1) 4 factorial design points (plusmn 1) 4star points (plusmn1414) and 3 central points (0) The repetitionof the central point is used to determine the experimentalerror which is assumed to be constant along the experimentaldomainThe experiments were performed randomly in orderto avoid systematic errors

The responses data was fitted to second-order polynomialmodels using decoded variables as follows

119884119894 = 1198870 + 11988711198831 + 11988721198832 + 1198871111988321 + 11988722119883

22 + 1198871211988311198832 (1)

International Journal of Food Science 3

Table 1 Experimental design with coded and decoded values of independent variables and spray drying responses

Run Independent variables Responses variablesArabic gum () T LC EE AA DY

1 94 (-1) 1232 (-1) 219 99 053 2252 94 (-1) 1868 (+1) 273 147 011 2693 306 (+1) 1232 (-1) 244 80 078 1634 306 (+1) 1868 (+1) 294 92 024 1595 20 (0) 155 (0) 159 139 022 4396 20 (0) 155 (0) 140 125 027 4027 20 (0) 155 (0) 167 138 017 4138 5 (-120572) 155 (0) 336 160 005 2389 35 (120572) 155 (0) 264 122 030 23210 20 (0) 110 (-120572) 119 62 036 28611 20 (0) 200(+120572) 214 148 012 343T temperature (∘C) LC loading capacity (mg 120573-carotenegminus1particles) EE encapsulation efficiency () AA antioxidant activity (120583mol troloxmgminus1120573-carotene) DY drying yield ()

where Yi corresponds to the response variables X1 and X2represent the coded independent variables (arabic gum con-centration and drying inlet temperature respectively) b0 isthe interception bi bj bij (i j = 1 2) are the linear quadraticand interaction coefficients respectively The adequacy of themodel to the experimental data was verified by applying theanalysis of variance (ANOVA) and coefficient of determina-tion (R2) and adjusted R2 (R2 adj) [33]The statistical analysiswas carried out using the software ldquoStatisticTMrdquo version 7(Statsoft USA)

The optimum conditions for the microencapsulation of120573-carotene were determined considering the results of theresponse variables that were significantly affected by spraydrying conditions using the desirability function

24 AntioxidantActivity beforeMicroencapsulation The totalantioxidant activity of samples was performed by radicalscavenging activity assessment expressed as Trolox Equiva-lentAntioxidantActivity (TEAC) described by do SMRufinoAlves [34] andNenadis Wang [35] with slightmodificationsAn ABTS stock solution was prepared by dissolving ABTSin water at a 7 mM concentration ABTS+ solution wasproduced by reaction of 5 mL of ABTS stock solution and88 120583L of a 140 mM potassium persulfate (K2S2O8) solutionto give a final concentration of 245 mM This solution waskept in a dark room at room temperature for 12-16 h Beforeanalysis ABTS+ solution was diluted with ethanol to obtainan initial absorbance value of 070 plusmn005 at 734 nm

For the evaluation of the antioxidant activity of 120573-carotene itself a volume of 30 120583L of diluted 120573-carotene withethanol was mixed with 3000 120583L of ABTS+ solution followedby incubation for 6min in the darkThen the absorbance wasmeasured in a spectrophotometer (Unicam UVVis Spec-trometer ndash UV4) at a wavelength of 734 nm A calibrationcurve was performed using Trolox as standard antioxidantat the concentration range of 250-2000 120583M in ethanol Allanalytical measurements were carried out in triplicate

25 Spray Drying and Microparticlesrsquo Characterization

251 Drying Yield Drying yield (DY) was determined gravi-metrically as described by Di Battista Constenla [36] as theratio of the mass of microparticles collected at the end of thespray drying process and the mass of solids contained in thefeed solutions

252 Morphological Characterization of Microparticles Themorphology of the particles obtained by spray drying wasobserved by scanning electron microscopy (SEM) The sam-ples were coated with a mixture of gold (80) and palladium(20) in a vacuum chamber and analysed using a HitachiS2400 scanning microscope operated at 15kV with differentmagnifications (500x to 2000x) Particles size was measuredby analysing SEM images using the image processing softwareImageJ (National Institute of Health USA) [37]

253 Loading Capacity and Encapsulation Efficiency For thedetermination of the concentration of the 120573-carotene presentin the microparticles (LC) the method described by RochaFavaro-Trindade [27] was used with some modifications Amass of 10 mg of microparticles was added to 50 ml ofethanol The suspension was homogenized with an Ultra-Turrax T25 (IKA Germany) at 13500 rpm during 3 min inorder to break the particles Aftermixing the suspension wasplaced in amber glass flasks and kept away from light forabout 12 h at 5∘C Afterwards the suspension was centrifuged(HERMLE Labortechnik Z 383 K) at 10000 rpm during10 min at 8∘C in order to recover the supernatant Theconcentration of 120573-carotene in the liquid phase (supernatant)was quantified in a spectrophotometer (Unicam UVVisSpectrometer UV4) at a wavelength of 450 nm A calibrationcurve was performed with 120573-carotene diluted in ethanolwith different concentrations (05-10 mgLminus1) The loadingcapacity (LC) of the particles was expressed as the mass of120573-carotene per mass of particles

4 International Journal of Food Science

(a) (b) (c)

(d) (e) (f)

(g) (h) (i)

Figure 1 Scanning electron microscopy (SEM) images (magnification x500) of arabic gum microparticles with microencapsulated 120573-carotene (a) 94 AG 1232∘C (b) 94 AG 1868∘C (c) 306 AG 1232∘C (d) 306 AG 1868∘C (e) 20 AG 155∘C (f) 5 AG 155∘C(g) 35 AG 155∘C (h) 20 AG 110∘C (i) 20 AG 200∘C

The encapsulation efficiency (EE) was calculated as byRocha Favaro-Trindade [27] quantifying the ratio betweenthe mass of 120573-carotene present in the microparticles and the120573-carotenersquo mass initially present in the feed solution

254 Antioxidant Activity of the Encapsulated Material Forthe measurement of the antioxidant activity (AA) of theencapsulated molecules the microparticles core materialswere previously extracted with ethanol as described in theprevious section Afterwards a volume of 800 120583L of super-natant was mixed with 2200 120583L of ABTS+ solution followedby the steps described in Section 24 for pure 120573-carotene

3 Results and Discussion

31 Microparticle Morphology and Size Distribution Themorphological characteristics of the obtained arabic gummicroparticles with 120573-carotene were investigated using SEMSEM images have shown that the particles maintain a similar

spherical-like shape with a smooth or wrinkled surfacedepending on the drying conditions (Figure 1)

Most of the particles did not present a significant inci-dence of cracks or fissures in the outer surface indicating aresistant external physical structureMicroparticles producedwithout apparent damage have a lower gas permeabilitypresenting a more effective protection of the bioactive com-pounds from oxidation reactions and avoiding their unde-sired release [38]

Higher drying inlet temperatures tend to produce parti-cles with a smoother surface and with a low degree of teethand concavities (Figures 1(a) 1(b) 1(c) 1(d) 1(h) and 1(i))This fact may be attributed to rapid water evaporation andhigher pressure inside the particles during microencapsula-tion at higher temperatures preventing shrinking [39] On theother hand water diffusion is slower at lower temperaturesallowing more time for the particles to deform wrinkleand collapse [40] Similar results were reported by Santiago-Adame Medina-Torres [41] for microparticles of cinnamon

International Journal of Food Science 5

(a) (b)

Figure 2 Scanning electron microscopy (SEM) images (magnification x2000) of the internal surface of Arabic gum microparticles with120573-carotene microencapsulated (a) 20 AG 110∘C (b) 94 AG 1232∘C

infusions with maltodextrin in which the effect of threedifferent drying temperatures (140 160 and 180∘C) wasevaluated They found microparticles morphologically moredefined and smoother without evident cracks or particleagglomerations in the spray drying process both at 160 and180∘C

At the contrary Figures 1(a) and 1(c) 1(b) and 1(d)and 1(e) and 1(f) show that the different values of arabicgum concentration studied did not influence substantially theparticles morphology as mixtures with a similar proportionof smooth and collapsed particles were obtained GoncalvesEstevinho [23] and Tonon Brabet [42] also found no influ-ence of the wall material concentration on the morphology ofthe particles obtained in themicroencapsulation of vitamin Awith arabic gum and acaı pulp with maltodextrin

The internal morphology is shown in Figure 2 Allmicroparticles obtained were shown to be microcapsulesenvisaging that the core material (120573-carotene) was entrappedwithin the wall or in the centre Central void formation acharacteristic of the spray drying process is related to theexpansion of the particles during the latter stages of thedrying process when the temperature exceeds the boilingpoint of the water [43 44] This internal structure of themicroparticles was also observed in microencapsulated soy-bean extract microencapsulated by spray drying in arabicgum or maltodextrin matrix [45] as well as in gelatinarabicgummicroparticles loaded with fish oil [46]

Particle size distribution is a physical parameter of thepowders which may influence their properties involvinghandling transport and storage such as bulk density angleof repose flowability rehydration capacity solubility anddispersibility [17 47] According toOnwulata [48] and Tontuland Topuz [49] the stability of the functional componentssensitive to environmental conditions is also affected by theparticle size

The particle size of 120573-carotene loaded arabic gummicro-capsules ranged from 182 to 4091 120583m In Figure 3 theparticle size distribution of the microcapsules produced atdifferent temperatures is shown (at 1232 and 1868∘C) andwith different arabic gum concentrations (5 and 35) In allcases more than 80 of the particles had a size below 10 120583m

In general a higher frequency of particles with sizesabove 10 120583m was observed with increasing arabic gumconcentration (Figures 3(a) and 3(b))This factmay be relatedto the higher viscosity of the spray drying feed solutionAccording to Tontul and Topuz [49] and Tonon Brabet [42]the liquid droplet size during atomization varies directly withthe liquid viscosity at constant atomizer speed resulting inlarger particles Similar results were obtained for differentpowders produced by spray drying such as blackberry juicein maltodextrin Ferrari Germer [50] and coffee oil in arabicgum Frascareli Silva [51]

The increase in inlet drying temperature also resulted in ahigher frequency of particles with sizes above 10 120583m (Figures3(c) and 3(d)) This can be related to increased swellingthereby preventing contraction of the particle as the dryingtemperature increases [50 52]These results are in agreementwith those obtained by Tonon Brabet [42] who evaluated themicroencapsulated acaı pulp inmaltodextrin by spray dryingAccording to the authors slower drying rate ie when theinlet drying temperature is low the particles shrink evenlymaking their size smaller However when the drying rateis higher the rapid evaporation of the water creates a hardcrust in the particle that prevents its contraction in the dryingprocess resulting in larger particles

32 Response Surface Analysis Response surface methodol-ogy (RSM) was performed to optimize spray drying condi-tions considering linear quadratic and interaction effectsbetween independent variables on the microencapsulationof 120573-carotene with arabic gum A second-order polynomialmodel described by (1) was fitted to the experimental datavalues obtained for each response variable studied which arepresented in Table 1 The determination coefficients (R2 andRAdj2) and the linear and quadratic effects of the factorsas well as their interaction for each response variable arepresented in Table 2

The results show that except for the antioxidant activityresponse the mathematical model used was fitted withgood determination coefficients (R2 gt 070) According toLundstedt Seifert [53] values above 07 represent a good fitof the model In addition ANOVA indicated that the lack of

6 International Journal of Food Science

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(a)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(b)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(c)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(d)

Figure 3 Relative frequency (bars) and cumulative frequency (line) equivalent to the diameter of microparticles (a) 94 AG 1232∘C (b)94 AG 1868∘C (c) 5 AG 155∘C (d) 35 AG 155∘C

Table 2 Second-order polynomial equations for each response variable

Equation R2 RAdj2

EE = minus48699 lowast + 03036AG minus 0001AG2 + 0710T lowast minus 0002T2 lowast minus 0003AGT 087 074DY = minus175962 lowast + 4222AG lowast minus 0097AG2 lowast + 2245T lowast minus 0007T2 lowast minus 0004AGT 085 071LC = 56961ndash2808AG lowast + 0069AG2 lowast minus 0257T + 00025T2 lowast minus 00003AGT 091 082AG arabic gum () T temperature (∘C) EE encapsulation efficiency () DY drying yield () LC loading capacity (mg 120573-carotenegminus1particles)lowastAffectingsignificantly the response variable (pgt005)

fit (p gt 005) relative to pure error was not significant at 95of confidence level The expected errors of the models on theprediction of the responses were estimated to be 76 72and 127 for LC EE and DY respectively Figures 4(a) 4(b)and 5 show the 3-dimensional response surfaces that illustratethe effects of arabic gum concentration (AG ) and dryinginlet temperature (T ∘C) on the responses studied

321 Encapsulation Efficiency and Loading Capacity Theencapsulation efficiency values of 120573-carotenewith arabic gum

ranged between 62 and 160 and the loading capacity valuesranged from 119 to 336mg120573-carotenegminus1particles as shownin Table 1 Similar results were found by Rocha Favaro-Trindade [27] uponmicroencapsulation of lycopene inmodi-fied starch that found an EE around 21 and by Botrel Borges[54] who microencapsulated oregano oil using a mixtureof arabic gum maltodextrin and modified starch as wallmaterial by spray drying found an EE between 51 and 339

As seen in Figures 4(a) and 4(b) the increase in dryingtemperature and decrease in arabic gum concentration lead

International Journal of Food Science 7

18

16

14

12

10

8

6

4

200

180

160

140

1205

1015

2025

3035

EncapsulationEffi

ciency ()

Temperature ( ∘C) Arabic gum ()

(a)

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

45

40

35

30

25

20

15

10

Loading Capacity

(mg-caroteneg - 1particles)

(b)

Figure 4 Response surface fitted to (a) encapsulation efficiency and (b) loading capacity as a function of Arabic gum concentration anddrying inlet temperature

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

50

40

30

20

10

0

Drying yield (

)

Figure 5 Response surface fitted to drying yield as a function ofarabic gum concentration and drying

to an increase in the EE Regarding LC higher values wereobserved at both ends of the arabic gum concentrationthat is when the lowest (5) and the highest concentration(35) of the wall material were used In addition when thedrying temperature increased the loading capacity was alsoincreased The same behaviour was reported by Ferrari Ger-mer [50] in microparticles of blackberry using maltodextrinas wall material

According to Jafari Assadpoor [19] the encapsulationefficiency is influenced by the drying conditions emulsion

and bioactive compound characteristics and the wall materialproperties Low encapsulation efficiency value could be dueto 120573-carotene being extremely sensitive to environmentalfactors such as exposure to heat light and oxygen duringencapsulation processing

The experimental data obtained of the encapsulation effi-ciency and loading capacity of the particles were adjusted tothe second-order polynomialmodelwith a satisfactory coeffi-cient of determination (Table 2) Both independent variableshad a significant effect on these responses Arabic gumconcentration had a positive quadratic effect on the loadingcapacity of the microparticles whereas for the encapsulationefficiency arabic gum concentration showed a linear negativeeffect In relation to the drying inlet temperature a positivelinear and quadratic negative effect on the encapsulation effi-ciency and a positive linear effect on the loading capacitywereobserved However the interaction coefficient was found tobe nonsignificant indicating that there was no interactionbetween the independent variables on the EE of particles

The drying temperature is directly proportional to theevaporation rate and inversely proportional to the finalwater content of the dried microparticles At high dryingtemperatures there is a higher evaporation rate of water onthe droplet surface which leads to the rapid formation of asemipermeable membrane resulting in the protection of therelease of the bioactive compounds during the drying processand consequently in a higher bioactive retention Howeverhigher drying temperatures could cause cracks and fissureson the surface of the particles leading to loss of the bioactivecompound [19 21]

Wall material concentration is also a factor that affectsthe retention of the bioactive compounds due to their vis-cosity properties in the feed solution Some researchers have

8 International Journal of Food Science

reported that the wall material concentration has a positiveeffect on the encapsulation efficiency ie the increase ofsolids content in the feed increases bioactive retention [21 5556] This behaviour could be related to the reduction of thetime required to form a surface crust in the atomized dropletsin the initial drying process when the solids concentration inthe feed solution increases This rapidly formed crust is notpermeable to compounds thereby protecting the bioactivefrom oxidation [57 58]

However too high viscosity of the feed solutions delaysthe formation of discrete particles during spray dryingwhereas a low viscosity in feed delays the formation of asemipermeable surface crust favouring further losses of thebioactive compounds [59] Therefore according to Reinec-cius [60] each wall material has its ideal feed concentrationto obtain higher encapsulation efficiency which is basedon the solubility and viscosity of the feed solution In thiswork an ideal arabic gum concentration of 74 was foundfor higher values of encapsulation efficiency and loadingcapacity Fernandes Marques [57] who evaluated the effectof total solids concentration on the microencapsulation ofrosemary essential oil by spray drying using maltodextrinand modified starch (11) as wall materials found higherencapsulation efficiency when a concentration of the wallmaterial of 22 was used which was reported as the idealconcentration for maltodextrin as wall material

322 Drying Yield Drying yield of the spray drying processis directly related to the cost of production and efficiencythus it is an important indicator that the industry considersin its production line [49 61] According to Nunes andMercadante [62] and Rutz Borges [63] drying yield isinfluenced by both the equipment settings (feed rate feedinlet and outlet temperature and flow rate) and dryingconditions (type and wall material concentration)

In this study a second-order model was fitted to theexperimental data of the drying yield with acceptable coef-ficient of determination and Table 2 shows that both inde-pendent variables arabic gum concentration and the dryinginlet temperature had a significant negative quadratic effecton the drying yield According to Table 1 the drying yields of120573-carotene with arabic gum ranged between 159 and 439Other researchers have found values of drying yield around50 Roccia Martınez [64] who studied the microencapsu-lation of the sunflower oil by spray drying using maltodextrinas a carrier agent found drying yield values that ranged from544 to 3988 and Santana Kurozawa [31] produced arabicgum microparticles with pulp pequi extract by spray dryingand obtained a drying yield values between 258 and 561

Low drying yield in the spray drying process is mostlydue to retention of the powder in the drying chamber wallcyclone inefficient in collecting fine particles and the highviscosity of the feed solution This powder retention problemcauses considerable economic loss and it is not cost-effectivefor industry as there would be frequent interruptions tothe dryer cleaning besides affecting the quality of the finalproduct However drying yield in the microencapsulationtechnique could be improved by modifying the spray dryingconditions in order to decrease the adhesion of particles to

the drying chamber wall [64ndash66] According to Tontul andTopuz [49] and Jayasundera Adhikari [67] the mechanicalscraping of the drying chamber wall introduction of coldair from the bottom and the use of low temperature lowhumidity air are some examples of process-based approachesthat could increase drying yield

As shown in Figure 5 as the drying temperature andthe arabic gum concentration increased the drying yieldalso increased until a maximum value was achieved Afterthis value decreases in the drying yield were observed evenwith the increase of both independent variables The highestdrying yield value was found for the sample with 20 GAdried at 155∘C

Chong and Wong [68] also found an optimum dosageof the wall material concentration (30 maltodextrin) andtemperature value (180∘C) that maximized the drying yield(57) when producing sapodilla puree particles by spraydrying using different maltodextrin concentrations (10-50wv) The authors referred that increasing the wall materialconcentration above the optimum value leads to an increaseviscosity of the feed solution thereby negatively affecting thedrying yield

323 Antioxidant Activity The AA values of encapsulated120573-carotene range from 005 to 078 120583mol troloxmgminus1120573-carotene whereas the commercial 120573-carotene before encap-sulation possessed 235 120583mol troloxmgminus1120573-carotene Thelower antioxidant activity after the encapsulation may berelated not only to the encapsulation process itself but alsoto the incomplete extraction of the encapsulated moleculesbefore antioxidant activity measurement This decrease inantioxidant activity after the spray drying process was alsoobserved for example by Franceschinis Salvatori [69] in themicroencapsulation of blackberry juices with maltodextrinand Hee Tan [70] in virgin coconut oil microparticles in amixture of maltodextrin arabic gum sodium caseinate andwhey protein concentrate

The data obtained for the antioxidant activity did notfit the second-order polynomial model though from theresults of Table 1 the two independent variables studiedarabic gum concentration and drying inlet temperatureaffected antioxidant activity of the encapsulated moleculessince an AA increase was observed when the temperaturedecreased (runs 4-3 2-1 and 11-10) and when the arabic gumconcentration increased (runs 1-3 2-4 8-9)

Other researchers have also studied the influence ofdrying inlet temperature and wall material on AA of theparticles Kha Nguyen [71] studied the effects of varyingmaltodextrin concentrations and spray drying temperatureson the antioxidant activity of Gac fruit powder and theyreported that increasing the drying inlet temperature from120 to 200∘C showed a significant loss of AA Additionallywith increasing maltodextrin concentration from 20 to 30the loss of AA was also observed The authors explainedthat AA loss could be due to loss of antioxidant compoundspresent in Gac powder spray dried at high temperaturesMiravet Alacid [72] who evaluated the antioxidant activityof pomegranate juice powder produced by spray dryingusing prebiotic fibers and maltodextrin as wall material also

International Journal of Food Science 9

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

10

08

06

04

02

00

minus02

Desirability

Figure 6 Desirability surface for optimal conditions

observed that the increase of the drying inlet temperaturefrom 160 to 200∘C had a significant negative effect on theantioxidant activity for both wall materials studied

324 Optimization of Drying Process Conditions The desir-ability function was performed for the simultaneous opti-mization of the responses that fitted to the second-ordermodel (Table 2) and the desirability surface for optimalconditions is depicted in Figure 6 Desirability values higherthan 07 were considered indicating a good optimization ofthe experimental data of each response variable [73] Thebest conditions for the spray drying microencapsulation of 120573-carotene with arabic gum as wall material were determined inorder to obtain higher values for drying yield encapsulationefficiency and loading capacity

The inlet drying temperature of 173∘C and arabic gumconcentration of 119 are recommended as the ideal con-ditions for microencapsulation of 120573-carotene Under theseconditions the predicted EE DY and LC are 1562 3630and 2274 mg 120573-carotenegminus1particles respectively

4 Conclusions

Themicroencapsulation of120573-carotene in arabic gumby spraydrying was investigated The arabic gum concentration anddrying inlet temperature influenced the drying yield encap-sulation efficiency and load capacity responses Regardingthe AA the antioxidant activity of 120573-carotene was reducedwhen microencapsulated at high temperatures (200∘C) inrelation to low temperatures (110∘C)

SEM analysis showed that the microparticles are micro-capsules Most of them presented a similar morphology amixture of smooth and wrinkled particles with a diameterlower than 10 120583m Increases in drying temperature favouredthe formation of smoother and larger particles

From the experimental conditions the drying inlet tem-perature of 173∘C and the arabic gum concentration of 119

were those that allow obtaining higher 120573-carotene contenthigher encapsulation efficiency and higher drying yield

The systematic approach used for the study of 120573-carotenemicroencapsulation process by spray drying may be easilyapplied for other core and wall materials Further studies willfocus on release studies in several aqueous media and even-tually on the encapsulation of natural carotenoid extracts

Data Availability

The data used to support the findings of this study areincluded within the article

Conflicts of Interest

The authors declare that they have no conflicts of interest

Acknowledgments

This work was supported by Conselho Nacional de Desen-volvimento Cientıfico e TecnologicondashCNPq through theCiencia sem Fronteiras program (CSF) (Grant CSF 2062682014-9 to first author)The authors acknowledge the financialsupport from Fundacao para a Ciencia e a TecnologiaPortugal Project UIDAGR041292013

References

[1] M E Rodrıguez-Huezo R Pedroza-Islas L A Prado-Bar-ragan C I Beristain and E J Vernon-Carter ldquoMicroencapsu-lation by spray drying of multiple emulsions containing caro-tenoidsrdquo Journal of Food Science vol 69 no 7 pp 351ndash359 2004

[2] A V Rao and L G Rao ldquoCarotenoids and human healthrdquoPharmacological Research vol 55 no 3 pp 207ndash216 2007

[3] J Fiedor and K Burda ldquoPotential role of carotenoids as anti-oxidants in human health and diseaserdquo Nutrients vol 6 no 2pp 466ndash488 2014

[4] R Arimboor R B Natarajan K R Menon L P Chan-drasekhar and VMoorkoth ldquoRed pepper (Capsicum annuum)carotenoids as a source of natural food colors analysis andstabilitymdasha reviewrdquo Journal of Food Science and Technology vol52 no 3 pp 1258ndash1271 2015

[5] M H Walter and D Strack ldquoCarotenoids and their cleavageproducts Biosynthesis and functionsrdquoNatural Product Reportsvol 28 no 4 pp 663ndash692 2011

[6] A Kaczor M Baranska and K Czamara Carotenoids WileyOnline Library 2016

[7] A F Aissa M L P Bianchi J C Ribeiro et al ldquoComparativestudy of 120573-carotene and microencapsulated 120573-carotene Eval-uation of their genotoxic and antigenotoxic effectsrdquo Food andChemical Toxicology vol 50 no 5 pp 1418ndash1424 2012

[8] Z Al Tanoury A Piskunov and C Rochette-Egly ldquoVitamina and retinoid signaling Genomic and nongenomic effectsrdquoJournal of Lipid Research vol 54 no 7 pp 1761ndash1775 2013

[9] E G Donhowe F P Flores W L Kerr L Wicker and F KongldquoCharacterization and invitro bioavailability of 120573-caroteneEffects of microencapsulation method and food matrixrdquo LWT-Food Science and Technology vol 57 no 1 pp 42ndash48 2014

[10] K Gul A Tak A Singh et al ldquoChemistry encapsulation andhealth benefits of szlig-carotene-A reviewrdquo Cogent Food amp Agri-culture vol 1 no 1 Article ID 1018696 2015

10 International Journal of Food Science

[11] HW Kim J B Kim S Poovan et al ldquoEffect of processing con-ditions on the content of cistrans carotene isomers as provita-min A carotenoids in Korean sweet potato varietiesrdquo Interna-tional Journal of Food Sciences and Nutrition vol 65 no 7 pp821ndash826 2014

[12] C Qian E A Decker H Xiao and D J McClements ldquoNano-emulsion delivery systems Influence of carrier oil on 120573-caro-tene bioaccessibilityrdquo Food Chemistry vol 135 no 3 pp 1440ndash1447 2012

[13] J C Spada L D F Marczak I C Tessaro and C P Z NorenaldquoMicroencapsulation of 120573-carotene using native pinhao starchmodified pinhao starch and gelatin by freeze-dryingrdquo Interna-tional Journal of Food Science amp Technology vol 47 no 1 pp186ndash194 2012

[14] G Zakynthinos and T Varzakas ldquoCarotenoids From plants tofood industryrdquo Current Research in Nutrition and Food Sciencevol 4 no 1 pp 38ndash51 2016

[15] R Liang Q Huang J Ma C F Shoemaker and F ZhongldquoEffect of relative humidity on the store stability of spray-driedbeta-carotene nanoemulsionsrdquo Food Hydrocolloids vol 33 no2 pp 225ndash233 2013

[16] C Saenz S Tapia J Chavez and P Robert ldquoMicroencapsula-tion by spray drying of bioactive compounds from cactus pear(Opuntia ficus-indica)rdquo Food Chemistry vol 114 no 2 pp 616ndash622 2009

[17] S AkhavanMahdavi SM Jafari E Assadpoor andDDehnadldquoMicroencapsulation optimization of natural anthocyaninswith maltodextrin gum Arabic and gelatinrdquo InternationalJournal of Biological Macromolecules vol 85 pp 379ndash385 2016

[18] N V N Jyothi P M Prasanna S N Sakarkar K S PrabhaP S Ramaiah and G Y Srawan ldquoMicroencapsulation tech-niques factors influencing encapsulation efficiencyrdquo Journal ofMicroencapsulation vol 27 no 3 pp 187ndash197 2010

[19] S M Jafari E Assadpoor Y He and B Bhandari ldquoEncapsu-lation efficiency of food flavours and oils during spray dryingrdquoDrying Technology vol 26 no 7 pp 816ndash835 2008

[20] S C Samantha A S Bruna R M Adriana B Fabio A RSandro and R C Aline ldquoDrying by spray drying in the foodindustry Micro-encapsulation process parameters and maincarriers usedrdquo African Journal of Food Science vol 9 no 9 pp462ndash470 2015

[21] T C Kha M H Nguyen P D Roach and C E StathopoulosldquoMicroencapsulation of Gac oil Optimisation of spray dryingconditions using response surface methodologyrdquo Powder Tech-nology vol 264 pp 298ndash309 2014

[22] E Janiszewska-Turak ldquoCarotenoids microencapsulation byspray drying method and supercritical micronizationrdquo FoodResearch International vol 99 pp 891ndash901 2017

[23] A Goncalves B N Estevinho and F Rocha ldquoDesign andcharacterization of controlled-release vitamin A microparticlesprepared by a spray-drying processrdquo Powder Technology vol305 pp 411ndash417 2017

[24] MOrdonez and AHerrera ldquoMorphologic and stability cassavastarch matrices for encapsulating limonene by spray dryingrdquoPowder Technology vol 253 pp 89ndash97 2014

[25] S-M Jafari K Mahdavi-Khazaei and A Hemmati-KakhkildquoMicroencapsulation of saffron petal anthocyanins with cressseed gum compared with Arabic gum through freeze dryingrdquoCarbohydrate Polymers vol 140 pp 20ndash25 2016

[26] M P Rascon C I Beristain H S Garcıa and M A Sal-gado ldquoCarotenoid retention and storage stability of spray-dried encapsulated paprika oleoresin using gum Arabic and

Soy protein isolate as wall materialsrdquo LWT- Food Science andTechnology vol 44 no 2 pp 549ndash557 2011

[27] GA Rocha C S Favaro-Trindade andC R F Grosso ldquoMicro-encapsulation of lycopene by spray drying Characterizationstability and application of microcapsulesrdquo Food and Bioprod-ucts Processing vol 90 no 1 pp 37ndash42 2012

[28] Q Shen and S Y Quek ldquoMicroencapsulation of astaxanthinwith blends of milk protein and fiber by spray dryingrdquo Journalof Food Engineering vol 123 pp 165ndash171 2014

[29] A M Goula and K G Adamopoulos ldquoA new technique forspray-dried encapsulation of lycopenerdquoDrying Technology vol30 no 6 pp 641ndash652 2012

[30] J Loksuwan ldquoCharacteristics of microencapsulated 120573-caroteneformed by spray drying with modified tapioca starch nativetapioca starch andmaltodextrinrdquoFoodHydrocolloids vol 21 no5-6 pp 928ndash935 2007

[31] A A Santana L E Kurozawa R A de Oliveira and K JPark ldquoInfluence of Process Conditions on the PhysicochemicalProperties of Pequi Powder Produced by Spray Dryingrdquo DryingTechnology vol 31 no 7 pp 825ndash836 2013

[32] D Troya D S Tupuna-Yerovi and J Ruales ldquoEffects of WallMaterials and Operating Parameters on Physicochemical Pro-perties Process Efficiency and Total Carotenoid Content ofMicroencapsulated Banana Passionfruit Pulp (Passiflora tri-partita var mollissima) by Spray-Dryingrdquo Food and BioprocessTechnology vol 11 no 10 pp 1828ndash1839 2018

[33] D C Montgomery Design and Analysis of Experiments JohnWiley amp Sons 8th edition 2012

[34] M do S M Rufino R Alves E de Brito et al MetodologiaCientıfica Determinacao da Atividade Antioxidante Total emFrutas pela Captura do Radical Livre ABTS ComunicadoTecnico (Embrapa Agroindustria Tropical Online) 2007

[35] N Nenadis L-F Wang M Tsimidou and H-Y Zhang ldquoEsti-mation of scavenging activity of phenolic compounds using theABTS∙+ assayrdquo Journal of Agricultural and Food Chemistry vol52 no 15 pp 4669ndash4674 2004

[36] C A Di Battista D ConstenlaM V Ramırez-Rigo and J PinaldquoThe use of Arabic gum maltodextrin and surfactants in themicroencapsulation of phytosterols by spray dryingrdquo PowderTechnology vol 286 pp 193ndash201 2015

[37] C A Schneider W S Rasband and K W Eliceiri ldquoNIH Imageto ImageJ 25 years of image analysisrdquo Nature Methods vol 9no 7 pp 671ndash675 2012

[38] S Shamaei S S Seiiedlou M Aghbashlo E Tsotsas and AKharaghani ldquoMicroencapsulation of walnut oil by spray dry-ing effects of wall material and drying conditions on physico-chemical properties of microcapsulesrdquo Innovative Food Scienceand Emerging Technologies vol 39 pp 101ndash112 2017

[39] L Medina-Torres R Santiago-Adame F Calderas et alldquoMicroencapsulation by spray drying of laurel infusions (Litseaglaucescens) with maltodextrinrdquo Industrial Crops and Productsvol 90 pp 1ndash8 2016

[40] S Beirao-da-Costa C Duarte A I Bourbon et al ldquoInulinpotential for encapsulation and controlled delivery of Oreganoessential oilrdquo Food Hydrocolloids vol 33 no 2 pp 199ndash2062013

[41] R Santiago-Adame L Medina-Torres J A Gallegos-Infante etal ldquoSpray drying-microencapsulation of cinnamon infusions(Cinnamomum zeylanicum) with maltodextrinrdquo LWT- FoodScience and Technology vol 64 no 2 pp 571ndash577 2015

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

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Page 3: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

International Journal of Food Science 3

Table 1 Experimental design with coded and decoded values of independent variables and spray drying responses

Run Independent variables Responses variablesArabic gum () T LC EE AA DY

1 94 (-1) 1232 (-1) 219 99 053 2252 94 (-1) 1868 (+1) 273 147 011 2693 306 (+1) 1232 (-1) 244 80 078 1634 306 (+1) 1868 (+1) 294 92 024 1595 20 (0) 155 (0) 159 139 022 4396 20 (0) 155 (0) 140 125 027 4027 20 (0) 155 (0) 167 138 017 4138 5 (-120572) 155 (0) 336 160 005 2389 35 (120572) 155 (0) 264 122 030 23210 20 (0) 110 (-120572) 119 62 036 28611 20 (0) 200(+120572) 214 148 012 343T temperature (∘C) LC loading capacity (mg 120573-carotenegminus1particles) EE encapsulation efficiency () AA antioxidant activity (120583mol troloxmgminus1120573-carotene) DY drying yield ()

where Yi corresponds to the response variables X1 and X2represent the coded independent variables (arabic gum con-centration and drying inlet temperature respectively) b0 isthe interception bi bj bij (i j = 1 2) are the linear quadraticand interaction coefficients respectively The adequacy of themodel to the experimental data was verified by applying theanalysis of variance (ANOVA) and coefficient of determina-tion (R2) and adjusted R2 (R2 adj) [33]The statistical analysiswas carried out using the software ldquoStatisticTMrdquo version 7(Statsoft USA)

The optimum conditions for the microencapsulation of120573-carotene were determined considering the results of theresponse variables that were significantly affected by spraydrying conditions using the desirability function

24 AntioxidantActivity beforeMicroencapsulation The totalantioxidant activity of samples was performed by radicalscavenging activity assessment expressed as Trolox Equiva-lentAntioxidantActivity (TEAC) described by do SMRufinoAlves [34] andNenadis Wang [35] with slightmodificationsAn ABTS stock solution was prepared by dissolving ABTSin water at a 7 mM concentration ABTS+ solution wasproduced by reaction of 5 mL of ABTS stock solution and88 120583L of a 140 mM potassium persulfate (K2S2O8) solutionto give a final concentration of 245 mM This solution waskept in a dark room at room temperature for 12-16 h Beforeanalysis ABTS+ solution was diluted with ethanol to obtainan initial absorbance value of 070 plusmn005 at 734 nm

For the evaluation of the antioxidant activity of 120573-carotene itself a volume of 30 120583L of diluted 120573-carotene withethanol was mixed with 3000 120583L of ABTS+ solution followedby incubation for 6min in the darkThen the absorbance wasmeasured in a spectrophotometer (Unicam UVVis Spec-trometer ndash UV4) at a wavelength of 734 nm A calibrationcurve was performed using Trolox as standard antioxidantat the concentration range of 250-2000 120583M in ethanol Allanalytical measurements were carried out in triplicate

25 Spray Drying and Microparticlesrsquo Characterization

251 Drying Yield Drying yield (DY) was determined gravi-metrically as described by Di Battista Constenla [36] as theratio of the mass of microparticles collected at the end of thespray drying process and the mass of solids contained in thefeed solutions

252 Morphological Characterization of Microparticles Themorphology of the particles obtained by spray drying wasobserved by scanning electron microscopy (SEM) The sam-ples were coated with a mixture of gold (80) and palladium(20) in a vacuum chamber and analysed using a HitachiS2400 scanning microscope operated at 15kV with differentmagnifications (500x to 2000x) Particles size was measuredby analysing SEM images using the image processing softwareImageJ (National Institute of Health USA) [37]

253 Loading Capacity and Encapsulation Efficiency For thedetermination of the concentration of the 120573-carotene presentin the microparticles (LC) the method described by RochaFavaro-Trindade [27] was used with some modifications Amass of 10 mg of microparticles was added to 50 ml ofethanol The suspension was homogenized with an Ultra-Turrax T25 (IKA Germany) at 13500 rpm during 3 min inorder to break the particles Aftermixing the suspension wasplaced in amber glass flasks and kept away from light forabout 12 h at 5∘C Afterwards the suspension was centrifuged(HERMLE Labortechnik Z 383 K) at 10000 rpm during10 min at 8∘C in order to recover the supernatant Theconcentration of 120573-carotene in the liquid phase (supernatant)was quantified in a spectrophotometer (Unicam UVVisSpectrometer UV4) at a wavelength of 450 nm A calibrationcurve was performed with 120573-carotene diluted in ethanolwith different concentrations (05-10 mgLminus1) The loadingcapacity (LC) of the particles was expressed as the mass of120573-carotene per mass of particles

4 International Journal of Food Science

(a) (b) (c)

(d) (e) (f)

(g) (h) (i)

Figure 1 Scanning electron microscopy (SEM) images (magnification x500) of arabic gum microparticles with microencapsulated 120573-carotene (a) 94 AG 1232∘C (b) 94 AG 1868∘C (c) 306 AG 1232∘C (d) 306 AG 1868∘C (e) 20 AG 155∘C (f) 5 AG 155∘C(g) 35 AG 155∘C (h) 20 AG 110∘C (i) 20 AG 200∘C

The encapsulation efficiency (EE) was calculated as byRocha Favaro-Trindade [27] quantifying the ratio betweenthe mass of 120573-carotene present in the microparticles and the120573-carotenersquo mass initially present in the feed solution

254 Antioxidant Activity of the Encapsulated Material Forthe measurement of the antioxidant activity (AA) of theencapsulated molecules the microparticles core materialswere previously extracted with ethanol as described in theprevious section Afterwards a volume of 800 120583L of super-natant was mixed with 2200 120583L of ABTS+ solution followedby the steps described in Section 24 for pure 120573-carotene

3 Results and Discussion

31 Microparticle Morphology and Size Distribution Themorphological characteristics of the obtained arabic gummicroparticles with 120573-carotene were investigated using SEMSEM images have shown that the particles maintain a similar

spherical-like shape with a smooth or wrinkled surfacedepending on the drying conditions (Figure 1)

Most of the particles did not present a significant inci-dence of cracks or fissures in the outer surface indicating aresistant external physical structureMicroparticles producedwithout apparent damage have a lower gas permeabilitypresenting a more effective protection of the bioactive com-pounds from oxidation reactions and avoiding their unde-sired release [38]

Higher drying inlet temperatures tend to produce parti-cles with a smoother surface and with a low degree of teethand concavities (Figures 1(a) 1(b) 1(c) 1(d) 1(h) and 1(i))This fact may be attributed to rapid water evaporation andhigher pressure inside the particles during microencapsula-tion at higher temperatures preventing shrinking [39] On theother hand water diffusion is slower at lower temperaturesallowing more time for the particles to deform wrinkleand collapse [40] Similar results were reported by Santiago-Adame Medina-Torres [41] for microparticles of cinnamon

International Journal of Food Science 5

(a) (b)

Figure 2 Scanning electron microscopy (SEM) images (magnification x2000) of the internal surface of Arabic gum microparticles with120573-carotene microencapsulated (a) 20 AG 110∘C (b) 94 AG 1232∘C

infusions with maltodextrin in which the effect of threedifferent drying temperatures (140 160 and 180∘C) wasevaluated They found microparticles morphologically moredefined and smoother without evident cracks or particleagglomerations in the spray drying process both at 160 and180∘C

At the contrary Figures 1(a) and 1(c) 1(b) and 1(d)and 1(e) and 1(f) show that the different values of arabicgum concentration studied did not influence substantially theparticles morphology as mixtures with a similar proportionof smooth and collapsed particles were obtained GoncalvesEstevinho [23] and Tonon Brabet [42] also found no influ-ence of the wall material concentration on the morphology ofthe particles obtained in themicroencapsulation of vitamin Awith arabic gum and acaı pulp with maltodextrin

The internal morphology is shown in Figure 2 Allmicroparticles obtained were shown to be microcapsulesenvisaging that the core material (120573-carotene) was entrappedwithin the wall or in the centre Central void formation acharacteristic of the spray drying process is related to theexpansion of the particles during the latter stages of thedrying process when the temperature exceeds the boilingpoint of the water [43 44] This internal structure of themicroparticles was also observed in microencapsulated soy-bean extract microencapsulated by spray drying in arabicgum or maltodextrin matrix [45] as well as in gelatinarabicgummicroparticles loaded with fish oil [46]

Particle size distribution is a physical parameter of thepowders which may influence their properties involvinghandling transport and storage such as bulk density angleof repose flowability rehydration capacity solubility anddispersibility [17 47] According toOnwulata [48] and Tontuland Topuz [49] the stability of the functional componentssensitive to environmental conditions is also affected by theparticle size

The particle size of 120573-carotene loaded arabic gummicro-capsules ranged from 182 to 4091 120583m In Figure 3 theparticle size distribution of the microcapsules produced atdifferent temperatures is shown (at 1232 and 1868∘C) andwith different arabic gum concentrations (5 and 35) In allcases more than 80 of the particles had a size below 10 120583m

In general a higher frequency of particles with sizesabove 10 120583m was observed with increasing arabic gumconcentration (Figures 3(a) and 3(b))This factmay be relatedto the higher viscosity of the spray drying feed solutionAccording to Tontul and Topuz [49] and Tonon Brabet [42]the liquid droplet size during atomization varies directly withthe liquid viscosity at constant atomizer speed resulting inlarger particles Similar results were obtained for differentpowders produced by spray drying such as blackberry juicein maltodextrin Ferrari Germer [50] and coffee oil in arabicgum Frascareli Silva [51]

The increase in inlet drying temperature also resulted in ahigher frequency of particles with sizes above 10 120583m (Figures3(c) and 3(d)) This can be related to increased swellingthereby preventing contraction of the particle as the dryingtemperature increases [50 52]These results are in agreementwith those obtained by Tonon Brabet [42] who evaluated themicroencapsulated acaı pulp inmaltodextrin by spray dryingAccording to the authors slower drying rate ie when theinlet drying temperature is low the particles shrink evenlymaking their size smaller However when the drying rateis higher the rapid evaporation of the water creates a hardcrust in the particle that prevents its contraction in the dryingprocess resulting in larger particles

32 Response Surface Analysis Response surface methodol-ogy (RSM) was performed to optimize spray drying condi-tions considering linear quadratic and interaction effectsbetween independent variables on the microencapsulationof 120573-carotene with arabic gum A second-order polynomialmodel described by (1) was fitted to the experimental datavalues obtained for each response variable studied which arepresented in Table 1 The determination coefficients (R2 andRAdj2) and the linear and quadratic effects of the factorsas well as their interaction for each response variable arepresented in Table 2

The results show that except for the antioxidant activityresponse the mathematical model used was fitted withgood determination coefficients (R2 gt 070) According toLundstedt Seifert [53] values above 07 represent a good fitof the model In addition ANOVA indicated that the lack of

6 International Journal of Food Science

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(a)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(b)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(c)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(d)

Figure 3 Relative frequency (bars) and cumulative frequency (line) equivalent to the diameter of microparticles (a) 94 AG 1232∘C (b)94 AG 1868∘C (c) 5 AG 155∘C (d) 35 AG 155∘C

Table 2 Second-order polynomial equations for each response variable

Equation R2 RAdj2

EE = minus48699 lowast + 03036AG minus 0001AG2 + 0710T lowast minus 0002T2 lowast minus 0003AGT 087 074DY = minus175962 lowast + 4222AG lowast minus 0097AG2 lowast + 2245T lowast minus 0007T2 lowast minus 0004AGT 085 071LC = 56961ndash2808AG lowast + 0069AG2 lowast minus 0257T + 00025T2 lowast minus 00003AGT 091 082AG arabic gum () T temperature (∘C) EE encapsulation efficiency () DY drying yield () LC loading capacity (mg 120573-carotenegminus1particles)lowastAffectingsignificantly the response variable (pgt005)

fit (p gt 005) relative to pure error was not significant at 95of confidence level The expected errors of the models on theprediction of the responses were estimated to be 76 72and 127 for LC EE and DY respectively Figures 4(a) 4(b)and 5 show the 3-dimensional response surfaces that illustratethe effects of arabic gum concentration (AG ) and dryinginlet temperature (T ∘C) on the responses studied

321 Encapsulation Efficiency and Loading Capacity Theencapsulation efficiency values of 120573-carotenewith arabic gum

ranged between 62 and 160 and the loading capacity valuesranged from 119 to 336mg120573-carotenegminus1particles as shownin Table 1 Similar results were found by Rocha Favaro-Trindade [27] uponmicroencapsulation of lycopene inmodi-fied starch that found an EE around 21 and by Botrel Borges[54] who microencapsulated oregano oil using a mixtureof arabic gum maltodextrin and modified starch as wallmaterial by spray drying found an EE between 51 and 339

As seen in Figures 4(a) and 4(b) the increase in dryingtemperature and decrease in arabic gum concentration lead

International Journal of Food Science 7

18

16

14

12

10

8

6

4

200

180

160

140

1205

1015

2025

3035

EncapsulationEffi

ciency ()

Temperature ( ∘C) Arabic gum ()

(a)

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

45

40

35

30

25

20

15

10

Loading Capacity

(mg-caroteneg - 1particles)

(b)

Figure 4 Response surface fitted to (a) encapsulation efficiency and (b) loading capacity as a function of Arabic gum concentration anddrying inlet temperature

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

50

40

30

20

10

0

Drying yield (

)

Figure 5 Response surface fitted to drying yield as a function ofarabic gum concentration and drying

to an increase in the EE Regarding LC higher values wereobserved at both ends of the arabic gum concentrationthat is when the lowest (5) and the highest concentration(35) of the wall material were used In addition when thedrying temperature increased the loading capacity was alsoincreased The same behaviour was reported by Ferrari Ger-mer [50] in microparticles of blackberry using maltodextrinas wall material

According to Jafari Assadpoor [19] the encapsulationefficiency is influenced by the drying conditions emulsion

and bioactive compound characteristics and the wall materialproperties Low encapsulation efficiency value could be dueto 120573-carotene being extremely sensitive to environmentalfactors such as exposure to heat light and oxygen duringencapsulation processing

The experimental data obtained of the encapsulation effi-ciency and loading capacity of the particles were adjusted tothe second-order polynomialmodelwith a satisfactory coeffi-cient of determination (Table 2) Both independent variableshad a significant effect on these responses Arabic gumconcentration had a positive quadratic effect on the loadingcapacity of the microparticles whereas for the encapsulationefficiency arabic gum concentration showed a linear negativeeffect In relation to the drying inlet temperature a positivelinear and quadratic negative effect on the encapsulation effi-ciency and a positive linear effect on the loading capacitywereobserved However the interaction coefficient was found tobe nonsignificant indicating that there was no interactionbetween the independent variables on the EE of particles

The drying temperature is directly proportional to theevaporation rate and inversely proportional to the finalwater content of the dried microparticles At high dryingtemperatures there is a higher evaporation rate of water onthe droplet surface which leads to the rapid formation of asemipermeable membrane resulting in the protection of therelease of the bioactive compounds during the drying processand consequently in a higher bioactive retention Howeverhigher drying temperatures could cause cracks and fissureson the surface of the particles leading to loss of the bioactivecompound [19 21]

Wall material concentration is also a factor that affectsthe retention of the bioactive compounds due to their vis-cosity properties in the feed solution Some researchers have

8 International Journal of Food Science

reported that the wall material concentration has a positiveeffect on the encapsulation efficiency ie the increase ofsolids content in the feed increases bioactive retention [21 5556] This behaviour could be related to the reduction of thetime required to form a surface crust in the atomized dropletsin the initial drying process when the solids concentration inthe feed solution increases This rapidly formed crust is notpermeable to compounds thereby protecting the bioactivefrom oxidation [57 58]

However too high viscosity of the feed solutions delaysthe formation of discrete particles during spray dryingwhereas a low viscosity in feed delays the formation of asemipermeable surface crust favouring further losses of thebioactive compounds [59] Therefore according to Reinec-cius [60] each wall material has its ideal feed concentrationto obtain higher encapsulation efficiency which is basedon the solubility and viscosity of the feed solution In thiswork an ideal arabic gum concentration of 74 was foundfor higher values of encapsulation efficiency and loadingcapacity Fernandes Marques [57] who evaluated the effectof total solids concentration on the microencapsulation ofrosemary essential oil by spray drying using maltodextrinand modified starch (11) as wall materials found higherencapsulation efficiency when a concentration of the wallmaterial of 22 was used which was reported as the idealconcentration for maltodextrin as wall material

322 Drying Yield Drying yield of the spray drying processis directly related to the cost of production and efficiencythus it is an important indicator that the industry considersin its production line [49 61] According to Nunes andMercadante [62] and Rutz Borges [63] drying yield isinfluenced by both the equipment settings (feed rate feedinlet and outlet temperature and flow rate) and dryingconditions (type and wall material concentration)

In this study a second-order model was fitted to theexperimental data of the drying yield with acceptable coef-ficient of determination and Table 2 shows that both inde-pendent variables arabic gum concentration and the dryinginlet temperature had a significant negative quadratic effecton the drying yield According to Table 1 the drying yields of120573-carotene with arabic gum ranged between 159 and 439Other researchers have found values of drying yield around50 Roccia Martınez [64] who studied the microencapsu-lation of the sunflower oil by spray drying using maltodextrinas a carrier agent found drying yield values that ranged from544 to 3988 and Santana Kurozawa [31] produced arabicgum microparticles with pulp pequi extract by spray dryingand obtained a drying yield values between 258 and 561

Low drying yield in the spray drying process is mostlydue to retention of the powder in the drying chamber wallcyclone inefficient in collecting fine particles and the highviscosity of the feed solution This powder retention problemcauses considerable economic loss and it is not cost-effectivefor industry as there would be frequent interruptions tothe dryer cleaning besides affecting the quality of the finalproduct However drying yield in the microencapsulationtechnique could be improved by modifying the spray dryingconditions in order to decrease the adhesion of particles to

the drying chamber wall [64ndash66] According to Tontul andTopuz [49] and Jayasundera Adhikari [67] the mechanicalscraping of the drying chamber wall introduction of coldair from the bottom and the use of low temperature lowhumidity air are some examples of process-based approachesthat could increase drying yield

As shown in Figure 5 as the drying temperature andthe arabic gum concentration increased the drying yieldalso increased until a maximum value was achieved Afterthis value decreases in the drying yield were observed evenwith the increase of both independent variables The highestdrying yield value was found for the sample with 20 GAdried at 155∘C

Chong and Wong [68] also found an optimum dosageof the wall material concentration (30 maltodextrin) andtemperature value (180∘C) that maximized the drying yield(57) when producing sapodilla puree particles by spraydrying using different maltodextrin concentrations (10-50wv) The authors referred that increasing the wall materialconcentration above the optimum value leads to an increaseviscosity of the feed solution thereby negatively affecting thedrying yield

323 Antioxidant Activity The AA values of encapsulated120573-carotene range from 005 to 078 120583mol troloxmgminus1120573-carotene whereas the commercial 120573-carotene before encap-sulation possessed 235 120583mol troloxmgminus1120573-carotene Thelower antioxidant activity after the encapsulation may berelated not only to the encapsulation process itself but alsoto the incomplete extraction of the encapsulated moleculesbefore antioxidant activity measurement This decrease inantioxidant activity after the spray drying process was alsoobserved for example by Franceschinis Salvatori [69] in themicroencapsulation of blackberry juices with maltodextrinand Hee Tan [70] in virgin coconut oil microparticles in amixture of maltodextrin arabic gum sodium caseinate andwhey protein concentrate

The data obtained for the antioxidant activity did notfit the second-order polynomial model though from theresults of Table 1 the two independent variables studiedarabic gum concentration and drying inlet temperatureaffected antioxidant activity of the encapsulated moleculessince an AA increase was observed when the temperaturedecreased (runs 4-3 2-1 and 11-10) and when the arabic gumconcentration increased (runs 1-3 2-4 8-9)

Other researchers have also studied the influence ofdrying inlet temperature and wall material on AA of theparticles Kha Nguyen [71] studied the effects of varyingmaltodextrin concentrations and spray drying temperatureson the antioxidant activity of Gac fruit powder and theyreported that increasing the drying inlet temperature from120 to 200∘C showed a significant loss of AA Additionallywith increasing maltodextrin concentration from 20 to 30the loss of AA was also observed The authors explainedthat AA loss could be due to loss of antioxidant compoundspresent in Gac powder spray dried at high temperaturesMiravet Alacid [72] who evaluated the antioxidant activityof pomegranate juice powder produced by spray dryingusing prebiotic fibers and maltodextrin as wall material also

International Journal of Food Science 9

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

10

08

06

04

02

00

minus02

Desirability

Figure 6 Desirability surface for optimal conditions

observed that the increase of the drying inlet temperaturefrom 160 to 200∘C had a significant negative effect on theantioxidant activity for both wall materials studied

324 Optimization of Drying Process Conditions The desir-ability function was performed for the simultaneous opti-mization of the responses that fitted to the second-ordermodel (Table 2) and the desirability surface for optimalconditions is depicted in Figure 6 Desirability values higherthan 07 were considered indicating a good optimization ofthe experimental data of each response variable [73] Thebest conditions for the spray drying microencapsulation of 120573-carotene with arabic gum as wall material were determined inorder to obtain higher values for drying yield encapsulationefficiency and loading capacity

The inlet drying temperature of 173∘C and arabic gumconcentration of 119 are recommended as the ideal con-ditions for microencapsulation of 120573-carotene Under theseconditions the predicted EE DY and LC are 1562 3630and 2274 mg 120573-carotenegminus1particles respectively

4 Conclusions

Themicroencapsulation of120573-carotene in arabic gumby spraydrying was investigated The arabic gum concentration anddrying inlet temperature influenced the drying yield encap-sulation efficiency and load capacity responses Regardingthe AA the antioxidant activity of 120573-carotene was reducedwhen microencapsulated at high temperatures (200∘C) inrelation to low temperatures (110∘C)

SEM analysis showed that the microparticles are micro-capsules Most of them presented a similar morphology amixture of smooth and wrinkled particles with a diameterlower than 10 120583m Increases in drying temperature favouredthe formation of smoother and larger particles

From the experimental conditions the drying inlet tem-perature of 173∘C and the arabic gum concentration of 119

were those that allow obtaining higher 120573-carotene contenthigher encapsulation efficiency and higher drying yield

The systematic approach used for the study of 120573-carotenemicroencapsulation process by spray drying may be easilyapplied for other core and wall materials Further studies willfocus on release studies in several aqueous media and even-tually on the encapsulation of natural carotenoid extracts

Data Availability

The data used to support the findings of this study areincluded within the article

Conflicts of Interest

The authors declare that they have no conflicts of interest

Acknowledgments

This work was supported by Conselho Nacional de Desen-volvimento Cientıfico e TecnologicondashCNPq through theCiencia sem Fronteiras program (CSF) (Grant CSF 2062682014-9 to first author)The authors acknowledge the financialsupport from Fundacao para a Ciencia e a TecnologiaPortugal Project UIDAGR041292013

References

[1] M E Rodrıguez-Huezo R Pedroza-Islas L A Prado-Bar-ragan C I Beristain and E J Vernon-Carter ldquoMicroencapsu-lation by spray drying of multiple emulsions containing caro-tenoidsrdquo Journal of Food Science vol 69 no 7 pp 351ndash359 2004

[2] A V Rao and L G Rao ldquoCarotenoids and human healthrdquoPharmacological Research vol 55 no 3 pp 207ndash216 2007

[3] J Fiedor and K Burda ldquoPotential role of carotenoids as anti-oxidants in human health and diseaserdquo Nutrients vol 6 no 2pp 466ndash488 2014

[4] R Arimboor R B Natarajan K R Menon L P Chan-drasekhar and VMoorkoth ldquoRed pepper (Capsicum annuum)carotenoids as a source of natural food colors analysis andstabilitymdasha reviewrdquo Journal of Food Science and Technology vol52 no 3 pp 1258ndash1271 2015

[5] M H Walter and D Strack ldquoCarotenoids and their cleavageproducts Biosynthesis and functionsrdquoNatural Product Reportsvol 28 no 4 pp 663ndash692 2011

[6] A Kaczor M Baranska and K Czamara Carotenoids WileyOnline Library 2016

[7] A F Aissa M L P Bianchi J C Ribeiro et al ldquoComparativestudy of 120573-carotene and microencapsulated 120573-carotene Eval-uation of their genotoxic and antigenotoxic effectsrdquo Food andChemical Toxicology vol 50 no 5 pp 1418ndash1424 2012

[8] Z Al Tanoury A Piskunov and C Rochette-Egly ldquoVitamina and retinoid signaling Genomic and nongenomic effectsrdquoJournal of Lipid Research vol 54 no 7 pp 1761ndash1775 2013

[9] E G Donhowe F P Flores W L Kerr L Wicker and F KongldquoCharacterization and invitro bioavailability of 120573-caroteneEffects of microencapsulation method and food matrixrdquo LWT-Food Science and Technology vol 57 no 1 pp 42ndash48 2014

[10] K Gul A Tak A Singh et al ldquoChemistry encapsulation andhealth benefits of szlig-carotene-A reviewrdquo Cogent Food amp Agri-culture vol 1 no 1 Article ID 1018696 2015

10 International Journal of Food Science

[11] HW Kim J B Kim S Poovan et al ldquoEffect of processing con-ditions on the content of cistrans carotene isomers as provita-min A carotenoids in Korean sweet potato varietiesrdquo Interna-tional Journal of Food Sciences and Nutrition vol 65 no 7 pp821ndash826 2014

[12] C Qian E A Decker H Xiao and D J McClements ldquoNano-emulsion delivery systems Influence of carrier oil on 120573-caro-tene bioaccessibilityrdquo Food Chemistry vol 135 no 3 pp 1440ndash1447 2012

[13] J C Spada L D F Marczak I C Tessaro and C P Z NorenaldquoMicroencapsulation of 120573-carotene using native pinhao starchmodified pinhao starch and gelatin by freeze-dryingrdquo Interna-tional Journal of Food Science amp Technology vol 47 no 1 pp186ndash194 2012

[14] G Zakynthinos and T Varzakas ldquoCarotenoids From plants tofood industryrdquo Current Research in Nutrition and Food Sciencevol 4 no 1 pp 38ndash51 2016

[15] R Liang Q Huang J Ma C F Shoemaker and F ZhongldquoEffect of relative humidity on the store stability of spray-driedbeta-carotene nanoemulsionsrdquo Food Hydrocolloids vol 33 no2 pp 225ndash233 2013

[16] C Saenz S Tapia J Chavez and P Robert ldquoMicroencapsula-tion by spray drying of bioactive compounds from cactus pear(Opuntia ficus-indica)rdquo Food Chemistry vol 114 no 2 pp 616ndash622 2009

[17] S AkhavanMahdavi SM Jafari E Assadpoor andDDehnadldquoMicroencapsulation optimization of natural anthocyaninswith maltodextrin gum Arabic and gelatinrdquo InternationalJournal of Biological Macromolecules vol 85 pp 379ndash385 2016

[18] N V N Jyothi P M Prasanna S N Sakarkar K S PrabhaP S Ramaiah and G Y Srawan ldquoMicroencapsulation tech-niques factors influencing encapsulation efficiencyrdquo Journal ofMicroencapsulation vol 27 no 3 pp 187ndash197 2010

[19] S M Jafari E Assadpoor Y He and B Bhandari ldquoEncapsu-lation efficiency of food flavours and oils during spray dryingrdquoDrying Technology vol 26 no 7 pp 816ndash835 2008

[20] S C Samantha A S Bruna R M Adriana B Fabio A RSandro and R C Aline ldquoDrying by spray drying in the foodindustry Micro-encapsulation process parameters and maincarriers usedrdquo African Journal of Food Science vol 9 no 9 pp462ndash470 2015

[21] T C Kha M H Nguyen P D Roach and C E StathopoulosldquoMicroencapsulation of Gac oil Optimisation of spray dryingconditions using response surface methodologyrdquo Powder Tech-nology vol 264 pp 298ndash309 2014

[22] E Janiszewska-Turak ldquoCarotenoids microencapsulation byspray drying method and supercritical micronizationrdquo FoodResearch International vol 99 pp 891ndash901 2017

[23] A Goncalves B N Estevinho and F Rocha ldquoDesign andcharacterization of controlled-release vitamin A microparticlesprepared by a spray-drying processrdquo Powder Technology vol305 pp 411ndash417 2017

[24] MOrdonez and AHerrera ldquoMorphologic and stability cassavastarch matrices for encapsulating limonene by spray dryingrdquoPowder Technology vol 253 pp 89ndash97 2014

[25] S-M Jafari K Mahdavi-Khazaei and A Hemmati-KakhkildquoMicroencapsulation of saffron petal anthocyanins with cressseed gum compared with Arabic gum through freeze dryingrdquoCarbohydrate Polymers vol 140 pp 20ndash25 2016

[26] M P Rascon C I Beristain H S Garcıa and M A Sal-gado ldquoCarotenoid retention and storage stability of spray-dried encapsulated paprika oleoresin using gum Arabic and

Soy protein isolate as wall materialsrdquo LWT- Food Science andTechnology vol 44 no 2 pp 549ndash557 2011

[27] GA Rocha C S Favaro-Trindade andC R F Grosso ldquoMicro-encapsulation of lycopene by spray drying Characterizationstability and application of microcapsulesrdquo Food and Bioprod-ucts Processing vol 90 no 1 pp 37ndash42 2012

[28] Q Shen and S Y Quek ldquoMicroencapsulation of astaxanthinwith blends of milk protein and fiber by spray dryingrdquo Journalof Food Engineering vol 123 pp 165ndash171 2014

[29] A M Goula and K G Adamopoulos ldquoA new technique forspray-dried encapsulation of lycopenerdquoDrying Technology vol30 no 6 pp 641ndash652 2012

[30] J Loksuwan ldquoCharacteristics of microencapsulated 120573-caroteneformed by spray drying with modified tapioca starch nativetapioca starch andmaltodextrinrdquoFoodHydrocolloids vol 21 no5-6 pp 928ndash935 2007

[31] A A Santana L E Kurozawa R A de Oliveira and K JPark ldquoInfluence of Process Conditions on the PhysicochemicalProperties of Pequi Powder Produced by Spray Dryingrdquo DryingTechnology vol 31 no 7 pp 825ndash836 2013

[32] D Troya D S Tupuna-Yerovi and J Ruales ldquoEffects of WallMaterials and Operating Parameters on Physicochemical Pro-perties Process Efficiency and Total Carotenoid Content ofMicroencapsulated Banana Passionfruit Pulp (Passiflora tri-partita var mollissima) by Spray-Dryingrdquo Food and BioprocessTechnology vol 11 no 10 pp 1828ndash1839 2018

[33] D C Montgomery Design and Analysis of Experiments JohnWiley amp Sons 8th edition 2012

[34] M do S M Rufino R Alves E de Brito et al MetodologiaCientıfica Determinacao da Atividade Antioxidante Total emFrutas pela Captura do Radical Livre ABTS ComunicadoTecnico (Embrapa Agroindustria Tropical Online) 2007

[35] N Nenadis L-F Wang M Tsimidou and H-Y Zhang ldquoEsti-mation of scavenging activity of phenolic compounds using theABTS∙+ assayrdquo Journal of Agricultural and Food Chemistry vol52 no 15 pp 4669ndash4674 2004

[36] C A Di Battista D ConstenlaM V Ramırez-Rigo and J PinaldquoThe use of Arabic gum maltodextrin and surfactants in themicroencapsulation of phytosterols by spray dryingrdquo PowderTechnology vol 286 pp 193ndash201 2015

[37] C A Schneider W S Rasband and K W Eliceiri ldquoNIH Imageto ImageJ 25 years of image analysisrdquo Nature Methods vol 9no 7 pp 671ndash675 2012

[38] S Shamaei S S Seiiedlou M Aghbashlo E Tsotsas and AKharaghani ldquoMicroencapsulation of walnut oil by spray dry-ing effects of wall material and drying conditions on physico-chemical properties of microcapsulesrdquo Innovative Food Scienceand Emerging Technologies vol 39 pp 101ndash112 2017

[39] L Medina-Torres R Santiago-Adame F Calderas et alldquoMicroencapsulation by spray drying of laurel infusions (Litseaglaucescens) with maltodextrinrdquo Industrial Crops and Productsvol 90 pp 1ndash8 2016

[40] S Beirao-da-Costa C Duarte A I Bourbon et al ldquoInulinpotential for encapsulation and controlled delivery of Oreganoessential oilrdquo Food Hydrocolloids vol 33 no 2 pp 199ndash2062013

[41] R Santiago-Adame L Medina-Torres J A Gallegos-Infante etal ldquoSpray drying-microencapsulation of cinnamon infusions(Cinnamomum zeylanicum) with maltodextrinrdquo LWT- FoodScience and Technology vol 64 no 2 pp 571ndash577 2015

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

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Page 4: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

4 International Journal of Food Science

(a) (b) (c)

(d) (e) (f)

(g) (h) (i)

Figure 1 Scanning electron microscopy (SEM) images (magnification x500) of arabic gum microparticles with microencapsulated 120573-carotene (a) 94 AG 1232∘C (b) 94 AG 1868∘C (c) 306 AG 1232∘C (d) 306 AG 1868∘C (e) 20 AG 155∘C (f) 5 AG 155∘C(g) 35 AG 155∘C (h) 20 AG 110∘C (i) 20 AG 200∘C

The encapsulation efficiency (EE) was calculated as byRocha Favaro-Trindade [27] quantifying the ratio betweenthe mass of 120573-carotene present in the microparticles and the120573-carotenersquo mass initially present in the feed solution

254 Antioxidant Activity of the Encapsulated Material Forthe measurement of the antioxidant activity (AA) of theencapsulated molecules the microparticles core materialswere previously extracted with ethanol as described in theprevious section Afterwards a volume of 800 120583L of super-natant was mixed with 2200 120583L of ABTS+ solution followedby the steps described in Section 24 for pure 120573-carotene

3 Results and Discussion

31 Microparticle Morphology and Size Distribution Themorphological characteristics of the obtained arabic gummicroparticles with 120573-carotene were investigated using SEMSEM images have shown that the particles maintain a similar

spherical-like shape with a smooth or wrinkled surfacedepending on the drying conditions (Figure 1)

Most of the particles did not present a significant inci-dence of cracks or fissures in the outer surface indicating aresistant external physical structureMicroparticles producedwithout apparent damage have a lower gas permeabilitypresenting a more effective protection of the bioactive com-pounds from oxidation reactions and avoiding their unde-sired release [38]

Higher drying inlet temperatures tend to produce parti-cles with a smoother surface and with a low degree of teethand concavities (Figures 1(a) 1(b) 1(c) 1(d) 1(h) and 1(i))This fact may be attributed to rapid water evaporation andhigher pressure inside the particles during microencapsula-tion at higher temperatures preventing shrinking [39] On theother hand water diffusion is slower at lower temperaturesallowing more time for the particles to deform wrinkleand collapse [40] Similar results were reported by Santiago-Adame Medina-Torres [41] for microparticles of cinnamon

International Journal of Food Science 5

(a) (b)

Figure 2 Scanning electron microscopy (SEM) images (magnification x2000) of the internal surface of Arabic gum microparticles with120573-carotene microencapsulated (a) 20 AG 110∘C (b) 94 AG 1232∘C

infusions with maltodextrin in which the effect of threedifferent drying temperatures (140 160 and 180∘C) wasevaluated They found microparticles morphologically moredefined and smoother without evident cracks or particleagglomerations in the spray drying process both at 160 and180∘C

At the contrary Figures 1(a) and 1(c) 1(b) and 1(d)and 1(e) and 1(f) show that the different values of arabicgum concentration studied did not influence substantially theparticles morphology as mixtures with a similar proportionof smooth and collapsed particles were obtained GoncalvesEstevinho [23] and Tonon Brabet [42] also found no influ-ence of the wall material concentration on the morphology ofthe particles obtained in themicroencapsulation of vitamin Awith arabic gum and acaı pulp with maltodextrin

The internal morphology is shown in Figure 2 Allmicroparticles obtained were shown to be microcapsulesenvisaging that the core material (120573-carotene) was entrappedwithin the wall or in the centre Central void formation acharacteristic of the spray drying process is related to theexpansion of the particles during the latter stages of thedrying process when the temperature exceeds the boilingpoint of the water [43 44] This internal structure of themicroparticles was also observed in microencapsulated soy-bean extract microencapsulated by spray drying in arabicgum or maltodextrin matrix [45] as well as in gelatinarabicgummicroparticles loaded with fish oil [46]

Particle size distribution is a physical parameter of thepowders which may influence their properties involvinghandling transport and storage such as bulk density angleof repose flowability rehydration capacity solubility anddispersibility [17 47] According toOnwulata [48] and Tontuland Topuz [49] the stability of the functional componentssensitive to environmental conditions is also affected by theparticle size

The particle size of 120573-carotene loaded arabic gummicro-capsules ranged from 182 to 4091 120583m In Figure 3 theparticle size distribution of the microcapsules produced atdifferent temperatures is shown (at 1232 and 1868∘C) andwith different arabic gum concentrations (5 and 35) In allcases more than 80 of the particles had a size below 10 120583m

In general a higher frequency of particles with sizesabove 10 120583m was observed with increasing arabic gumconcentration (Figures 3(a) and 3(b))This factmay be relatedto the higher viscosity of the spray drying feed solutionAccording to Tontul and Topuz [49] and Tonon Brabet [42]the liquid droplet size during atomization varies directly withthe liquid viscosity at constant atomizer speed resulting inlarger particles Similar results were obtained for differentpowders produced by spray drying such as blackberry juicein maltodextrin Ferrari Germer [50] and coffee oil in arabicgum Frascareli Silva [51]

The increase in inlet drying temperature also resulted in ahigher frequency of particles with sizes above 10 120583m (Figures3(c) and 3(d)) This can be related to increased swellingthereby preventing contraction of the particle as the dryingtemperature increases [50 52]These results are in agreementwith those obtained by Tonon Brabet [42] who evaluated themicroencapsulated acaı pulp inmaltodextrin by spray dryingAccording to the authors slower drying rate ie when theinlet drying temperature is low the particles shrink evenlymaking their size smaller However when the drying rateis higher the rapid evaporation of the water creates a hardcrust in the particle that prevents its contraction in the dryingprocess resulting in larger particles

32 Response Surface Analysis Response surface methodol-ogy (RSM) was performed to optimize spray drying condi-tions considering linear quadratic and interaction effectsbetween independent variables on the microencapsulationof 120573-carotene with arabic gum A second-order polynomialmodel described by (1) was fitted to the experimental datavalues obtained for each response variable studied which arepresented in Table 1 The determination coefficients (R2 andRAdj2) and the linear and quadratic effects of the factorsas well as their interaction for each response variable arepresented in Table 2

The results show that except for the antioxidant activityresponse the mathematical model used was fitted withgood determination coefficients (R2 gt 070) According toLundstedt Seifert [53] values above 07 represent a good fitof the model In addition ANOVA indicated that the lack of

6 International Journal of Food Science

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(a)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(b)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(c)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(d)

Figure 3 Relative frequency (bars) and cumulative frequency (line) equivalent to the diameter of microparticles (a) 94 AG 1232∘C (b)94 AG 1868∘C (c) 5 AG 155∘C (d) 35 AG 155∘C

Table 2 Second-order polynomial equations for each response variable

Equation R2 RAdj2

EE = minus48699 lowast + 03036AG minus 0001AG2 + 0710T lowast minus 0002T2 lowast minus 0003AGT 087 074DY = minus175962 lowast + 4222AG lowast minus 0097AG2 lowast + 2245T lowast minus 0007T2 lowast minus 0004AGT 085 071LC = 56961ndash2808AG lowast + 0069AG2 lowast minus 0257T + 00025T2 lowast minus 00003AGT 091 082AG arabic gum () T temperature (∘C) EE encapsulation efficiency () DY drying yield () LC loading capacity (mg 120573-carotenegminus1particles)lowastAffectingsignificantly the response variable (pgt005)

fit (p gt 005) relative to pure error was not significant at 95of confidence level The expected errors of the models on theprediction of the responses were estimated to be 76 72and 127 for LC EE and DY respectively Figures 4(a) 4(b)and 5 show the 3-dimensional response surfaces that illustratethe effects of arabic gum concentration (AG ) and dryinginlet temperature (T ∘C) on the responses studied

321 Encapsulation Efficiency and Loading Capacity Theencapsulation efficiency values of 120573-carotenewith arabic gum

ranged between 62 and 160 and the loading capacity valuesranged from 119 to 336mg120573-carotenegminus1particles as shownin Table 1 Similar results were found by Rocha Favaro-Trindade [27] uponmicroencapsulation of lycopene inmodi-fied starch that found an EE around 21 and by Botrel Borges[54] who microencapsulated oregano oil using a mixtureof arabic gum maltodextrin and modified starch as wallmaterial by spray drying found an EE between 51 and 339

As seen in Figures 4(a) and 4(b) the increase in dryingtemperature and decrease in arabic gum concentration lead

International Journal of Food Science 7

18

16

14

12

10

8

6

4

200

180

160

140

1205

1015

2025

3035

EncapsulationEffi

ciency ()

Temperature ( ∘C) Arabic gum ()

(a)

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

45

40

35

30

25

20

15

10

Loading Capacity

(mg-caroteneg - 1particles)

(b)

Figure 4 Response surface fitted to (a) encapsulation efficiency and (b) loading capacity as a function of Arabic gum concentration anddrying inlet temperature

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

50

40

30

20

10

0

Drying yield (

)

Figure 5 Response surface fitted to drying yield as a function ofarabic gum concentration and drying

to an increase in the EE Regarding LC higher values wereobserved at both ends of the arabic gum concentrationthat is when the lowest (5) and the highest concentration(35) of the wall material were used In addition when thedrying temperature increased the loading capacity was alsoincreased The same behaviour was reported by Ferrari Ger-mer [50] in microparticles of blackberry using maltodextrinas wall material

According to Jafari Assadpoor [19] the encapsulationefficiency is influenced by the drying conditions emulsion

and bioactive compound characteristics and the wall materialproperties Low encapsulation efficiency value could be dueto 120573-carotene being extremely sensitive to environmentalfactors such as exposure to heat light and oxygen duringencapsulation processing

The experimental data obtained of the encapsulation effi-ciency and loading capacity of the particles were adjusted tothe second-order polynomialmodelwith a satisfactory coeffi-cient of determination (Table 2) Both independent variableshad a significant effect on these responses Arabic gumconcentration had a positive quadratic effect on the loadingcapacity of the microparticles whereas for the encapsulationefficiency arabic gum concentration showed a linear negativeeffect In relation to the drying inlet temperature a positivelinear and quadratic negative effect on the encapsulation effi-ciency and a positive linear effect on the loading capacitywereobserved However the interaction coefficient was found tobe nonsignificant indicating that there was no interactionbetween the independent variables on the EE of particles

The drying temperature is directly proportional to theevaporation rate and inversely proportional to the finalwater content of the dried microparticles At high dryingtemperatures there is a higher evaporation rate of water onthe droplet surface which leads to the rapid formation of asemipermeable membrane resulting in the protection of therelease of the bioactive compounds during the drying processand consequently in a higher bioactive retention Howeverhigher drying temperatures could cause cracks and fissureson the surface of the particles leading to loss of the bioactivecompound [19 21]

Wall material concentration is also a factor that affectsthe retention of the bioactive compounds due to their vis-cosity properties in the feed solution Some researchers have

8 International Journal of Food Science

reported that the wall material concentration has a positiveeffect on the encapsulation efficiency ie the increase ofsolids content in the feed increases bioactive retention [21 5556] This behaviour could be related to the reduction of thetime required to form a surface crust in the atomized dropletsin the initial drying process when the solids concentration inthe feed solution increases This rapidly formed crust is notpermeable to compounds thereby protecting the bioactivefrom oxidation [57 58]

However too high viscosity of the feed solutions delaysthe formation of discrete particles during spray dryingwhereas a low viscosity in feed delays the formation of asemipermeable surface crust favouring further losses of thebioactive compounds [59] Therefore according to Reinec-cius [60] each wall material has its ideal feed concentrationto obtain higher encapsulation efficiency which is basedon the solubility and viscosity of the feed solution In thiswork an ideal arabic gum concentration of 74 was foundfor higher values of encapsulation efficiency and loadingcapacity Fernandes Marques [57] who evaluated the effectof total solids concentration on the microencapsulation ofrosemary essential oil by spray drying using maltodextrinand modified starch (11) as wall materials found higherencapsulation efficiency when a concentration of the wallmaterial of 22 was used which was reported as the idealconcentration for maltodextrin as wall material

322 Drying Yield Drying yield of the spray drying processis directly related to the cost of production and efficiencythus it is an important indicator that the industry considersin its production line [49 61] According to Nunes andMercadante [62] and Rutz Borges [63] drying yield isinfluenced by both the equipment settings (feed rate feedinlet and outlet temperature and flow rate) and dryingconditions (type and wall material concentration)

In this study a second-order model was fitted to theexperimental data of the drying yield with acceptable coef-ficient of determination and Table 2 shows that both inde-pendent variables arabic gum concentration and the dryinginlet temperature had a significant negative quadratic effecton the drying yield According to Table 1 the drying yields of120573-carotene with arabic gum ranged between 159 and 439Other researchers have found values of drying yield around50 Roccia Martınez [64] who studied the microencapsu-lation of the sunflower oil by spray drying using maltodextrinas a carrier agent found drying yield values that ranged from544 to 3988 and Santana Kurozawa [31] produced arabicgum microparticles with pulp pequi extract by spray dryingand obtained a drying yield values between 258 and 561

Low drying yield in the spray drying process is mostlydue to retention of the powder in the drying chamber wallcyclone inefficient in collecting fine particles and the highviscosity of the feed solution This powder retention problemcauses considerable economic loss and it is not cost-effectivefor industry as there would be frequent interruptions tothe dryer cleaning besides affecting the quality of the finalproduct However drying yield in the microencapsulationtechnique could be improved by modifying the spray dryingconditions in order to decrease the adhesion of particles to

the drying chamber wall [64ndash66] According to Tontul andTopuz [49] and Jayasundera Adhikari [67] the mechanicalscraping of the drying chamber wall introduction of coldair from the bottom and the use of low temperature lowhumidity air are some examples of process-based approachesthat could increase drying yield

As shown in Figure 5 as the drying temperature andthe arabic gum concentration increased the drying yieldalso increased until a maximum value was achieved Afterthis value decreases in the drying yield were observed evenwith the increase of both independent variables The highestdrying yield value was found for the sample with 20 GAdried at 155∘C

Chong and Wong [68] also found an optimum dosageof the wall material concentration (30 maltodextrin) andtemperature value (180∘C) that maximized the drying yield(57) when producing sapodilla puree particles by spraydrying using different maltodextrin concentrations (10-50wv) The authors referred that increasing the wall materialconcentration above the optimum value leads to an increaseviscosity of the feed solution thereby negatively affecting thedrying yield

323 Antioxidant Activity The AA values of encapsulated120573-carotene range from 005 to 078 120583mol troloxmgminus1120573-carotene whereas the commercial 120573-carotene before encap-sulation possessed 235 120583mol troloxmgminus1120573-carotene Thelower antioxidant activity after the encapsulation may berelated not only to the encapsulation process itself but alsoto the incomplete extraction of the encapsulated moleculesbefore antioxidant activity measurement This decrease inantioxidant activity after the spray drying process was alsoobserved for example by Franceschinis Salvatori [69] in themicroencapsulation of blackberry juices with maltodextrinand Hee Tan [70] in virgin coconut oil microparticles in amixture of maltodextrin arabic gum sodium caseinate andwhey protein concentrate

The data obtained for the antioxidant activity did notfit the second-order polynomial model though from theresults of Table 1 the two independent variables studiedarabic gum concentration and drying inlet temperatureaffected antioxidant activity of the encapsulated moleculessince an AA increase was observed when the temperaturedecreased (runs 4-3 2-1 and 11-10) and when the arabic gumconcentration increased (runs 1-3 2-4 8-9)

Other researchers have also studied the influence ofdrying inlet temperature and wall material on AA of theparticles Kha Nguyen [71] studied the effects of varyingmaltodextrin concentrations and spray drying temperatureson the antioxidant activity of Gac fruit powder and theyreported that increasing the drying inlet temperature from120 to 200∘C showed a significant loss of AA Additionallywith increasing maltodextrin concentration from 20 to 30the loss of AA was also observed The authors explainedthat AA loss could be due to loss of antioxidant compoundspresent in Gac powder spray dried at high temperaturesMiravet Alacid [72] who evaluated the antioxidant activityof pomegranate juice powder produced by spray dryingusing prebiotic fibers and maltodextrin as wall material also

International Journal of Food Science 9

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

10

08

06

04

02

00

minus02

Desirability

Figure 6 Desirability surface for optimal conditions

observed that the increase of the drying inlet temperaturefrom 160 to 200∘C had a significant negative effect on theantioxidant activity for both wall materials studied

324 Optimization of Drying Process Conditions The desir-ability function was performed for the simultaneous opti-mization of the responses that fitted to the second-ordermodel (Table 2) and the desirability surface for optimalconditions is depicted in Figure 6 Desirability values higherthan 07 were considered indicating a good optimization ofthe experimental data of each response variable [73] Thebest conditions for the spray drying microencapsulation of 120573-carotene with arabic gum as wall material were determined inorder to obtain higher values for drying yield encapsulationefficiency and loading capacity

The inlet drying temperature of 173∘C and arabic gumconcentration of 119 are recommended as the ideal con-ditions for microencapsulation of 120573-carotene Under theseconditions the predicted EE DY and LC are 1562 3630and 2274 mg 120573-carotenegminus1particles respectively

4 Conclusions

Themicroencapsulation of120573-carotene in arabic gumby spraydrying was investigated The arabic gum concentration anddrying inlet temperature influenced the drying yield encap-sulation efficiency and load capacity responses Regardingthe AA the antioxidant activity of 120573-carotene was reducedwhen microencapsulated at high temperatures (200∘C) inrelation to low temperatures (110∘C)

SEM analysis showed that the microparticles are micro-capsules Most of them presented a similar morphology amixture of smooth and wrinkled particles with a diameterlower than 10 120583m Increases in drying temperature favouredthe formation of smoother and larger particles

From the experimental conditions the drying inlet tem-perature of 173∘C and the arabic gum concentration of 119

were those that allow obtaining higher 120573-carotene contenthigher encapsulation efficiency and higher drying yield

The systematic approach used for the study of 120573-carotenemicroencapsulation process by spray drying may be easilyapplied for other core and wall materials Further studies willfocus on release studies in several aqueous media and even-tually on the encapsulation of natural carotenoid extracts

Data Availability

The data used to support the findings of this study areincluded within the article

Conflicts of Interest

The authors declare that they have no conflicts of interest

Acknowledgments

This work was supported by Conselho Nacional de Desen-volvimento Cientıfico e TecnologicondashCNPq through theCiencia sem Fronteiras program (CSF) (Grant CSF 2062682014-9 to first author)The authors acknowledge the financialsupport from Fundacao para a Ciencia e a TecnologiaPortugal Project UIDAGR041292013

References

[1] M E Rodrıguez-Huezo R Pedroza-Islas L A Prado-Bar-ragan C I Beristain and E J Vernon-Carter ldquoMicroencapsu-lation by spray drying of multiple emulsions containing caro-tenoidsrdquo Journal of Food Science vol 69 no 7 pp 351ndash359 2004

[2] A V Rao and L G Rao ldquoCarotenoids and human healthrdquoPharmacological Research vol 55 no 3 pp 207ndash216 2007

[3] J Fiedor and K Burda ldquoPotential role of carotenoids as anti-oxidants in human health and diseaserdquo Nutrients vol 6 no 2pp 466ndash488 2014

[4] R Arimboor R B Natarajan K R Menon L P Chan-drasekhar and VMoorkoth ldquoRed pepper (Capsicum annuum)carotenoids as a source of natural food colors analysis andstabilitymdasha reviewrdquo Journal of Food Science and Technology vol52 no 3 pp 1258ndash1271 2015

[5] M H Walter and D Strack ldquoCarotenoids and their cleavageproducts Biosynthesis and functionsrdquoNatural Product Reportsvol 28 no 4 pp 663ndash692 2011

[6] A Kaczor M Baranska and K Czamara Carotenoids WileyOnline Library 2016

[7] A F Aissa M L P Bianchi J C Ribeiro et al ldquoComparativestudy of 120573-carotene and microencapsulated 120573-carotene Eval-uation of their genotoxic and antigenotoxic effectsrdquo Food andChemical Toxicology vol 50 no 5 pp 1418ndash1424 2012

[8] Z Al Tanoury A Piskunov and C Rochette-Egly ldquoVitamina and retinoid signaling Genomic and nongenomic effectsrdquoJournal of Lipid Research vol 54 no 7 pp 1761ndash1775 2013

[9] E G Donhowe F P Flores W L Kerr L Wicker and F KongldquoCharacterization and invitro bioavailability of 120573-caroteneEffects of microencapsulation method and food matrixrdquo LWT-Food Science and Technology vol 57 no 1 pp 42ndash48 2014

[10] K Gul A Tak A Singh et al ldquoChemistry encapsulation andhealth benefits of szlig-carotene-A reviewrdquo Cogent Food amp Agri-culture vol 1 no 1 Article ID 1018696 2015

10 International Journal of Food Science

[11] HW Kim J B Kim S Poovan et al ldquoEffect of processing con-ditions on the content of cistrans carotene isomers as provita-min A carotenoids in Korean sweet potato varietiesrdquo Interna-tional Journal of Food Sciences and Nutrition vol 65 no 7 pp821ndash826 2014

[12] C Qian E A Decker H Xiao and D J McClements ldquoNano-emulsion delivery systems Influence of carrier oil on 120573-caro-tene bioaccessibilityrdquo Food Chemistry vol 135 no 3 pp 1440ndash1447 2012

[13] J C Spada L D F Marczak I C Tessaro and C P Z NorenaldquoMicroencapsulation of 120573-carotene using native pinhao starchmodified pinhao starch and gelatin by freeze-dryingrdquo Interna-tional Journal of Food Science amp Technology vol 47 no 1 pp186ndash194 2012

[14] G Zakynthinos and T Varzakas ldquoCarotenoids From plants tofood industryrdquo Current Research in Nutrition and Food Sciencevol 4 no 1 pp 38ndash51 2016

[15] R Liang Q Huang J Ma C F Shoemaker and F ZhongldquoEffect of relative humidity on the store stability of spray-driedbeta-carotene nanoemulsionsrdquo Food Hydrocolloids vol 33 no2 pp 225ndash233 2013

[16] C Saenz S Tapia J Chavez and P Robert ldquoMicroencapsula-tion by spray drying of bioactive compounds from cactus pear(Opuntia ficus-indica)rdquo Food Chemistry vol 114 no 2 pp 616ndash622 2009

[17] S AkhavanMahdavi SM Jafari E Assadpoor andDDehnadldquoMicroencapsulation optimization of natural anthocyaninswith maltodextrin gum Arabic and gelatinrdquo InternationalJournal of Biological Macromolecules vol 85 pp 379ndash385 2016

[18] N V N Jyothi P M Prasanna S N Sakarkar K S PrabhaP S Ramaiah and G Y Srawan ldquoMicroencapsulation tech-niques factors influencing encapsulation efficiencyrdquo Journal ofMicroencapsulation vol 27 no 3 pp 187ndash197 2010

[19] S M Jafari E Assadpoor Y He and B Bhandari ldquoEncapsu-lation efficiency of food flavours and oils during spray dryingrdquoDrying Technology vol 26 no 7 pp 816ndash835 2008

[20] S C Samantha A S Bruna R M Adriana B Fabio A RSandro and R C Aline ldquoDrying by spray drying in the foodindustry Micro-encapsulation process parameters and maincarriers usedrdquo African Journal of Food Science vol 9 no 9 pp462ndash470 2015

[21] T C Kha M H Nguyen P D Roach and C E StathopoulosldquoMicroencapsulation of Gac oil Optimisation of spray dryingconditions using response surface methodologyrdquo Powder Tech-nology vol 264 pp 298ndash309 2014

[22] E Janiszewska-Turak ldquoCarotenoids microencapsulation byspray drying method and supercritical micronizationrdquo FoodResearch International vol 99 pp 891ndash901 2017

[23] A Goncalves B N Estevinho and F Rocha ldquoDesign andcharacterization of controlled-release vitamin A microparticlesprepared by a spray-drying processrdquo Powder Technology vol305 pp 411ndash417 2017

[24] MOrdonez and AHerrera ldquoMorphologic and stability cassavastarch matrices for encapsulating limonene by spray dryingrdquoPowder Technology vol 253 pp 89ndash97 2014

[25] S-M Jafari K Mahdavi-Khazaei and A Hemmati-KakhkildquoMicroencapsulation of saffron petal anthocyanins with cressseed gum compared with Arabic gum through freeze dryingrdquoCarbohydrate Polymers vol 140 pp 20ndash25 2016

[26] M P Rascon C I Beristain H S Garcıa and M A Sal-gado ldquoCarotenoid retention and storage stability of spray-dried encapsulated paprika oleoresin using gum Arabic and

Soy protein isolate as wall materialsrdquo LWT- Food Science andTechnology vol 44 no 2 pp 549ndash557 2011

[27] GA Rocha C S Favaro-Trindade andC R F Grosso ldquoMicro-encapsulation of lycopene by spray drying Characterizationstability and application of microcapsulesrdquo Food and Bioprod-ucts Processing vol 90 no 1 pp 37ndash42 2012

[28] Q Shen and S Y Quek ldquoMicroencapsulation of astaxanthinwith blends of milk protein and fiber by spray dryingrdquo Journalof Food Engineering vol 123 pp 165ndash171 2014

[29] A M Goula and K G Adamopoulos ldquoA new technique forspray-dried encapsulation of lycopenerdquoDrying Technology vol30 no 6 pp 641ndash652 2012

[30] J Loksuwan ldquoCharacteristics of microencapsulated 120573-caroteneformed by spray drying with modified tapioca starch nativetapioca starch andmaltodextrinrdquoFoodHydrocolloids vol 21 no5-6 pp 928ndash935 2007

[31] A A Santana L E Kurozawa R A de Oliveira and K JPark ldquoInfluence of Process Conditions on the PhysicochemicalProperties of Pequi Powder Produced by Spray Dryingrdquo DryingTechnology vol 31 no 7 pp 825ndash836 2013

[32] D Troya D S Tupuna-Yerovi and J Ruales ldquoEffects of WallMaterials and Operating Parameters on Physicochemical Pro-perties Process Efficiency and Total Carotenoid Content ofMicroencapsulated Banana Passionfruit Pulp (Passiflora tri-partita var mollissima) by Spray-Dryingrdquo Food and BioprocessTechnology vol 11 no 10 pp 1828ndash1839 2018

[33] D C Montgomery Design and Analysis of Experiments JohnWiley amp Sons 8th edition 2012

[34] M do S M Rufino R Alves E de Brito et al MetodologiaCientıfica Determinacao da Atividade Antioxidante Total emFrutas pela Captura do Radical Livre ABTS ComunicadoTecnico (Embrapa Agroindustria Tropical Online) 2007

[35] N Nenadis L-F Wang M Tsimidou and H-Y Zhang ldquoEsti-mation of scavenging activity of phenolic compounds using theABTS∙+ assayrdquo Journal of Agricultural and Food Chemistry vol52 no 15 pp 4669ndash4674 2004

[36] C A Di Battista D ConstenlaM V Ramırez-Rigo and J PinaldquoThe use of Arabic gum maltodextrin and surfactants in themicroencapsulation of phytosterols by spray dryingrdquo PowderTechnology vol 286 pp 193ndash201 2015

[37] C A Schneider W S Rasband and K W Eliceiri ldquoNIH Imageto ImageJ 25 years of image analysisrdquo Nature Methods vol 9no 7 pp 671ndash675 2012

[38] S Shamaei S S Seiiedlou M Aghbashlo E Tsotsas and AKharaghani ldquoMicroencapsulation of walnut oil by spray dry-ing effects of wall material and drying conditions on physico-chemical properties of microcapsulesrdquo Innovative Food Scienceand Emerging Technologies vol 39 pp 101ndash112 2017

[39] L Medina-Torres R Santiago-Adame F Calderas et alldquoMicroencapsulation by spray drying of laurel infusions (Litseaglaucescens) with maltodextrinrdquo Industrial Crops and Productsvol 90 pp 1ndash8 2016

[40] S Beirao-da-Costa C Duarte A I Bourbon et al ldquoInulinpotential for encapsulation and controlled delivery of Oreganoessential oilrdquo Food Hydrocolloids vol 33 no 2 pp 199ndash2062013

[41] R Santiago-Adame L Medina-Torres J A Gallegos-Infante etal ldquoSpray drying-microencapsulation of cinnamon infusions(Cinnamomum zeylanicum) with maltodextrinrdquo LWT- FoodScience and Technology vol 64 no 2 pp 571ndash577 2015

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

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Page 5: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

International Journal of Food Science 5

(a) (b)

Figure 2 Scanning electron microscopy (SEM) images (magnification x2000) of the internal surface of Arabic gum microparticles with120573-carotene microencapsulated (a) 20 AG 110∘C (b) 94 AG 1232∘C

infusions with maltodextrin in which the effect of threedifferent drying temperatures (140 160 and 180∘C) wasevaluated They found microparticles morphologically moredefined and smoother without evident cracks or particleagglomerations in the spray drying process both at 160 and180∘C

At the contrary Figures 1(a) and 1(c) 1(b) and 1(d)and 1(e) and 1(f) show that the different values of arabicgum concentration studied did not influence substantially theparticles morphology as mixtures with a similar proportionof smooth and collapsed particles were obtained GoncalvesEstevinho [23] and Tonon Brabet [42] also found no influ-ence of the wall material concentration on the morphology ofthe particles obtained in themicroencapsulation of vitamin Awith arabic gum and acaı pulp with maltodextrin

The internal morphology is shown in Figure 2 Allmicroparticles obtained were shown to be microcapsulesenvisaging that the core material (120573-carotene) was entrappedwithin the wall or in the centre Central void formation acharacteristic of the spray drying process is related to theexpansion of the particles during the latter stages of thedrying process when the temperature exceeds the boilingpoint of the water [43 44] This internal structure of themicroparticles was also observed in microencapsulated soy-bean extract microencapsulated by spray drying in arabicgum or maltodextrin matrix [45] as well as in gelatinarabicgummicroparticles loaded with fish oil [46]

Particle size distribution is a physical parameter of thepowders which may influence their properties involvinghandling transport and storage such as bulk density angleof repose flowability rehydration capacity solubility anddispersibility [17 47] According toOnwulata [48] and Tontuland Topuz [49] the stability of the functional componentssensitive to environmental conditions is also affected by theparticle size

The particle size of 120573-carotene loaded arabic gummicro-capsules ranged from 182 to 4091 120583m In Figure 3 theparticle size distribution of the microcapsules produced atdifferent temperatures is shown (at 1232 and 1868∘C) andwith different arabic gum concentrations (5 and 35) In allcases more than 80 of the particles had a size below 10 120583m

In general a higher frequency of particles with sizesabove 10 120583m was observed with increasing arabic gumconcentration (Figures 3(a) and 3(b))This factmay be relatedto the higher viscosity of the spray drying feed solutionAccording to Tontul and Topuz [49] and Tonon Brabet [42]the liquid droplet size during atomization varies directly withthe liquid viscosity at constant atomizer speed resulting inlarger particles Similar results were obtained for differentpowders produced by spray drying such as blackberry juicein maltodextrin Ferrari Germer [50] and coffee oil in arabicgum Frascareli Silva [51]

The increase in inlet drying temperature also resulted in ahigher frequency of particles with sizes above 10 120583m (Figures3(c) and 3(d)) This can be related to increased swellingthereby preventing contraction of the particle as the dryingtemperature increases [50 52]These results are in agreementwith those obtained by Tonon Brabet [42] who evaluated themicroencapsulated acaı pulp inmaltodextrin by spray dryingAccording to the authors slower drying rate ie when theinlet drying temperature is low the particles shrink evenlymaking their size smaller However when the drying rateis higher the rapid evaporation of the water creates a hardcrust in the particle that prevents its contraction in the dryingprocess resulting in larger particles

32 Response Surface Analysis Response surface methodol-ogy (RSM) was performed to optimize spray drying condi-tions considering linear quadratic and interaction effectsbetween independent variables on the microencapsulationof 120573-carotene with arabic gum A second-order polynomialmodel described by (1) was fitted to the experimental datavalues obtained for each response variable studied which arepresented in Table 1 The determination coefficients (R2 andRAdj2) and the linear and quadratic effects of the factorsas well as their interaction for each response variable arepresented in Table 2

The results show that except for the antioxidant activityresponse the mathematical model used was fitted withgood determination coefficients (R2 gt 070) According toLundstedt Seifert [53] values above 07 represent a good fitof the model In addition ANOVA indicated that the lack of

6 International Journal of Food Science

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(a)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(b)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(c)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(d)

Figure 3 Relative frequency (bars) and cumulative frequency (line) equivalent to the diameter of microparticles (a) 94 AG 1232∘C (b)94 AG 1868∘C (c) 5 AG 155∘C (d) 35 AG 155∘C

Table 2 Second-order polynomial equations for each response variable

Equation R2 RAdj2

EE = minus48699 lowast + 03036AG minus 0001AG2 + 0710T lowast minus 0002T2 lowast minus 0003AGT 087 074DY = minus175962 lowast + 4222AG lowast minus 0097AG2 lowast + 2245T lowast minus 0007T2 lowast minus 0004AGT 085 071LC = 56961ndash2808AG lowast + 0069AG2 lowast minus 0257T + 00025T2 lowast minus 00003AGT 091 082AG arabic gum () T temperature (∘C) EE encapsulation efficiency () DY drying yield () LC loading capacity (mg 120573-carotenegminus1particles)lowastAffectingsignificantly the response variable (pgt005)

fit (p gt 005) relative to pure error was not significant at 95of confidence level The expected errors of the models on theprediction of the responses were estimated to be 76 72and 127 for LC EE and DY respectively Figures 4(a) 4(b)and 5 show the 3-dimensional response surfaces that illustratethe effects of arabic gum concentration (AG ) and dryinginlet temperature (T ∘C) on the responses studied

321 Encapsulation Efficiency and Loading Capacity Theencapsulation efficiency values of 120573-carotenewith arabic gum

ranged between 62 and 160 and the loading capacity valuesranged from 119 to 336mg120573-carotenegminus1particles as shownin Table 1 Similar results were found by Rocha Favaro-Trindade [27] uponmicroencapsulation of lycopene inmodi-fied starch that found an EE around 21 and by Botrel Borges[54] who microencapsulated oregano oil using a mixtureof arabic gum maltodextrin and modified starch as wallmaterial by spray drying found an EE between 51 and 339

As seen in Figures 4(a) and 4(b) the increase in dryingtemperature and decrease in arabic gum concentration lead

International Journal of Food Science 7

18

16

14

12

10

8

6

4

200

180

160

140

1205

1015

2025

3035

EncapsulationEffi

ciency ()

Temperature ( ∘C) Arabic gum ()

(a)

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

45

40

35

30

25

20

15

10

Loading Capacity

(mg-caroteneg - 1particles)

(b)

Figure 4 Response surface fitted to (a) encapsulation efficiency and (b) loading capacity as a function of Arabic gum concentration anddrying inlet temperature

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

50

40

30

20

10

0

Drying yield (

)

Figure 5 Response surface fitted to drying yield as a function ofarabic gum concentration and drying

to an increase in the EE Regarding LC higher values wereobserved at both ends of the arabic gum concentrationthat is when the lowest (5) and the highest concentration(35) of the wall material were used In addition when thedrying temperature increased the loading capacity was alsoincreased The same behaviour was reported by Ferrari Ger-mer [50] in microparticles of blackberry using maltodextrinas wall material

According to Jafari Assadpoor [19] the encapsulationefficiency is influenced by the drying conditions emulsion

and bioactive compound characteristics and the wall materialproperties Low encapsulation efficiency value could be dueto 120573-carotene being extremely sensitive to environmentalfactors such as exposure to heat light and oxygen duringencapsulation processing

The experimental data obtained of the encapsulation effi-ciency and loading capacity of the particles were adjusted tothe second-order polynomialmodelwith a satisfactory coeffi-cient of determination (Table 2) Both independent variableshad a significant effect on these responses Arabic gumconcentration had a positive quadratic effect on the loadingcapacity of the microparticles whereas for the encapsulationefficiency arabic gum concentration showed a linear negativeeffect In relation to the drying inlet temperature a positivelinear and quadratic negative effect on the encapsulation effi-ciency and a positive linear effect on the loading capacitywereobserved However the interaction coefficient was found tobe nonsignificant indicating that there was no interactionbetween the independent variables on the EE of particles

The drying temperature is directly proportional to theevaporation rate and inversely proportional to the finalwater content of the dried microparticles At high dryingtemperatures there is a higher evaporation rate of water onthe droplet surface which leads to the rapid formation of asemipermeable membrane resulting in the protection of therelease of the bioactive compounds during the drying processand consequently in a higher bioactive retention Howeverhigher drying temperatures could cause cracks and fissureson the surface of the particles leading to loss of the bioactivecompound [19 21]

Wall material concentration is also a factor that affectsthe retention of the bioactive compounds due to their vis-cosity properties in the feed solution Some researchers have

8 International Journal of Food Science

reported that the wall material concentration has a positiveeffect on the encapsulation efficiency ie the increase ofsolids content in the feed increases bioactive retention [21 5556] This behaviour could be related to the reduction of thetime required to form a surface crust in the atomized dropletsin the initial drying process when the solids concentration inthe feed solution increases This rapidly formed crust is notpermeable to compounds thereby protecting the bioactivefrom oxidation [57 58]

However too high viscosity of the feed solutions delaysthe formation of discrete particles during spray dryingwhereas a low viscosity in feed delays the formation of asemipermeable surface crust favouring further losses of thebioactive compounds [59] Therefore according to Reinec-cius [60] each wall material has its ideal feed concentrationto obtain higher encapsulation efficiency which is basedon the solubility and viscosity of the feed solution In thiswork an ideal arabic gum concentration of 74 was foundfor higher values of encapsulation efficiency and loadingcapacity Fernandes Marques [57] who evaluated the effectof total solids concentration on the microencapsulation ofrosemary essential oil by spray drying using maltodextrinand modified starch (11) as wall materials found higherencapsulation efficiency when a concentration of the wallmaterial of 22 was used which was reported as the idealconcentration for maltodextrin as wall material

322 Drying Yield Drying yield of the spray drying processis directly related to the cost of production and efficiencythus it is an important indicator that the industry considersin its production line [49 61] According to Nunes andMercadante [62] and Rutz Borges [63] drying yield isinfluenced by both the equipment settings (feed rate feedinlet and outlet temperature and flow rate) and dryingconditions (type and wall material concentration)

In this study a second-order model was fitted to theexperimental data of the drying yield with acceptable coef-ficient of determination and Table 2 shows that both inde-pendent variables arabic gum concentration and the dryinginlet temperature had a significant negative quadratic effecton the drying yield According to Table 1 the drying yields of120573-carotene with arabic gum ranged between 159 and 439Other researchers have found values of drying yield around50 Roccia Martınez [64] who studied the microencapsu-lation of the sunflower oil by spray drying using maltodextrinas a carrier agent found drying yield values that ranged from544 to 3988 and Santana Kurozawa [31] produced arabicgum microparticles with pulp pequi extract by spray dryingand obtained a drying yield values between 258 and 561

Low drying yield in the spray drying process is mostlydue to retention of the powder in the drying chamber wallcyclone inefficient in collecting fine particles and the highviscosity of the feed solution This powder retention problemcauses considerable economic loss and it is not cost-effectivefor industry as there would be frequent interruptions tothe dryer cleaning besides affecting the quality of the finalproduct However drying yield in the microencapsulationtechnique could be improved by modifying the spray dryingconditions in order to decrease the adhesion of particles to

the drying chamber wall [64ndash66] According to Tontul andTopuz [49] and Jayasundera Adhikari [67] the mechanicalscraping of the drying chamber wall introduction of coldair from the bottom and the use of low temperature lowhumidity air are some examples of process-based approachesthat could increase drying yield

As shown in Figure 5 as the drying temperature andthe arabic gum concentration increased the drying yieldalso increased until a maximum value was achieved Afterthis value decreases in the drying yield were observed evenwith the increase of both independent variables The highestdrying yield value was found for the sample with 20 GAdried at 155∘C

Chong and Wong [68] also found an optimum dosageof the wall material concentration (30 maltodextrin) andtemperature value (180∘C) that maximized the drying yield(57) when producing sapodilla puree particles by spraydrying using different maltodextrin concentrations (10-50wv) The authors referred that increasing the wall materialconcentration above the optimum value leads to an increaseviscosity of the feed solution thereby negatively affecting thedrying yield

323 Antioxidant Activity The AA values of encapsulated120573-carotene range from 005 to 078 120583mol troloxmgminus1120573-carotene whereas the commercial 120573-carotene before encap-sulation possessed 235 120583mol troloxmgminus1120573-carotene Thelower antioxidant activity after the encapsulation may berelated not only to the encapsulation process itself but alsoto the incomplete extraction of the encapsulated moleculesbefore antioxidant activity measurement This decrease inantioxidant activity after the spray drying process was alsoobserved for example by Franceschinis Salvatori [69] in themicroencapsulation of blackberry juices with maltodextrinand Hee Tan [70] in virgin coconut oil microparticles in amixture of maltodextrin arabic gum sodium caseinate andwhey protein concentrate

The data obtained for the antioxidant activity did notfit the second-order polynomial model though from theresults of Table 1 the two independent variables studiedarabic gum concentration and drying inlet temperatureaffected antioxidant activity of the encapsulated moleculessince an AA increase was observed when the temperaturedecreased (runs 4-3 2-1 and 11-10) and when the arabic gumconcentration increased (runs 1-3 2-4 8-9)

Other researchers have also studied the influence ofdrying inlet temperature and wall material on AA of theparticles Kha Nguyen [71] studied the effects of varyingmaltodextrin concentrations and spray drying temperatureson the antioxidant activity of Gac fruit powder and theyreported that increasing the drying inlet temperature from120 to 200∘C showed a significant loss of AA Additionallywith increasing maltodextrin concentration from 20 to 30the loss of AA was also observed The authors explainedthat AA loss could be due to loss of antioxidant compoundspresent in Gac powder spray dried at high temperaturesMiravet Alacid [72] who evaluated the antioxidant activityof pomegranate juice powder produced by spray dryingusing prebiotic fibers and maltodextrin as wall material also

International Journal of Food Science 9

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

10

08

06

04

02

00

minus02

Desirability

Figure 6 Desirability surface for optimal conditions

observed that the increase of the drying inlet temperaturefrom 160 to 200∘C had a significant negative effect on theantioxidant activity for both wall materials studied

324 Optimization of Drying Process Conditions The desir-ability function was performed for the simultaneous opti-mization of the responses that fitted to the second-ordermodel (Table 2) and the desirability surface for optimalconditions is depicted in Figure 6 Desirability values higherthan 07 were considered indicating a good optimization ofthe experimental data of each response variable [73] Thebest conditions for the spray drying microencapsulation of 120573-carotene with arabic gum as wall material were determined inorder to obtain higher values for drying yield encapsulationefficiency and loading capacity

The inlet drying temperature of 173∘C and arabic gumconcentration of 119 are recommended as the ideal con-ditions for microencapsulation of 120573-carotene Under theseconditions the predicted EE DY and LC are 1562 3630and 2274 mg 120573-carotenegminus1particles respectively

4 Conclusions

Themicroencapsulation of120573-carotene in arabic gumby spraydrying was investigated The arabic gum concentration anddrying inlet temperature influenced the drying yield encap-sulation efficiency and load capacity responses Regardingthe AA the antioxidant activity of 120573-carotene was reducedwhen microencapsulated at high temperatures (200∘C) inrelation to low temperatures (110∘C)

SEM analysis showed that the microparticles are micro-capsules Most of them presented a similar morphology amixture of smooth and wrinkled particles with a diameterlower than 10 120583m Increases in drying temperature favouredthe formation of smoother and larger particles

From the experimental conditions the drying inlet tem-perature of 173∘C and the arabic gum concentration of 119

were those that allow obtaining higher 120573-carotene contenthigher encapsulation efficiency and higher drying yield

The systematic approach used for the study of 120573-carotenemicroencapsulation process by spray drying may be easilyapplied for other core and wall materials Further studies willfocus on release studies in several aqueous media and even-tually on the encapsulation of natural carotenoid extracts

Data Availability

The data used to support the findings of this study areincluded within the article

Conflicts of Interest

The authors declare that they have no conflicts of interest

Acknowledgments

This work was supported by Conselho Nacional de Desen-volvimento Cientıfico e TecnologicondashCNPq through theCiencia sem Fronteiras program (CSF) (Grant CSF 2062682014-9 to first author)The authors acknowledge the financialsupport from Fundacao para a Ciencia e a TecnologiaPortugal Project UIDAGR041292013

References

[1] M E Rodrıguez-Huezo R Pedroza-Islas L A Prado-Bar-ragan C I Beristain and E J Vernon-Carter ldquoMicroencapsu-lation by spray drying of multiple emulsions containing caro-tenoidsrdquo Journal of Food Science vol 69 no 7 pp 351ndash359 2004

[2] A V Rao and L G Rao ldquoCarotenoids and human healthrdquoPharmacological Research vol 55 no 3 pp 207ndash216 2007

[3] J Fiedor and K Burda ldquoPotential role of carotenoids as anti-oxidants in human health and diseaserdquo Nutrients vol 6 no 2pp 466ndash488 2014

[4] R Arimboor R B Natarajan K R Menon L P Chan-drasekhar and VMoorkoth ldquoRed pepper (Capsicum annuum)carotenoids as a source of natural food colors analysis andstabilitymdasha reviewrdquo Journal of Food Science and Technology vol52 no 3 pp 1258ndash1271 2015

[5] M H Walter and D Strack ldquoCarotenoids and their cleavageproducts Biosynthesis and functionsrdquoNatural Product Reportsvol 28 no 4 pp 663ndash692 2011

[6] A Kaczor M Baranska and K Czamara Carotenoids WileyOnline Library 2016

[7] A F Aissa M L P Bianchi J C Ribeiro et al ldquoComparativestudy of 120573-carotene and microencapsulated 120573-carotene Eval-uation of their genotoxic and antigenotoxic effectsrdquo Food andChemical Toxicology vol 50 no 5 pp 1418ndash1424 2012

[8] Z Al Tanoury A Piskunov and C Rochette-Egly ldquoVitamina and retinoid signaling Genomic and nongenomic effectsrdquoJournal of Lipid Research vol 54 no 7 pp 1761ndash1775 2013

[9] E G Donhowe F P Flores W L Kerr L Wicker and F KongldquoCharacterization and invitro bioavailability of 120573-caroteneEffects of microencapsulation method and food matrixrdquo LWT-Food Science and Technology vol 57 no 1 pp 42ndash48 2014

[10] K Gul A Tak A Singh et al ldquoChemistry encapsulation andhealth benefits of szlig-carotene-A reviewrdquo Cogent Food amp Agri-culture vol 1 no 1 Article ID 1018696 2015

10 International Journal of Food Science

[11] HW Kim J B Kim S Poovan et al ldquoEffect of processing con-ditions on the content of cistrans carotene isomers as provita-min A carotenoids in Korean sweet potato varietiesrdquo Interna-tional Journal of Food Sciences and Nutrition vol 65 no 7 pp821ndash826 2014

[12] C Qian E A Decker H Xiao and D J McClements ldquoNano-emulsion delivery systems Influence of carrier oil on 120573-caro-tene bioaccessibilityrdquo Food Chemistry vol 135 no 3 pp 1440ndash1447 2012

[13] J C Spada L D F Marczak I C Tessaro and C P Z NorenaldquoMicroencapsulation of 120573-carotene using native pinhao starchmodified pinhao starch and gelatin by freeze-dryingrdquo Interna-tional Journal of Food Science amp Technology vol 47 no 1 pp186ndash194 2012

[14] G Zakynthinos and T Varzakas ldquoCarotenoids From plants tofood industryrdquo Current Research in Nutrition and Food Sciencevol 4 no 1 pp 38ndash51 2016

[15] R Liang Q Huang J Ma C F Shoemaker and F ZhongldquoEffect of relative humidity on the store stability of spray-driedbeta-carotene nanoemulsionsrdquo Food Hydrocolloids vol 33 no2 pp 225ndash233 2013

[16] C Saenz S Tapia J Chavez and P Robert ldquoMicroencapsula-tion by spray drying of bioactive compounds from cactus pear(Opuntia ficus-indica)rdquo Food Chemistry vol 114 no 2 pp 616ndash622 2009

[17] S AkhavanMahdavi SM Jafari E Assadpoor andDDehnadldquoMicroencapsulation optimization of natural anthocyaninswith maltodextrin gum Arabic and gelatinrdquo InternationalJournal of Biological Macromolecules vol 85 pp 379ndash385 2016

[18] N V N Jyothi P M Prasanna S N Sakarkar K S PrabhaP S Ramaiah and G Y Srawan ldquoMicroencapsulation tech-niques factors influencing encapsulation efficiencyrdquo Journal ofMicroencapsulation vol 27 no 3 pp 187ndash197 2010

[19] S M Jafari E Assadpoor Y He and B Bhandari ldquoEncapsu-lation efficiency of food flavours and oils during spray dryingrdquoDrying Technology vol 26 no 7 pp 816ndash835 2008

[20] S C Samantha A S Bruna R M Adriana B Fabio A RSandro and R C Aline ldquoDrying by spray drying in the foodindustry Micro-encapsulation process parameters and maincarriers usedrdquo African Journal of Food Science vol 9 no 9 pp462ndash470 2015

[21] T C Kha M H Nguyen P D Roach and C E StathopoulosldquoMicroencapsulation of Gac oil Optimisation of spray dryingconditions using response surface methodologyrdquo Powder Tech-nology vol 264 pp 298ndash309 2014

[22] E Janiszewska-Turak ldquoCarotenoids microencapsulation byspray drying method and supercritical micronizationrdquo FoodResearch International vol 99 pp 891ndash901 2017

[23] A Goncalves B N Estevinho and F Rocha ldquoDesign andcharacterization of controlled-release vitamin A microparticlesprepared by a spray-drying processrdquo Powder Technology vol305 pp 411ndash417 2017

[24] MOrdonez and AHerrera ldquoMorphologic and stability cassavastarch matrices for encapsulating limonene by spray dryingrdquoPowder Technology vol 253 pp 89ndash97 2014

[25] S-M Jafari K Mahdavi-Khazaei and A Hemmati-KakhkildquoMicroencapsulation of saffron petal anthocyanins with cressseed gum compared with Arabic gum through freeze dryingrdquoCarbohydrate Polymers vol 140 pp 20ndash25 2016

[26] M P Rascon C I Beristain H S Garcıa and M A Sal-gado ldquoCarotenoid retention and storage stability of spray-dried encapsulated paprika oleoresin using gum Arabic and

Soy protein isolate as wall materialsrdquo LWT- Food Science andTechnology vol 44 no 2 pp 549ndash557 2011

[27] GA Rocha C S Favaro-Trindade andC R F Grosso ldquoMicro-encapsulation of lycopene by spray drying Characterizationstability and application of microcapsulesrdquo Food and Bioprod-ucts Processing vol 90 no 1 pp 37ndash42 2012

[28] Q Shen and S Y Quek ldquoMicroencapsulation of astaxanthinwith blends of milk protein and fiber by spray dryingrdquo Journalof Food Engineering vol 123 pp 165ndash171 2014

[29] A M Goula and K G Adamopoulos ldquoA new technique forspray-dried encapsulation of lycopenerdquoDrying Technology vol30 no 6 pp 641ndash652 2012

[30] J Loksuwan ldquoCharacteristics of microencapsulated 120573-caroteneformed by spray drying with modified tapioca starch nativetapioca starch andmaltodextrinrdquoFoodHydrocolloids vol 21 no5-6 pp 928ndash935 2007

[31] A A Santana L E Kurozawa R A de Oliveira and K JPark ldquoInfluence of Process Conditions on the PhysicochemicalProperties of Pequi Powder Produced by Spray Dryingrdquo DryingTechnology vol 31 no 7 pp 825ndash836 2013

[32] D Troya D S Tupuna-Yerovi and J Ruales ldquoEffects of WallMaterials and Operating Parameters on Physicochemical Pro-perties Process Efficiency and Total Carotenoid Content ofMicroencapsulated Banana Passionfruit Pulp (Passiflora tri-partita var mollissima) by Spray-Dryingrdquo Food and BioprocessTechnology vol 11 no 10 pp 1828ndash1839 2018

[33] D C Montgomery Design and Analysis of Experiments JohnWiley amp Sons 8th edition 2012

[34] M do S M Rufino R Alves E de Brito et al MetodologiaCientıfica Determinacao da Atividade Antioxidante Total emFrutas pela Captura do Radical Livre ABTS ComunicadoTecnico (Embrapa Agroindustria Tropical Online) 2007

[35] N Nenadis L-F Wang M Tsimidou and H-Y Zhang ldquoEsti-mation of scavenging activity of phenolic compounds using theABTS∙+ assayrdquo Journal of Agricultural and Food Chemistry vol52 no 15 pp 4669ndash4674 2004

[36] C A Di Battista D ConstenlaM V Ramırez-Rigo and J PinaldquoThe use of Arabic gum maltodextrin and surfactants in themicroencapsulation of phytosterols by spray dryingrdquo PowderTechnology vol 286 pp 193ndash201 2015

[37] C A Schneider W S Rasband and K W Eliceiri ldquoNIH Imageto ImageJ 25 years of image analysisrdquo Nature Methods vol 9no 7 pp 671ndash675 2012

[38] S Shamaei S S Seiiedlou M Aghbashlo E Tsotsas and AKharaghani ldquoMicroencapsulation of walnut oil by spray dry-ing effects of wall material and drying conditions on physico-chemical properties of microcapsulesrdquo Innovative Food Scienceand Emerging Technologies vol 39 pp 101ndash112 2017

[39] L Medina-Torres R Santiago-Adame F Calderas et alldquoMicroencapsulation by spray drying of laurel infusions (Litseaglaucescens) with maltodextrinrdquo Industrial Crops and Productsvol 90 pp 1ndash8 2016

[40] S Beirao-da-Costa C Duarte A I Bourbon et al ldquoInulinpotential for encapsulation and controlled delivery of Oreganoessential oilrdquo Food Hydrocolloids vol 33 no 2 pp 199ndash2062013

[41] R Santiago-Adame L Medina-Torres J A Gallegos-Infante etal ldquoSpray drying-microencapsulation of cinnamon infusions(Cinnamomum zeylanicum) with maltodextrinrdquo LWT- FoodScience and Technology vol 64 no 2 pp 571ndash577 2015

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

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Page 6: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

6 International Journal of Food Science

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(a)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

10

20

30

40

50

60

Rela

tive f

requ

ency

()

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

(b)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(c)

Particle size (m)

[0-5[

[5-10

[

[10-1

5[

[15-2

0[

[20-2

5[

0

20

40

60

80

100

Cum

ulat

ive f

requ

ency

()

0

10

20

30

40

50

Rela

tive f

requ

ency

()

(d)

Figure 3 Relative frequency (bars) and cumulative frequency (line) equivalent to the diameter of microparticles (a) 94 AG 1232∘C (b)94 AG 1868∘C (c) 5 AG 155∘C (d) 35 AG 155∘C

Table 2 Second-order polynomial equations for each response variable

Equation R2 RAdj2

EE = minus48699 lowast + 03036AG minus 0001AG2 + 0710T lowast minus 0002T2 lowast minus 0003AGT 087 074DY = minus175962 lowast + 4222AG lowast minus 0097AG2 lowast + 2245T lowast minus 0007T2 lowast minus 0004AGT 085 071LC = 56961ndash2808AG lowast + 0069AG2 lowast minus 0257T + 00025T2 lowast minus 00003AGT 091 082AG arabic gum () T temperature (∘C) EE encapsulation efficiency () DY drying yield () LC loading capacity (mg 120573-carotenegminus1particles)lowastAffectingsignificantly the response variable (pgt005)

fit (p gt 005) relative to pure error was not significant at 95of confidence level The expected errors of the models on theprediction of the responses were estimated to be 76 72and 127 for LC EE and DY respectively Figures 4(a) 4(b)and 5 show the 3-dimensional response surfaces that illustratethe effects of arabic gum concentration (AG ) and dryinginlet temperature (T ∘C) on the responses studied

321 Encapsulation Efficiency and Loading Capacity Theencapsulation efficiency values of 120573-carotenewith arabic gum

ranged between 62 and 160 and the loading capacity valuesranged from 119 to 336mg120573-carotenegminus1particles as shownin Table 1 Similar results were found by Rocha Favaro-Trindade [27] uponmicroencapsulation of lycopene inmodi-fied starch that found an EE around 21 and by Botrel Borges[54] who microencapsulated oregano oil using a mixtureof arabic gum maltodextrin and modified starch as wallmaterial by spray drying found an EE between 51 and 339

As seen in Figures 4(a) and 4(b) the increase in dryingtemperature and decrease in arabic gum concentration lead

International Journal of Food Science 7

18

16

14

12

10

8

6

4

200

180

160

140

1205

1015

2025

3035

EncapsulationEffi

ciency ()

Temperature ( ∘C) Arabic gum ()

(a)

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

45

40

35

30

25

20

15

10

Loading Capacity

(mg-caroteneg - 1particles)

(b)

Figure 4 Response surface fitted to (a) encapsulation efficiency and (b) loading capacity as a function of Arabic gum concentration anddrying inlet temperature

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

50

40

30

20

10

0

Drying yield (

)

Figure 5 Response surface fitted to drying yield as a function ofarabic gum concentration and drying

to an increase in the EE Regarding LC higher values wereobserved at both ends of the arabic gum concentrationthat is when the lowest (5) and the highest concentration(35) of the wall material were used In addition when thedrying temperature increased the loading capacity was alsoincreased The same behaviour was reported by Ferrari Ger-mer [50] in microparticles of blackberry using maltodextrinas wall material

According to Jafari Assadpoor [19] the encapsulationefficiency is influenced by the drying conditions emulsion

and bioactive compound characteristics and the wall materialproperties Low encapsulation efficiency value could be dueto 120573-carotene being extremely sensitive to environmentalfactors such as exposure to heat light and oxygen duringencapsulation processing

The experimental data obtained of the encapsulation effi-ciency and loading capacity of the particles were adjusted tothe second-order polynomialmodelwith a satisfactory coeffi-cient of determination (Table 2) Both independent variableshad a significant effect on these responses Arabic gumconcentration had a positive quadratic effect on the loadingcapacity of the microparticles whereas for the encapsulationefficiency arabic gum concentration showed a linear negativeeffect In relation to the drying inlet temperature a positivelinear and quadratic negative effect on the encapsulation effi-ciency and a positive linear effect on the loading capacitywereobserved However the interaction coefficient was found tobe nonsignificant indicating that there was no interactionbetween the independent variables on the EE of particles

The drying temperature is directly proportional to theevaporation rate and inversely proportional to the finalwater content of the dried microparticles At high dryingtemperatures there is a higher evaporation rate of water onthe droplet surface which leads to the rapid formation of asemipermeable membrane resulting in the protection of therelease of the bioactive compounds during the drying processand consequently in a higher bioactive retention Howeverhigher drying temperatures could cause cracks and fissureson the surface of the particles leading to loss of the bioactivecompound [19 21]

Wall material concentration is also a factor that affectsthe retention of the bioactive compounds due to their vis-cosity properties in the feed solution Some researchers have

8 International Journal of Food Science

reported that the wall material concentration has a positiveeffect on the encapsulation efficiency ie the increase ofsolids content in the feed increases bioactive retention [21 5556] This behaviour could be related to the reduction of thetime required to form a surface crust in the atomized dropletsin the initial drying process when the solids concentration inthe feed solution increases This rapidly formed crust is notpermeable to compounds thereby protecting the bioactivefrom oxidation [57 58]

However too high viscosity of the feed solutions delaysthe formation of discrete particles during spray dryingwhereas a low viscosity in feed delays the formation of asemipermeable surface crust favouring further losses of thebioactive compounds [59] Therefore according to Reinec-cius [60] each wall material has its ideal feed concentrationto obtain higher encapsulation efficiency which is basedon the solubility and viscosity of the feed solution In thiswork an ideal arabic gum concentration of 74 was foundfor higher values of encapsulation efficiency and loadingcapacity Fernandes Marques [57] who evaluated the effectof total solids concentration on the microencapsulation ofrosemary essential oil by spray drying using maltodextrinand modified starch (11) as wall materials found higherencapsulation efficiency when a concentration of the wallmaterial of 22 was used which was reported as the idealconcentration for maltodextrin as wall material

322 Drying Yield Drying yield of the spray drying processis directly related to the cost of production and efficiencythus it is an important indicator that the industry considersin its production line [49 61] According to Nunes andMercadante [62] and Rutz Borges [63] drying yield isinfluenced by both the equipment settings (feed rate feedinlet and outlet temperature and flow rate) and dryingconditions (type and wall material concentration)

In this study a second-order model was fitted to theexperimental data of the drying yield with acceptable coef-ficient of determination and Table 2 shows that both inde-pendent variables arabic gum concentration and the dryinginlet temperature had a significant negative quadratic effecton the drying yield According to Table 1 the drying yields of120573-carotene with arabic gum ranged between 159 and 439Other researchers have found values of drying yield around50 Roccia Martınez [64] who studied the microencapsu-lation of the sunflower oil by spray drying using maltodextrinas a carrier agent found drying yield values that ranged from544 to 3988 and Santana Kurozawa [31] produced arabicgum microparticles with pulp pequi extract by spray dryingand obtained a drying yield values between 258 and 561

Low drying yield in the spray drying process is mostlydue to retention of the powder in the drying chamber wallcyclone inefficient in collecting fine particles and the highviscosity of the feed solution This powder retention problemcauses considerable economic loss and it is not cost-effectivefor industry as there would be frequent interruptions tothe dryer cleaning besides affecting the quality of the finalproduct However drying yield in the microencapsulationtechnique could be improved by modifying the spray dryingconditions in order to decrease the adhesion of particles to

the drying chamber wall [64ndash66] According to Tontul andTopuz [49] and Jayasundera Adhikari [67] the mechanicalscraping of the drying chamber wall introduction of coldair from the bottom and the use of low temperature lowhumidity air are some examples of process-based approachesthat could increase drying yield

As shown in Figure 5 as the drying temperature andthe arabic gum concentration increased the drying yieldalso increased until a maximum value was achieved Afterthis value decreases in the drying yield were observed evenwith the increase of both independent variables The highestdrying yield value was found for the sample with 20 GAdried at 155∘C

Chong and Wong [68] also found an optimum dosageof the wall material concentration (30 maltodextrin) andtemperature value (180∘C) that maximized the drying yield(57) when producing sapodilla puree particles by spraydrying using different maltodextrin concentrations (10-50wv) The authors referred that increasing the wall materialconcentration above the optimum value leads to an increaseviscosity of the feed solution thereby negatively affecting thedrying yield

323 Antioxidant Activity The AA values of encapsulated120573-carotene range from 005 to 078 120583mol troloxmgminus1120573-carotene whereas the commercial 120573-carotene before encap-sulation possessed 235 120583mol troloxmgminus1120573-carotene Thelower antioxidant activity after the encapsulation may berelated not only to the encapsulation process itself but alsoto the incomplete extraction of the encapsulated moleculesbefore antioxidant activity measurement This decrease inantioxidant activity after the spray drying process was alsoobserved for example by Franceschinis Salvatori [69] in themicroencapsulation of blackberry juices with maltodextrinand Hee Tan [70] in virgin coconut oil microparticles in amixture of maltodextrin arabic gum sodium caseinate andwhey protein concentrate

The data obtained for the antioxidant activity did notfit the second-order polynomial model though from theresults of Table 1 the two independent variables studiedarabic gum concentration and drying inlet temperatureaffected antioxidant activity of the encapsulated moleculessince an AA increase was observed when the temperaturedecreased (runs 4-3 2-1 and 11-10) and when the arabic gumconcentration increased (runs 1-3 2-4 8-9)

Other researchers have also studied the influence ofdrying inlet temperature and wall material on AA of theparticles Kha Nguyen [71] studied the effects of varyingmaltodextrin concentrations and spray drying temperatureson the antioxidant activity of Gac fruit powder and theyreported that increasing the drying inlet temperature from120 to 200∘C showed a significant loss of AA Additionallywith increasing maltodextrin concentration from 20 to 30the loss of AA was also observed The authors explainedthat AA loss could be due to loss of antioxidant compoundspresent in Gac powder spray dried at high temperaturesMiravet Alacid [72] who evaluated the antioxidant activityof pomegranate juice powder produced by spray dryingusing prebiotic fibers and maltodextrin as wall material also

International Journal of Food Science 9

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

10

08

06

04

02

00

minus02

Desirability

Figure 6 Desirability surface for optimal conditions

observed that the increase of the drying inlet temperaturefrom 160 to 200∘C had a significant negative effect on theantioxidant activity for both wall materials studied

324 Optimization of Drying Process Conditions The desir-ability function was performed for the simultaneous opti-mization of the responses that fitted to the second-ordermodel (Table 2) and the desirability surface for optimalconditions is depicted in Figure 6 Desirability values higherthan 07 were considered indicating a good optimization ofthe experimental data of each response variable [73] Thebest conditions for the spray drying microencapsulation of 120573-carotene with arabic gum as wall material were determined inorder to obtain higher values for drying yield encapsulationefficiency and loading capacity

The inlet drying temperature of 173∘C and arabic gumconcentration of 119 are recommended as the ideal con-ditions for microencapsulation of 120573-carotene Under theseconditions the predicted EE DY and LC are 1562 3630and 2274 mg 120573-carotenegminus1particles respectively

4 Conclusions

Themicroencapsulation of120573-carotene in arabic gumby spraydrying was investigated The arabic gum concentration anddrying inlet temperature influenced the drying yield encap-sulation efficiency and load capacity responses Regardingthe AA the antioxidant activity of 120573-carotene was reducedwhen microencapsulated at high temperatures (200∘C) inrelation to low temperatures (110∘C)

SEM analysis showed that the microparticles are micro-capsules Most of them presented a similar morphology amixture of smooth and wrinkled particles with a diameterlower than 10 120583m Increases in drying temperature favouredthe formation of smoother and larger particles

From the experimental conditions the drying inlet tem-perature of 173∘C and the arabic gum concentration of 119

were those that allow obtaining higher 120573-carotene contenthigher encapsulation efficiency and higher drying yield

The systematic approach used for the study of 120573-carotenemicroencapsulation process by spray drying may be easilyapplied for other core and wall materials Further studies willfocus on release studies in several aqueous media and even-tually on the encapsulation of natural carotenoid extracts

Data Availability

The data used to support the findings of this study areincluded within the article

Conflicts of Interest

The authors declare that they have no conflicts of interest

Acknowledgments

This work was supported by Conselho Nacional de Desen-volvimento Cientıfico e TecnologicondashCNPq through theCiencia sem Fronteiras program (CSF) (Grant CSF 2062682014-9 to first author)The authors acknowledge the financialsupport from Fundacao para a Ciencia e a TecnologiaPortugal Project UIDAGR041292013

References

[1] M E Rodrıguez-Huezo R Pedroza-Islas L A Prado-Bar-ragan C I Beristain and E J Vernon-Carter ldquoMicroencapsu-lation by spray drying of multiple emulsions containing caro-tenoidsrdquo Journal of Food Science vol 69 no 7 pp 351ndash359 2004

[2] A V Rao and L G Rao ldquoCarotenoids and human healthrdquoPharmacological Research vol 55 no 3 pp 207ndash216 2007

[3] J Fiedor and K Burda ldquoPotential role of carotenoids as anti-oxidants in human health and diseaserdquo Nutrients vol 6 no 2pp 466ndash488 2014

[4] R Arimboor R B Natarajan K R Menon L P Chan-drasekhar and VMoorkoth ldquoRed pepper (Capsicum annuum)carotenoids as a source of natural food colors analysis andstabilitymdasha reviewrdquo Journal of Food Science and Technology vol52 no 3 pp 1258ndash1271 2015

[5] M H Walter and D Strack ldquoCarotenoids and their cleavageproducts Biosynthesis and functionsrdquoNatural Product Reportsvol 28 no 4 pp 663ndash692 2011

[6] A Kaczor M Baranska and K Czamara Carotenoids WileyOnline Library 2016

[7] A F Aissa M L P Bianchi J C Ribeiro et al ldquoComparativestudy of 120573-carotene and microencapsulated 120573-carotene Eval-uation of their genotoxic and antigenotoxic effectsrdquo Food andChemical Toxicology vol 50 no 5 pp 1418ndash1424 2012

[8] Z Al Tanoury A Piskunov and C Rochette-Egly ldquoVitamina and retinoid signaling Genomic and nongenomic effectsrdquoJournal of Lipid Research vol 54 no 7 pp 1761ndash1775 2013

[9] E G Donhowe F P Flores W L Kerr L Wicker and F KongldquoCharacterization and invitro bioavailability of 120573-caroteneEffects of microencapsulation method and food matrixrdquo LWT-Food Science and Technology vol 57 no 1 pp 42ndash48 2014

[10] K Gul A Tak A Singh et al ldquoChemistry encapsulation andhealth benefits of szlig-carotene-A reviewrdquo Cogent Food amp Agri-culture vol 1 no 1 Article ID 1018696 2015

10 International Journal of Food Science

[11] HW Kim J B Kim S Poovan et al ldquoEffect of processing con-ditions on the content of cistrans carotene isomers as provita-min A carotenoids in Korean sweet potato varietiesrdquo Interna-tional Journal of Food Sciences and Nutrition vol 65 no 7 pp821ndash826 2014

[12] C Qian E A Decker H Xiao and D J McClements ldquoNano-emulsion delivery systems Influence of carrier oil on 120573-caro-tene bioaccessibilityrdquo Food Chemistry vol 135 no 3 pp 1440ndash1447 2012

[13] J C Spada L D F Marczak I C Tessaro and C P Z NorenaldquoMicroencapsulation of 120573-carotene using native pinhao starchmodified pinhao starch and gelatin by freeze-dryingrdquo Interna-tional Journal of Food Science amp Technology vol 47 no 1 pp186ndash194 2012

[14] G Zakynthinos and T Varzakas ldquoCarotenoids From plants tofood industryrdquo Current Research in Nutrition and Food Sciencevol 4 no 1 pp 38ndash51 2016

[15] R Liang Q Huang J Ma C F Shoemaker and F ZhongldquoEffect of relative humidity on the store stability of spray-driedbeta-carotene nanoemulsionsrdquo Food Hydrocolloids vol 33 no2 pp 225ndash233 2013

[16] C Saenz S Tapia J Chavez and P Robert ldquoMicroencapsula-tion by spray drying of bioactive compounds from cactus pear(Opuntia ficus-indica)rdquo Food Chemistry vol 114 no 2 pp 616ndash622 2009

[17] S AkhavanMahdavi SM Jafari E Assadpoor andDDehnadldquoMicroencapsulation optimization of natural anthocyaninswith maltodextrin gum Arabic and gelatinrdquo InternationalJournal of Biological Macromolecules vol 85 pp 379ndash385 2016

[18] N V N Jyothi P M Prasanna S N Sakarkar K S PrabhaP S Ramaiah and G Y Srawan ldquoMicroencapsulation tech-niques factors influencing encapsulation efficiencyrdquo Journal ofMicroencapsulation vol 27 no 3 pp 187ndash197 2010

[19] S M Jafari E Assadpoor Y He and B Bhandari ldquoEncapsu-lation efficiency of food flavours and oils during spray dryingrdquoDrying Technology vol 26 no 7 pp 816ndash835 2008

[20] S C Samantha A S Bruna R M Adriana B Fabio A RSandro and R C Aline ldquoDrying by spray drying in the foodindustry Micro-encapsulation process parameters and maincarriers usedrdquo African Journal of Food Science vol 9 no 9 pp462ndash470 2015

[21] T C Kha M H Nguyen P D Roach and C E StathopoulosldquoMicroencapsulation of Gac oil Optimisation of spray dryingconditions using response surface methodologyrdquo Powder Tech-nology vol 264 pp 298ndash309 2014

[22] E Janiszewska-Turak ldquoCarotenoids microencapsulation byspray drying method and supercritical micronizationrdquo FoodResearch International vol 99 pp 891ndash901 2017

[23] A Goncalves B N Estevinho and F Rocha ldquoDesign andcharacterization of controlled-release vitamin A microparticlesprepared by a spray-drying processrdquo Powder Technology vol305 pp 411ndash417 2017

[24] MOrdonez and AHerrera ldquoMorphologic and stability cassavastarch matrices for encapsulating limonene by spray dryingrdquoPowder Technology vol 253 pp 89ndash97 2014

[25] S-M Jafari K Mahdavi-Khazaei and A Hemmati-KakhkildquoMicroencapsulation of saffron petal anthocyanins with cressseed gum compared with Arabic gum through freeze dryingrdquoCarbohydrate Polymers vol 140 pp 20ndash25 2016

[26] M P Rascon C I Beristain H S Garcıa and M A Sal-gado ldquoCarotenoid retention and storage stability of spray-dried encapsulated paprika oleoresin using gum Arabic and

Soy protein isolate as wall materialsrdquo LWT- Food Science andTechnology vol 44 no 2 pp 549ndash557 2011

[27] GA Rocha C S Favaro-Trindade andC R F Grosso ldquoMicro-encapsulation of lycopene by spray drying Characterizationstability and application of microcapsulesrdquo Food and Bioprod-ucts Processing vol 90 no 1 pp 37ndash42 2012

[28] Q Shen and S Y Quek ldquoMicroencapsulation of astaxanthinwith blends of milk protein and fiber by spray dryingrdquo Journalof Food Engineering vol 123 pp 165ndash171 2014

[29] A M Goula and K G Adamopoulos ldquoA new technique forspray-dried encapsulation of lycopenerdquoDrying Technology vol30 no 6 pp 641ndash652 2012

[30] J Loksuwan ldquoCharacteristics of microencapsulated 120573-caroteneformed by spray drying with modified tapioca starch nativetapioca starch andmaltodextrinrdquoFoodHydrocolloids vol 21 no5-6 pp 928ndash935 2007

[31] A A Santana L E Kurozawa R A de Oliveira and K JPark ldquoInfluence of Process Conditions on the PhysicochemicalProperties of Pequi Powder Produced by Spray Dryingrdquo DryingTechnology vol 31 no 7 pp 825ndash836 2013

[32] D Troya D S Tupuna-Yerovi and J Ruales ldquoEffects of WallMaterials and Operating Parameters on Physicochemical Pro-perties Process Efficiency and Total Carotenoid Content ofMicroencapsulated Banana Passionfruit Pulp (Passiflora tri-partita var mollissima) by Spray-Dryingrdquo Food and BioprocessTechnology vol 11 no 10 pp 1828ndash1839 2018

[33] D C Montgomery Design and Analysis of Experiments JohnWiley amp Sons 8th edition 2012

[34] M do S M Rufino R Alves E de Brito et al MetodologiaCientıfica Determinacao da Atividade Antioxidante Total emFrutas pela Captura do Radical Livre ABTS ComunicadoTecnico (Embrapa Agroindustria Tropical Online) 2007

[35] N Nenadis L-F Wang M Tsimidou and H-Y Zhang ldquoEsti-mation of scavenging activity of phenolic compounds using theABTS∙+ assayrdquo Journal of Agricultural and Food Chemistry vol52 no 15 pp 4669ndash4674 2004

[36] C A Di Battista D ConstenlaM V Ramırez-Rigo and J PinaldquoThe use of Arabic gum maltodextrin and surfactants in themicroencapsulation of phytosterols by spray dryingrdquo PowderTechnology vol 286 pp 193ndash201 2015

[37] C A Schneider W S Rasband and K W Eliceiri ldquoNIH Imageto ImageJ 25 years of image analysisrdquo Nature Methods vol 9no 7 pp 671ndash675 2012

[38] S Shamaei S S Seiiedlou M Aghbashlo E Tsotsas and AKharaghani ldquoMicroencapsulation of walnut oil by spray dry-ing effects of wall material and drying conditions on physico-chemical properties of microcapsulesrdquo Innovative Food Scienceand Emerging Technologies vol 39 pp 101ndash112 2017

[39] L Medina-Torres R Santiago-Adame F Calderas et alldquoMicroencapsulation by spray drying of laurel infusions (Litseaglaucescens) with maltodextrinrdquo Industrial Crops and Productsvol 90 pp 1ndash8 2016

[40] S Beirao-da-Costa C Duarte A I Bourbon et al ldquoInulinpotential for encapsulation and controlled delivery of Oreganoessential oilrdquo Food Hydrocolloids vol 33 no 2 pp 199ndash2062013

[41] R Santiago-Adame L Medina-Torres J A Gallegos-Infante etal ldquoSpray drying-microencapsulation of cinnamon infusions(Cinnamomum zeylanicum) with maltodextrinrdquo LWT- FoodScience and Technology vol 64 no 2 pp 571ndash577 2015

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

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Page 7: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

International Journal of Food Science 7

18

16

14

12

10

8

6

4

200

180

160

140

1205

1015

2025

3035

EncapsulationEffi

ciency ()

Temperature ( ∘C) Arabic gum ()

(a)

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

45

40

35

30

25

20

15

10

Loading Capacity

(mg-caroteneg - 1particles)

(b)

Figure 4 Response surface fitted to (a) encapsulation efficiency and (b) loading capacity as a function of Arabic gum concentration anddrying inlet temperature

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

50

40

30

20

10

0

Drying yield (

)

Figure 5 Response surface fitted to drying yield as a function ofarabic gum concentration and drying

to an increase in the EE Regarding LC higher values wereobserved at both ends of the arabic gum concentrationthat is when the lowest (5) and the highest concentration(35) of the wall material were used In addition when thedrying temperature increased the loading capacity was alsoincreased The same behaviour was reported by Ferrari Ger-mer [50] in microparticles of blackberry using maltodextrinas wall material

According to Jafari Assadpoor [19] the encapsulationefficiency is influenced by the drying conditions emulsion

and bioactive compound characteristics and the wall materialproperties Low encapsulation efficiency value could be dueto 120573-carotene being extremely sensitive to environmentalfactors such as exposure to heat light and oxygen duringencapsulation processing

The experimental data obtained of the encapsulation effi-ciency and loading capacity of the particles were adjusted tothe second-order polynomialmodelwith a satisfactory coeffi-cient of determination (Table 2) Both independent variableshad a significant effect on these responses Arabic gumconcentration had a positive quadratic effect on the loadingcapacity of the microparticles whereas for the encapsulationefficiency arabic gum concentration showed a linear negativeeffect In relation to the drying inlet temperature a positivelinear and quadratic negative effect on the encapsulation effi-ciency and a positive linear effect on the loading capacitywereobserved However the interaction coefficient was found tobe nonsignificant indicating that there was no interactionbetween the independent variables on the EE of particles

The drying temperature is directly proportional to theevaporation rate and inversely proportional to the finalwater content of the dried microparticles At high dryingtemperatures there is a higher evaporation rate of water onthe droplet surface which leads to the rapid formation of asemipermeable membrane resulting in the protection of therelease of the bioactive compounds during the drying processand consequently in a higher bioactive retention Howeverhigher drying temperatures could cause cracks and fissureson the surface of the particles leading to loss of the bioactivecompound [19 21]

Wall material concentration is also a factor that affectsthe retention of the bioactive compounds due to their vis-cosity properties in the feed solution Some researchers have

8 International Journal of Food Science

reported that the wall material concentration has a positiveeffect on the encapsulation efficiency ie the increase ofsolids content in the feed increases bioactive retention [21 5556] This behaviour could be related to the reduction of thetime required to form a surface crust in the atomized dropletsin the initial drying process when the solids concentration inthe feed solution increases This rapidly formed crust is notpermeable to compounds thereby protecting the bioactivefrom oxidation [57 58]

However too high viscosity of the feed solutions delaysthe formation of discrete particles during spray dryingwhereas a low viscosity in feed delays the formation of asemipermeable surface crust favouring further losses of thebioactive compounds [59] Therefore according to Reinec-cius [60] each wall material has its ideal feed concentrationto obtain higher encapsulation efficiency which is basedon the solubility and viscosity of the feed solution In thiswork an ideal arabic gum concentration of 74 was foundfor higher values of encapsulation efficiency and loadingcapacity Fernandes Marques [57] who evaluated the effectof total solids concentration on the microencapsulation ofrosemary essential oil by spray drying using maltodextrinand modified starch (11) as wall materials found higherencapsulation efficiency when a concentration of the wallmaterial of 22 was used which was reported as the idealconcentration for maltodextrin as wall material

322 Drying Yield Drying yield of the spray drying processis directly related to the cost of production and efficiencythus it is an important indicator that the industry considersin its production line [49 61] According to Nunes andMercadante [62] and Rutz Borges [63] drying yield isinfluenced by both the equipment settings (feed rate feedinlet and outlet temperature and flow rate) and dryingconditions (type and wall material concentration)

In this study a second-order model was fitted to theexperimental data of the drying yield with acceptable coef-ficient of determination and Table 2 shows that both inde-pendent variables arabic gum concentration and the dryinginlet temperature had a significant negative quadratic effecton the drying yield According to Table 1 the drying yields of120573-carotene with arabic gum ranged between 159 and 439Other researchers have found values of drying yield around50 Roccia Martınez [64] who studied the microencapsu-lation of the sunflower oil by spray drying using maltodextrinas a carrier agent found drying yield values that ranged from544 to 3988 and Santana Kurozawa [31] produced arabicgum microparticles with pulp pequi extract by spray dryingand obtained a drying yield values between 258 and 561

Low drying yield in the spray drying process is mostlydue to retention of the powder in the drying chamber wallcyclone inefficient in collecting fine particles and the highviscosity of the feed solution This powder retention problemcauses considerable economic loss and it is not cost-effectivefor industry as there would be frequent interruptions tothe dryer cleaning besides affecting the quality of the finalproduct However drying yield in the microencapsulationtechnique could be improved by modifying the spray dryingconditions in order to decrease the adhesion of particles to

the drying chamber wall [64ndash66] According to Tontul andTopuz [49] and Jayasundera Adhikari [67] the mechanicalscraping of the drying chamber wall introduction of coldair from the bottom and the use of low temperature lowhumidity air are some examples of process-based approachesthat could increase drying yield

As shown in Figure 5 as the drying temperature andthe arabic gum concentration increased the drying yieldalso increased until a maximum value was achieved Afterthis value decreases in the drying yield were observed evenwith the increase of both independent variables The highestdrying yield value was found for the sample with 20 GAdried at 155∘C

Chong and Wong [68] also found an optimum dosageof the wall material concentration (30 maltodextrin) andtemperature value (180∘C) that maximized the drying yield(57) when producing sapodilla puree particles by spraydrying using different maltodextrin concentrations (10-50wv) The authors referred that increasing the wall materialconcentration above the optimum value leads to an increaseviscosity of the feed solution thereby negatively affecting thedrying yield

323 Antioxidant Activity The AA values of encapsulated120573-carotene range from 005 to 078 120583mol troloxmgminus1120573-carotene whereas the commercial 120573-carotene before encap-sulation possessed 235 120583mol troloxmgminus1120573-carotene Thelower antioxidant activity after the encapsulation may berelated not only to the encapsulation process itself but alsoto the incomplete extraction of the encapsulated moleculesbefore antioxidant activity measurement This decrease inantioxidant activity after the spray drying process was alsoobserved for example by Franceschinis Salvatori [69] in themicroencapsulation of blackberry juices with maltodextrinand Hee Tan [70] in virgin coconut oil microparticles in amixture of maltodextrin arabic gum sodium caseinate andwhey protein concentrate

The data obtained for the antioxidant activity did notfit the second-order polynomial model though from theresults of Table 1 the two independent variables studiedarabic gum concentration and drying inlet temperatureaffected antioxidant activity of the encapsulated moleculessince an AA increase was observed when the temperaturedecreased (runs 4-3 2-1 and 11-10) and when the arabic gumconcentration increased (runs 1-3 2-4 8-9)

Other researchers have also studied the influence ofdrying inlet temperature and wall material on AA of theparticles Kha Nguyen [71] studied the effects of varyingmaltodextrin concentrations and spray drying temperatureson the antioxidant activity of Gac fruit powder and theyreported that increasing the drying inlet temperature from120 to 200∘C showed a significant loss of AA Additionallywith increasing maltodextrin concentration from 20 to 30the loss of AA was also observed The authors explainedthat AA loss could be due to loss of antioxidant compoundspresent in Gac powder spray dried at high temperaturesMiravet Alacid [72] who evaluated the antioxidant activityof pomegranate juice powder produced by spray dryingusing prebiotic fibers and maltodextrin as wall material also

International Journal of Food Science 9

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

10

08

06

04

02

00

minus02

Desirability

Figure 6 Desirability surface for optimal conditions

observed that the increase of the drying inlet temperaturefrom 160 to 200∘C had a significant negative effect on theantioxidant activity for both wall materials studied

324 Optimization of Drying Process Conditions The desir-ability function was performed for the simultaneous opti-mization of the responses that fitted to the second-ordermodel (Table 2) and the desirability surface for optimalconditions is depicted in Figure 6 Desirability values higherthan 07 were considered indicating a good optimization ofthe experimental data of each response variable [73] Thebest conditions for the spray drying microencapsulation of 120573-carotene with arabic gum as wall material were determined inorder to obtain higher values for drying yield encapsulationefficiency and loading capacity

The inlet drying temperature of 173∘C and arabic gumconcentration of 119 are recommended as the ideal con-ditions for microencapsulation of 120573-carotene Under theseconditions the predicted EE DY and LC are 1562 3630and 2274 mg 120573-carotenegminus1particles respectively

4 Conclusions

Themicroencapsulation of120573-carotene in arabic gumby spraydrying was investigated The arabic gum concentration anddrying inlet temperature influenced the drying yield encap-sulation efficiency and load capacity responses Regardingthe AA the antioxidant activity of 120573-carotene was reducedwhen microencapsulated at high temperatures (200∘C) inrelation to low temperatures (110∘C)

SEM analysis showed that the microparticles are micro-capsules Most of them presented a similar morphology amixture of smooth and wrinkled particles with a diameterlower than 10 120583m Increases in drying temperature favouredthe formation of smoother and larger particles

From the experimental conditions the drying inlet tem-perature of 173∘C and the arabic gum concentration of 119

were those that allow obtaining higher 120573-carotene contenthigher encapsulation efficiency and higher drying yield

The systematic approach used for the study of 120573-carotenemicroencapsulation process by spray drying may be easilyapplied for other core and wall materials Further studies willfocus on release studies in several aqueous media and even-tually on the encapsulation of natural carotenoid extracts

Data Availability

The data used to support the findings of this study areincluded within the article

Conflicts of Interest

The authors declare that they have no conflicts of interest

Acknowledgments

This work was supported by Conselho Nacional de Desen-volvimento Cientıfico e TecnologicondashCNPq through theCiencia sem Fronteiras program (CSF) (Grant CSF 2062682014-9 to first author)The authors acknowledge the financialsupport from Fundacao para a Ciencia e a TecnologiaPortugal Project UIDAGR041292013

References

[1] M E Rodrıguez-Huezo R Pedroza-Islas L A Prado-Bar-ragan C I Beristain and E J Vernon-Carter ldquoMicroencapsu-lation by spray drying of multiple emulsions containing caro-tenoidsrdquo Journal of Food Science vol 69 no 7 pp 351ndash359 2004

[2] A V Rao and L G Rao ldquoCarotenoids and human healthrdquoPharmacological Research vol 55 no 3 pp 207ndash216 2007

[3] J Fiedor and K Burda ldquoPotential role of carotenoids as anti-oxidants in human health and diseaserdquo Nutrients vol 6 no 2pp 466ndash488 2014

[4] R Arimboor R B Natarajan K R Menon L P Chan-drasekhar and VMoorkoth ldquoRed pepper (Capsicum annuum)carotenoids as a source of natural food colors analysis andstabilitymdasha reviewrdquo Journal of Food Science and Technology vol52 no 3 pp 1258ndash1271 2015

[5] M H Walter and D Strack ldquoCarotenoids and their cleavageproducts Biosynthesis and functionsrdquoNatural Product Reportsvol 28 no 4 pp 663ndash692 2011

[6] A Kaczor M Baranska and K Czamara Carotenoids WileyOnline Library 2016

[7] A F Aissa M L P Bianchi J C Ribeiro et al ldquoComparativestudy of 120573-carotene and microencapsulated 120573-carotene Eval-uation of their genotoxic and antigenotoxic effectsrdquo Food andChemical Toxicology vol 50 no 5 pp 1418ndash1424 2012

[8] Z Al Tanoury A Piskunov and C Rochette-Egly ldquoVitamina and retinoid signaling Genomic and nongenomic effectsrdquoJournal of Lipid Research vol 54 no 7 pp 1761ndash1775 2013

[9] E G Donhowe F P Flores W L Kerr L Wicker and F KongldquoCharacterization and invitro bioavailability of 120573-caroteneEffects of microencapsulation method and food matrixrdquo LWT-Food Science and Technology vol 57 no 1 pp 42ndash48 2014

[10] K Gul A Tak A Singh et al ldquoChemistry encapsulation andhealth benefits of szlig-carotene-A reviewrdquo Cogent Food amp Agri-culture vol 1 no 1 Article ID 1018696 2015

10 International Journal of Food Science

[11] HW Kim J B Kim S Poovan et al ldquoEffect of processing con-ditions on the content of cistrans carotene isomers as provita-min A carotenoids in Korean sweet potato varietiesrdquo Interna-tional Journal of Food Sciences and Nutrition vol 65 no 7 pp821ndash826 2014

[12] C Qian E A Decker H Xiao and D J McClements ldquoNano-emulsion delivery systems Influence of carrier oil on 120573-caro-tene bioaccessibilityrdquo Food Chemistry vol 135 no 3 pp 1440ndash1447 2012

[13] J C Spada L D F Marczak I C Tessaro and C P Z NorenaldquoMicroencapsulation of 120573-carotene using native pinhao starchmodified pinhao starch and gelatin by freeze-dryingrdquo Interna-tional Journal of Food Science amp Technology vol 47 no 1 pp186ndash194 2012

[14] G Zakynthinos and T Varzakas ldquoCarotenoids From plants tofood industryrdquo Current Research in Nutrition and Food Sciencevol 4 no 1 pp 38ndash51 2016

[15] R Liang Q Huang J Ma C F Shoemaker and F ZhongldquoEffect of relative humidity on the store stability of spray-driedbeta-carotene nanoemulsionsrdquo Food Hydrocolloids vol 33 no2 pp 225ndash233 2013

[16] C Saenz S Tapia J Chavez and P Robert ldquoMicroencapsula-tion by spray drying of bioactive compounds from cactus pear(Opuntia ficus-indica)rdquo Food Chemistry vol 114 no 2 pp 616ndash622 2009

[17] S AkhavanMahdavi SM Jafari E Assadpoor andDDehnadldquoMicroencapsulation optimization of natural anthocyaninswith maltodextrin gum Arabic and gelatinrdquo InternationalJournal of Biological Macromolecules vol 85 pp 379ndash385 2016

[18] N V N Jyothi P M Prasanna S N Sakarkar K S PrabhaP S Ramaiah and G Y Srawan ldquoMicroencapsulation tech-niques factors influencing encapsulation efficiencyrdquo Journal ofMicroencapsulation vol 27 no 3 pp 187ndash197 2010

[19] S M Jafari E Assadpoor Y He and B Bhandari ldquoEncapsu-lation efficiency of food flavours and oils during spray dryingrdquoDrying Technology vol 26 no 7 pp 816ndash835 2008

[20] S C Samantha A S Bruna R M Adriana B Fabio A RSandro and R C Aline ldquoDrying by spray drying in the foodindustry Micro-encapsulation process parameters and maincarriers usedrdquo African Journal of Food Science vol 9 no 9 pp462ndash470 2015

[21] T C Kha M H Nguyen P D Roach and C E StathopoulosldquoMicroencapsulation of Gac oil Optimisation of spray dryingconditions using response surface methodologyrdquo Powder Tech-nology vol 264 pp 298ndash309 2014

[22] E Janiszewska-Turak ldquoCarotenoids microencapsulation byspray drying method and supercritical micronizationrdquo FoodResearch International vol 99 pp 891ndash901 2017

[23] A Goncalves B N Estevinho and F Rocha ldquoDesign andcharacterization of controlled-release vitamin A microparticlesprepared by a spray-drying processrdquo Powder Technology vol305 pp 411ndash417 2017

[24] MOrdonez and AHerrera ldquoMorphologic and stability cassavastarch matrices for encapsulating limonene by spray dryingrdquoPowder Technology vol 253 pp 89ndash97 2014

[25] S-M Jafari K Mahdavi-Khazaei and A Hemmati-KakhkildquoMicroencapsulation of saffron petal anthocyanins with cressseed gum compared with Arabic gum through freeze dryingrdquoCarbohydrate Polymers vol 140 pp 20ndash25 2016

[26] M P Rascon C I Beristain H S Garcıa and M A Sal-gado ldquoCarotenoid retention and storage stability of spray-dried encapsulated paprika oleoresin using gum Arabic and

Soy protein isolate as wall materialsrdquo LWT- Food Science andTechnology vol 44 no 2 pp 549ndash557 2011

[27] GA Rocha C S Favaro-Trindade andC R F Grosso ldquoMicro-encapsulation of lycopene by spray drying Characterizationstability and application of microcapsulesrdquo Food and Bioprod-ucts Processing vol 90 no 1 pp 37ndash42 2012

[28] Q Shen and S Y Quek ldquoMicroencapsulation of astaxanthinwith blends of milk protein and fiber by spray dryingrdquo Journalof Food Engineering vol 123 pp 165ndash171 2014

[29] A M Goula and K G Adamopoulos ldquoA new technique forspray-dried encapsulation of lycopenerdquoDrying Technology vol30 no 6 pp 641ndash652 2012

[30] J Loksuwan ldquoCharacteristics of microencapsulated 120573-caroteneformed by spray drying with modified tapioca starch nativetapioca starch andmaltodextrinrdquoFoodHydrocolloids vol 21 no5-6 pp 928ndash935 2007

[31] A A Santana L E Kurozawa R A de Oliveira and K JPark ldquoInfluence of Process Conditions on the PhysicochemicalProperties of Pequi Powder Produced by Spray Dryingrdquo DryingTechnology vol 31 no 7 pp 825ndash836 2013

[32] D Troya D S Tupuna-Yerovi and J Ruales ldquoEffects of WallMaterials and Operating Parameters on Physicochemical Pro-perties Process Efficiency and Total Carotenoid Content ofMicroencapsulated Banana Passionfruit Pulp (Passiflora tri-partita var mollissima) by Spray-Dryingrdquo Food and BioprocessTechnology vol 11 no 10 pp 1828ndash1839 2018

[33] D C Montgomery Design and Analysis of Experiments JohnWiley amp Sons 8th edition 2012

[34] M do S M Rufino R Alves E de Brito et al MetodologiaCientıfica Determinacao da Atividade Antioxidante Total emFrutas pela Captura do Radical Livre ABTS ComunicadoTecnico (Embrapa Agroindustria Tropical Online) 2007

[35] N Nenadis L-F Wang M Tsimidou and H-Y Zhang ldquoEsti-mation of scavenging activity of phenolic compounds using theABTS∙+ assayrdquo Journal of Agricultural and Food Chemistry vol52 no 15 pp 4669ndash4674 2004

[36] C A Di Battista D ConstenlaM V Ramırez-Rigo and J PinaldquoThe use of Arabic gum maltodextrin and surfactants in themicroencapsulation of phytosterols by spray dryingrdquo PowderTechnology vol 286 pp 193ndash201 2015

[37] C A Schneider W S Rasband and K W Eliceiri ldquoNIH Imageto ImageJ 25 years of image analysisrdquo Nature Methods vol 9no 7 pp 671ndash675 2012

[38] S Shamaei S S Seiiedlou M Aghbashlo E Tsotsas and AKharaghani ldquoMicroencapsulation of walnut oil by spray dry-ing effects of wall material and drying conditions on physico-chemical properties of microcapsulesrdquo Innovative Food Scienceand Emerging Technologies vol 39 pp 101ndash112 2017

[39] L Medina-Torres R Santiago-Adame F Calderas et alldquoMicroencapsulation by spray drying of laurel infusions (Litseaglaucescens) with maltodextrinrdquo Industrial Crops and Productsvol 90 pp 1ndash8 2016

[40] S Beirao-da-Costa C Duarte A I Bourbon et al ldquoInulinpotential for encapsulation and controlled delivery of Oreganoessential oilrdquo Food Hydrocolloids vol 33 no 2 pp 199ndash2062013

[41] R Santiago-Adame L Medina-Torres J A Gallegos-Infante etal ldquoSpray drying-microencapsulation of cinnamon infusions(Cinnamomum zeylanicum) with maltodextrinrdquo LWT- FoodScience and Technology vol 64 no 2 pp 571ndash577 2015

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

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Page 8: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

8 International Journal of Food Science

reported that the wall material concentration has a positiveeffect on the encapsulation efficiency ie the increase ofsolids content in the feed increases bioactive retention [21 5556] This behaviour could be related to the reduction of thetime required to form a surface crust in the atomized dropletsin the initial drying process when the solids concentration inthe feed solution increases This rapidly formed crust is notpermeable to compounds thereby protecting the bioactivefrom oxidation [57 58]

However too high viscosity of the feed solutions delaysthe formation of discrete particles during spray dryingwhereas a low viscosity in feed delays the formation of asemipermeable surface crust favouring further losses of thebioactive compounds [59] Therefore according to Reinec-cius [60] each wall material has its ideal feed concentrationto obtain higher encapsulation efficiency which is basedon the solubility and viscosity of the feed solution In thiswork an ideal arabic gum concentration of 74 was foundfor higher values of encapsulation efficiency and loadingcapacity Fernandes Marques [57] who evaluated the effectof total solids concentration on the microencapsulation ofrosemary essential oil by spray drying using maltodextrinand modified starch (11) as wall materials found higherencapsulation efficiency when a concentration of the wallmaterial of 22 was used which was reported as the idealconcentration for maltodextrin as wall material

322 Drying Yield Drying yield of the spray drying processis directly related to the cost of production and efficiencythus it is an important indicator that the industry considersin its production line [49 61] According to Nunes andMercadante [62] and Rutz Borges [63] drying yield isinfluenced by both the equipment settings (feed rate feedinlet and outlet temperature and flow rate) and dryingconditions (type and wall material concentration)

In this study a second-order model was fitted to theexperimental data of the drying yield with acceptable coef-ficient of determination and Table 2 shows that both inde-pendent variables arabic gum concentration and the dryinginlet temperature had a significant negative quadratic effecton the drying yield According to Table 1 the drying yields of120573-carotene with arabic gum ranged between 159 and 439Other researchers have found values of drying yield around50 Roccia Martınez [64] who studied the microencapsu-lation of the sunflower oil by spray drying using maltodextrinas a carrier agent found drying yield values that ranged from544 to 3988 and Santana Kurozawa [31] produced arabicgum microparticles with pulp pequi extract by spray dryingand obtained a drying yield values between 258 and 561

Low drying yield in the spray drying process is mostlydue to retention of the powder in the drying chamber wallcyclone inefficient in collecting fine particles and the highviscosity of the feed solution This powder retention problemcauses considerable economic loss and it is not cost-effectivefor industry as there would be frequent interruptions tothe dryer cleaning besides affecting the quality of the finalproduct However drying yield in the microencapsulationtechnique could be improved by modifying the spray dryingconditions in order to decrease the adhesion of particles to

the drying chamber wall [64ndash66] According to Tontul andTopuz [49] and Jayasundera Adhikari [67] the mechanicalscraping of the drying chamber wall introduction of coldair from the bottom and the use of low temperature lowhumidity air are some examples of process-based approachesthat could increase drying yield

As shown in Figure 5 as the drying temperature andthe arabic gum concentration increased the drying yieldalso increased until a maximum value was achieved Afterthis value decreases in the drying yield were observed evenwith the increase of both independent variables The highestdrying yield value was found for the sample with 20 GAdried at 155∘C

Chong and Wong [68] also found an optimum dosageof the wall material concentration (30 maltodextrin) andtemperature value (180∘C) that maximized the drying yield(57) when producing sapodilla puree particles by spraydrying using different maltodextrin concentrations (10-50wv) The authors referred that increasing the wall materialconcentration above the optimum value leads to an increaseviscosity of the feed solution thereby negatively affecting thedrying yield

323 Antioxidant Activity The AA values of encapsulated120573-carotene range from 005 to 078 120583mol troloxmgminus1120573-carotene whereas the commercial 120573-carotene before encap-sulation possessed 235 120583mol troloxmgminus1120573-carotene Thelower antioxidant activity after the encapsulation may berelated not only to the encapsulation process itself but alsoto the incomplete extraction of the encapsulated moleculesbefore antioxidant activity measurement This decrease inantioxidant activity after the spray drying process was alsoobserved for example by Franceschinis Salvatori [69] in themicroencapsulation of blackberry juices with maltodextrinand Hee Tan [70] in virgin coconut oil microparticles in amixture of maltodextrin arabic gum sodium caseinate andwhey protein concentrate

The data obtained for the antioxidant activity did notfit the second-order polynomial model though from theresults of Table 1 the two independent variables studiedarabic gum concentration and drying inlet temperatureaffected antioxidant activity of the encapsulated moleculessince an AA increase was observed when the temperaturedecreased (runs 4-3 2-1 and 11-10) and when the arabic gumconcentration increased (runs 1-3 2-4 8-9)

Other researchers have also studied the influence ofdrying inlet temperature and wall material on AA of theparticles Kha Nguyen [71] studied the effects of varyingmaltodextrin concentrations and spray drying temperatureson the antioxidant activity of Gac fruit powder and theyreported that increasing the drying inlet temperature from120 to 200∘C showed a significant loss of AA Additionallywith increasing maltodextrin concentration from 20 to 30the loss of AA was also observed The authors explainedthat AA loss could be due to loss of antioxidant compoundspresent in Gac powder spray dried at high temperaturesMiravet Alacid [72] who evaluated the antioxidant activityof pomegranate juice powder produced by spray dryingusing prebiotic fibers and maltodextrin as wall material also

International Journal of Food Science 9

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

10

08

06

04

02

00

minus02

Desirability

Figure 6 Desirability surface for optimal conditions

observed that the increase of the drying inlet temperaturefrom 160 to 200∘C had a significant negative effect on theantioxidant activity for both wall materials studied

324 Optimization of Drying Process Conditions The desir-ability function was performed for the simultaneous opti-mization of the responses that fitted to the second-ordermodel (Table 2) and the desirability surface for optimalconditions is depicted in Figure 6 Desirability values higherthan 07 were considered indicating a good optimization ofthe experimental data of each response variable [73] Thebest conditions for the spray drying microencapsulation of 120573-carotene with arabic gum as wall material were determined inorder to obtain higher values for drying yield encapsulationefficiency and loading capacity

The inlet drying temperature of 173∘C and arabic gumconcentration of 119 are recommended as the ideal con-ditions for microencapsulation of 120573-carotene Under theseconditions the predicted EE DY and LC are 1562 3630and 2274 mg 120573-carotenegminus1particles respectively

4 Conclusions

Themicroencapsulation of120573-carotene in arabic gumby spraydrying was investigated The arabic gum concentration anddrying inlet temperature influenced the drying yield encap-sulation efficiency and load capacity responses Regardingthe AA the antioxidant activity of 120573-carotene was reducedwhen microencapsulated at high temperatures (200∘C) inrelation to low temperatures (110∘C)

SEM analysis showed that the microparticles are micro-capsules Most of them presented a similar morphology amixture of smooth and wrinkled particles with a diameterlower than 10 120583m Increases in drying temperature favouredthe formation of smoother and larger particles

From the experimental conditions the drying inlet tem-perature of 173∘C and the arabic gum concentration of 119

were those that allow obtaining higher 120573-carotene contenthigher encapsulation efficiency and higher drying yield

The systematic approach used for the study of 120573-carotenemicroencapsulation process by spray drying may be easilyapplied for other core and wall materials Further studies willfocus on release studies in several aqueous media and even-tually on the encapsulation of natural carotenoid extracts

Data Availability

The data used to support the findings of this study areincluded within the article

Conflicts of Interest

The authors declare that they have no conflicts of interest

Acknowledgments

This work was supported by Conselho Nacional de Desen-volvimento Cientıfico e TecnologicondashCNPq through theCiencia sem Fronteiras program (CSF) (Grant CSF 2062682014-9 to first author)The authors acknowledge the financialsupport from Fundacao para a Ciencia e a TecnologiaPortugal Project UIDAGR041292013

References

[1] M E Rodrıguez-Huezo R Pedroza-Islas L A Prado-Bar-ragan C I Beristain and E J Vernon-Carter ldquoMicroencapsu-lation by spray drying of multiple emulsions containing caro-tenoidsrdquo Journal of Food Science vol 69 no 7 pp 351ndash359 2004

[2] A V Rao and L G Rao ldquoCarotenoids and human healthrdquoPharmacological Research vol 55 no 3 pp 207ndash216 2007

[3] J Fiedor and K Burda ldquoPotential role of carotenoids as anti-oxidants in human health and diseaserdquo Nutrients vol 6 no 2pp 466ndash488 2014

[4] R Arimboor R B Natarajan K R Menon L P Chan-drasekhar and VMoorkoth ldquoRed pepper (Capsicum annuum)carotenoids as a source of natural food colors analysis andstabilitymdasha reviewrdquo Journal of Food Science and Technology vol52 no 3 pp 1258ndash1271 2015

[5] M H Walter and D Strack ldquoCarotenoids and their cleavageproducts Biosynthesis and functionsrdquoNatural Product Reportsvol 28 no 4 pp 663ndash692 2011

[6] A Kaczor M Baranska and K Czamara Carotenoids WileyOnline Library 2016

[7] A F Aissa M L P Bianchi J C Ribeiro et al ldquoComparativestudy of 120573-carotene and microencapsulated 120573-carotene Eval-uation of their genotoxic and antigenotoxic effectsrdquo Food andChemical Toxicology vol 50 no 5 pp 1418ndash1424 2012

[8] Z Al Tanoury A Piskunov and C Rochette-Egly ldquoVitamina and retinoid signaling Genomic and nongenomic effectsrdquoJournal of Lipid Research vol 54 no 7 pp 1761ndash1775 2013

[9] E G Donhowe F P Flores W L Kerr L Wicker and F KongldquoCharacterization and invitro bioavailability of 120573-caroteneEffects of microencapsulation method and food matrixrdquo LWT-Food Science and Technology vol 57 no 1 pp 42ndash48 2014

[10] K Gul A Tak A Singh et al ldquoChemistry encapsulation andhealth benefits of szlig-carotene-A reviewrdquo Cogent Food amp Agri-culture vol 1 no 1 Article ID 1018696 2015

10 International Journal of Food Science

[11] HW Kim J B Kim S Poovan et al ldquoEffect of processing con-ditions on the content of cistrans carotene isomers as provita-min A carotenoids in Korean sweet potato varietiesrdquo Interna-tional Journal of Food Sciences and Nutrition vol 65 no 7 pp821ndash826 2014

[12] C Qian E A Decker H Xiao and D J McClements ldquoNano-emulsion delivery systems Influence of carrier oil on 120573-caro-tene bioaccessibilityrdquo Food Chemistry vol 135 no 3 pp 1440ndash1447 2012

[13] J C Spada L D F Marczak I C Tessaro and C P Z NorenaldquoMicroencapsulation of 120573-carotene using native pinhao starchmodified pinhao starch and gelatin by freeze-dryingrdquo Interna-tional Journal of Food Science amp Technology vol 47 no 1 pp186ndash194 2012

[14] G Zakynthinos and T Varzakas ldquoCarotenoids From plants tofood industryrdquo Current Research in Nutrition and Food Sciencevol 4 no 1 pp 38ndash51 2016

[15] R Liang Q Huang J Ma C F Shoemaker and F ZhongldquoEffect of relative humidity on the store stability of spray-driedbeta-carotene nanoemulsionsrdquo Food Hydrocolloids vol 33 no2 pp 225ndash233 2013

[16] C Saenz S Tapia J Chavez and P Robert ldquoMicroencapsula-tion by spray drying of bioactive compounds from cactus pear(Opuntia ficus-indica)rdquo Food Chemistry vol 114 no 2 pp 616ndash622 2009

[17] S AkhavanMahdavi SM Jafari E Assadpoor andDDehnadldquoMicroencapsulation optimization of natural anthocyaninswith maltodextrin gum Arabic and gelatinrdquo InternationalJournal of Biological Macromolecules vol 85 pp 379ndash385 2016

[18] N V N Jyothi P M Prasanna S N Sakarkar K S PrabhaP S Ramaiah and G Y Srawan ldquoMicroencapsulation tech-niques factors influencing encapsulation efficiencyrdquo Journal ofMicroencapsulation vol 27 no 3 pp 187ndash197 2010

[19] S M Jafari E Assadpoor Y He and B Bhandari ldquoEncapsu-lation efficiency of food flavours and oils during spray dryingrdquoDrying Technology vol 26 no 7 pp 816ndash835 2008

[20] S C Samantha A S Bruna R M Adriana B Fabio A RSandro and R C Aline ldquoDrying by spray drying in the foodindustry Micro-encapsulation process parameters and maincarriers usedrdquo African Journal of Food Science vol 9 no 9 pp462ndash470 2015

[21] T C Kha M H Nguyen P D Roach and C E StathopoulosldquoMicroencapsulation of Gac oil Optimisation of spray dryingconditions using response surface methodologyrdquo Powder Tech-nology vol 264 pp 298ndash309 2014

[22] E Janiszewska-Turak ldquoCarotenoids microencapsulation byspray drying method and supercritical micronizationrdquo FoodResearch International vol 99 pp 891ndash901 2017

[23] A Goncalves B N Estevinho and F Rocha ldquoDesign andcharacterization of controlled-release vitamin A microparticlesprepared by a spray-drying processrdquo Powder Technology vol305 pp 411ndash417 2017

[24] MOrdonez and AHerrera ldquoMorphologic and stability cassavastarch matrices for encapsulating limonene by spray dryingrdquoPowder Technology vol 253 pp 89ndash97 2014

[25] S-M Jafari K Mahdavi-Khazaei and A Hemmati-KakhkildquoMicroencapsulation of saffron petal anthocyanins with cressseed gum compared with Arabic gum through freeze dryingrdquoCarbohydrate Polymers vol 140 pp 20ndash25 2016

[26] M P Rascon C I Beristain H S Garcıa and M A Sal-gado ldquoCarotenoid retention and storage stability of spray-dried encapsulated paprika oleoresin using gum Arabic and

Soy protein isolate as wall materialsrdquo LWT- Food Science andTechnology vol 44 no 2 pp 549ndash557 2011

[27] GA Rocha C S Favaro-Trindade andC R F Grosso ldquoMicro-encapsulation of lycopene by spray drying Characterizationstability and application of microcapsulesrdquo Food and Bioprod-ucts Processing vol 90 no 1 pp 37ndash42 2012

[28] Q Shen and S Y Quek ldquoMicroencapsulation of astaxanthinwith blends of milk protein and fiber by spray dryingrdquo Journalof Food Engineering vol 123 pp 165ndash171 2014

[29] A M Goula and K G Adamopoulos ldquoA new technique forspray-dried encapsulation of lycopenerdquoDrying Technology vol30 no 6 pp 641ndash652 2012

[30] J Loksuwan ldquoCharacteristics of microencapsulated 120573-caroteneformed by spray drying with modified tapioca starch nativetapioca starch andmaltodextrinrdquoFoodHydrocolloids vol 21 no5-6 pp 928ndash935 2007

[31] A A Santana L E Kurozawa R A de Oliveira and K JPark ldquoInfluence of Process Conditions on the PhysicochemicalProperties of Pequi Powder Produced by Spray Dryingrdquo DryingTechnology vol 31 no 7 pp 825ndash836 2013

[32] D Troya D S Tupuna-Yerovi and J Ruales ldquoEffects of WallMaterials and Operating Parameters on Physicochemical Pro-perties Process Efficiency and Total Carotenoid Content ofMicroencapsulated Banana Passionfruit Pulp (Passiflora tri-partita var mollissima) by Spray-Dryingrdquo Food and BioprocessTechnology vol 11 no 10 pp 1828ndash1839 2018

[33] D C Montgomery Design and Analysis of Experiments JohnWiley amp Sons 8th edition 2012

[34] M do S M Rufino R Alves E de Brito et al MetodologiaCientıfica Determinacao da Atividade Antioxidante Total emFrutas pela Captura do Radical Livre ABTS ComunicadoTecnico (Embrapa Agroindustria Tropical Online) 2007

[35] N Nenadis L-F Wang M Tsimidou and H-Y Zhang ldquoEsti-mation of scavenging activity of phenolic compounds using theABTS∙+ assayrdquo Journal of Agricultural and Food Chemistry vol52 no 15 pp 4669ndash4674 2004

[36] C A Di Battista D ConstenlaM V Ramırez-Rigo and J PinaldquoThe use of Arabic gum maltodextrin and surfactants in themicroencapsulation of phytosterols by spray dryingrdquo PowderTechnology vol 286 pp 193ndash201 2015

[37] C A Schneider W S Rasband and K W Eliceiri ldquoNIH Imageto ImageJ 25 years of image analysisrdquo Nature Methods vol 9no 7 pp 671ndash675 2012

[38] S Shamaei S S Seiiedlou M Aghbashlo E Tsotsas and AKharaghani ldquoMicroencapsulation of walnut oil by spray dry-ing effects of wall material and drying conditions on physico-chemical properties of microcapsulesrdquo Innovative Food Scienceand Emerging Technologies vol 39 pp 101ndash112 2017

[39] L Medina-Torres R Santiago-Adame F Calderas et alldquoMicroencapsulation by spray drying of laurel infusions (Litseaglaucescens) with maltodextrinrdquo Industrial Crops and Productsvol 90 pp 1ndash8 2016

[40] S Beirao-da-Costa C Duarte A I Bourbon et al ldquoInulinpotential for encapsulation and controlled delivery of Oreganoessential oilrdquo Food Hydrocolloids vol 33 no 2 pp 199ndash2062013

[41] R Santiago-Adame L Medina-Torres J A Gallegos-Infante etal ldquoSpray drying-microencapsulation of cinnamon infusions(Cinnamomum zeylanicum) with maltodextrinrdquo LWT- FoodScience and Technology vol 64 no 2 pp 571ndash577 2015

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

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Submit your manuscripts atwwwhindawicom

Page 9: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

International Journal of Food Science 9

200

180

160

140

1205

1015

2025

3035

Temperature ( ∘C) Arabic gum ()

10

08

06

04

02

00

minus02

Desirability

Figure 6 Desirability surface for optimal conditions

observed that the increase of the drying inlet temperaturefrom 160 to 200∘C had a significant negative effect on theantioxidant activity for both wall materials studied

324 Optimization of Drying Process Conditions The desir-ability function was performed for the simultaneous opti-mization of the responses that fitted to the second-ordermodel (Table 2) and the desirability surface for optimalconditions is depicted in Figure 6 Desirability values higherthan 07 were considered indicating a good optimization ofthe experimental data of each response variable [73] Thebest conditions for the spray drying microencapsulation of 120573-carotene with arabic gum as wall material were determined inorder to obtain higher values for drying yield encapsulationefficiency and loading capacity

The inlet drying temperature of 173∘C and arabic gumconcentration of 119 are recommended as the ideal con-ditions for microencapsulation of 120573-carotene Under theseconditions the predicted EE DY and LC are 1562 3630and 2274 mg 120573-carotenegminus1particles respectively

4 Conclusions

Themicroencapsulation of120573-carotene in arabic gumby spraydrying was investigated The arabic gum concentration anddrying inlet temperature influenced the drying yield encap-sulation efficiency and load capacity responses Regardingthe AA the antioxidant activity of 120573-carotene was reducedwhen microencapsulated at high temperatures (200∘C) inrelation to low temperatures (110∘C)

SEM analysis showed that the microparticles are micro-capsules Most of them presented a similar morphology amixture of smooth and wrinkled particles with a diameterlower than 10 120583m Increases in drying temperature favouredthe formation of smoother and larger particles

From the experimental conditions the drying inlet tem-perature of 173∘C and the arabic gum concentration of 119

were those that allow obtaining higher 120573-carotene contenthigher encapsulation efficiency and higher drying yield

The systematic approach used for the study of 120573-carotenemicroencapsulation process by spray drying may be easilyapplied for other core and wall materials Further studies willfocus on release studies in several aqueous media and even-tually on the encapsulation of natural carotenoid extracts

Data Availability

The data used to support the findings of this study areincluded within the article

Conflicts of Interest

The authors declare that they have no conflicts of interest

Acknowledgments

This work was supported by Conselho Nacional de Desen-volvimento Cientıfico e TecnologicondashCNPq through theCiencia sem Fronteiras program (CSF) (Grant CSF 2062682014-9 to first author)The authors acknowledge the financialsupport from Fundacao para a Ciencia e a TecnologiaPortugal Project UIDAGR041292013

References

[1] M E Rodrıguez-Huezo R Pedroza-Islas L A Prado-Bar-ragan C I Beristain and E J Vernon-Carter ldquoMicroencapsu-lation by spray drying of multiple emulsions containing caro-tenoidsrdquo Journal of Food Science vol 69 no 7 pp 351ndash359 2004

[2] A V Rao and L G Rao ldquoCarotenoids and human healthrdquoPharmacological Research vol 55 no 3 pp 207ndash216 2007

[3] J Fiedor and K Burda ldquoPotential role of carotenoids as anti-oxidants in human health and diseaserdquo Nutrients vol 6 no 2pp 466ndash488 2014

[4] R Arimboor R B Natarajan K R Menon L P Chan-drasekhar and VMoorkoth ldquoRed pepper (Capsicum annuum)carotenoids as a source of natural food colors analysis andstabilitymdasha reviewrdquo Journal of Food Science and Technology vol52 no 3 pp 1258ndash1271 2015

[5] M H Walter and D Strack ldquoCarotenoids and their cleavageproducts Biosynthesis and functionsrdquoNatural Product Reportsvol 28 no 4 pp 663ndash692 2011

[6] A Kaczor M Baranska and K Czamara Carotenoids WileyOnline Library 2016

[7] A F Aissa M L P Bianchi J C Ribeiro et al ldquoComparativestudy of 120573-carotene and microencapsulated 120573-carotene Eval-uation of their genotoxic and antigenotoxic effectsrdquo Food andChemical Toxicology vol 50 no 5 pp 1418ndash1424 2012

[8] Z Al Tanoury A Piskunov and C Rochette-Egly ldquoVitamina and retinoid signaling Genomic and nongenomic effectsrdquoJournal of Lipid Research vol 54 no 7 pp 1761ndash1775 2013

[9] E G Donhowe F P Flores W L Kerr L Wicker and F KongldquoCharacterization and invitro bioavailability of 120573-caroteneEffects of microencapsulation method and food matrixrdquo LWT-Food Science and Technology vol 57 no 1 pp 42ndash48 2014

[10] K Gul A Tak A Singh et al ldquoChemistry encapsulation andhealth benefits of szlig-carotene-A reviewrdquo Cogent Food amp Agri-culture vol 1 no 1 Article ID 1018696 2015

10 International Journal of Food Science

[11] HW Kim J B Kim S Poovan et al ldquoEffect of processing con-ditions on the content of cistrans carotene isomers as provita-min A carotenoids in Korean sweet potato varietiesrdquo Interna-tional Journal of Food Sciences and Nutrition vol 65 no 7 pp821ndash826 2014

[12] C Qian E A Decker H Xiao and D J McClements ldquoNano-emulsion delivery systems Influence of carrier oil on 120573-caro-tene bioaccessibilityrdquo Food Chemistry vol 135 no 3 pp 1440ndash1447 2012

[13] J C Spada L D F Marczak I C Tessaro and C P Z NorenaldquoMicroencapsulation of 120573-carotene using native pinhao starchmodified pinhao starch and gelatin by freeze-dryingrdquo Interna-tional Journal of Food Science amp Technology vol 47 no 1 pp186ndash194 2012

[14] G Zakynthinos and T Varzakas ldquoCarotenoids From plants tofood industryrdquo Current Research in Nutrition and Food Sciencevol 4 no 1 pp 38ndash51 2016

[15] R Liang Q Huang J Ma C F Shoemaker and F ZhongldquoEffect of relative humidity on the store stability of spray-driedbeta-carotene nanoemulsionsrdquo Food Hydrocolloids vol 33 no2 pp 225ndash233 2013

[16] C Saenz S Tapia J Chavez and P Robert ldquoMicroencapsula-tion by spray drying of bioactive compounds from cactus pear(Opuntia ficus-indica)rdquo Food Chemistry vol 114 no 2 pp 616ndash622 2009

[17] S AkhavanMahdavi SM Jafari E Assadpoor andDDehnadldquoMicroencapsulation optimization of natural anthocyaninswith maltodextrin gum Arabic and gelatinrdquo InternationalJournal of Biological Macromolecules vol 85 pp 379ndash385 2016

[18] N V N Jyothi P M Prasanna S N Sakarkar K S PrabhaP S Ramaiah and G Y Srawan ldquoMicroencapsulation tech-niques factors influencing encapsulation efficiencyrdquo Journal ofMicroencapsulation vol 27 no 3 pp 187ndash197 2010

[19] S M Jafari E Assadpoor Y He and B Bhandari ldquoEncapsu-lation efficiency of food flavours and oils during spray dryingrdquoDrying Technology vol 26 no 7 pp 816ndash835 2008

[20] S C Samantha A S Bruna R M Adriana B Fabio A RSandro and R C Aline ldquoDrying by spray drying in the foodindustry Micro-encapsulation process parameters and maincarriers usedrdquo African Journal of Food Science vol 9 no 9 pp462ndash470 2015

[21] T C Kha M H Nguyen P D Roach and C E StathopoulosldquoMicroencapsulation of Gac oil Optimisation of spray dryingconditions using response surface methodologyrdquo Powder Tech-nology vol 264 pp 298ndash309 2014

[22] E Janiszewska-Turak ldquoCarotenoids microencapsulation byspray drying method and supercritical micronizationrdquo FoodResearch International vol 99 pp 891ndash901 2017

[23] A Goncalves B N Estevinho and F Rocha ldquoDesign andcharacterization of controlled-release vitamin A microparticlesprepared by a spray-drying processrdquo Powder Technology vol305 pp 411ndash417 2017

[24] MOrdonez and AHerrera ldquoMorphologic and stability cassavastarch matrices for encapsulating limonene by spray dryingrdquoPowder Technology vol 253 pp 89ndash97 2014

[25] S-M Jafari K Mahdavi-Khazaei and A Hemmati-KakhkildquoMicroencapsulation of saffron petal anthocyanins with cressseed gum compared with Arabic gum through freeze dryingrdquoCarbohydrate Polymers vol 140 pp 20ndash25 2016

[26] M P Rascon C I Beristain H S Garcıa and M A Sal-gado ldquoCarotenoid retention and storage stability of spray-dried encapsulated paprika oleoresin using gum Arabic and

Soy protein isolate as wall materialsrdquo LWT- Food Science andTechnology vol 44 no 2 pp 549ndash557 2011

[27] GA Rocha C S Favaro-Trindade andC R F Grosso ldquoMicro-encapsulation of lycopene by spray drying Characterizationstability and application of microcapsulesrdquo Food and Bioprod-ucts Processing vol 90 no 1 pp 37ndash42 2012

[28] Q Shen and S Y Quek ldquoMicroencapsulation of astaxanthinwith blends of milk protein and fiber by spray dryingrdquo Journalof Food Engineering vol 123 pp 165ndash171 2014

[29] A M Goula and K G Adamopoulos ldquoA new technique forspray-dried encapsulation of lycopenerdquoDrying Technology vol30 no 6 pp 641ndash652 2012

[30] J Loksuwan ldquoCharacteristics of microencapsulated 120573-caroteneformed by spray drying with modified tapioca starch nativetapioca starch andmaltodextrinrdquoFoodHydrocolloids vol 21 no5-6 pp 928ndash935 2007

[31] A A Santana L E Kurozawa R A de Oliveira and K JPark ldquoInfluence of Process Conditions on the PhysicochemicalProperties of Pequi Powder Produced by Spray Dryingrdquo DryingTechnology vol 31 no 7 pp 825ndash836 2013

[32] D Troya D S Tupuna-Yerovi and J Ruales ldquoEffects of WallMaterials and Operating Parameters on Physicochemical Pro-perties Process Efficiency and Total Carotenoid Content ofMicroencapsulated Banana Passionfruit Pulp (Passiflora tri-partita var mollissima) by Spray-Dryingrdquo Food and BioprocessTechnology vol 11 no 10 pp 1828ndash1839 2018

[33] D C Montgomery Design and Analysis of Experiments JohnWiley amp Sons 8th edition 2012

[34] M do S M Rufino R Alves E de Brito et al MetodologiaCientıfica Determinacao da Atividade Antioxidante Total emFrutas pela Captura do Radical Livre ABTS ComunicadoTecnico (Embrapa Agroindustria Tropical Online) 2007

[35] N Nenadis L-F Wang M Tsimidou and H-Y Zhang ldquoEsti-mation of scavenging activity of phenolic compounds using theABTS∙+ assayrdquo Journal of Agricultural and Food Chemistry vol52 no 15 pp 4669ndash4674 2004

[36] C A Di Battista D ConstenlaM V Ramırez-Rigo and J PinaldquoThe use of Arabic gum maltodextrin and surfactants in themicroencapsulation of phytosterols by spray dryingrdquo PowderTechnology vol 286 pp 193ndash201 2015

[37] C A Schneider W S Rasband and K W Eliceiri ldquoNIH Imageto ImageJ 25 years of image analysisrdquo Nature Methods vol 9no 7 pp 671ndash675 2012

[38] S Shamaei S S Seiiedlou M Aghbashlo E Tsotsas and AKharaghani ldquoMicroencapsulation of walnut oil by spray dry-ing effects of wall material and drying conditions on physico-chemical properties of microcapsulesrdquo Innovative Food Scienceand Emerging Technologies vol 39 pp 101ndash112 2017

[39] L Medina-Torres R Santiago-Adame F Calderas et alldquoMicroencapsulation by spray drying of laurel infusions (Litseaglaucescens) with maltodextrinrdquo Industrial Crops and Productsvol 90 pp 1ndash8 2016

[40] S Beirao-da-Costa C Duarte A I Bourbon et al ldquoInulinpotential for encapsulation and controlled delivery of Oreganoessential oilrdquo Food Hydrocolloids vol 33 no 2 pp 199ndash2062013

[41] R Santiago-Adame L Medina-Torres J A Gallegos-Infante etal ldquoSpray drying-microencapsulation of cinnamon infusions(Cinnamomum zeylanicum) with maltodextrinrdquo LWT- FoodScience and Technology vol 64 no 2 pp 571ndash577 2015

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

Hindawiwwwhindawicom

International Journal of

Volume 2018

Zoology

Hindawiwwwhindawicom Volume 2018

Anatomy Research International

PeptidesInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Journal of Parasitology Research

GenomicsInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawi Publishing Corporation httpwwwhindawicom Volume 2013Hindawiwwwhindawicom

The Scientific World Journal

Volume 2018

Hindawiwwwhindawicom Volume 2018

BioinformaticsAdvances in

Marine BiologyJournal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Neuroscience Journal

Hindawiwwwhindawicom Volume 2018

BioMed Research International

Cell BiologyInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Biochemistry Research International

ArchaeaHindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Genetics Research International

Hindawiwwwhindawicom Volume 2018

Advances in

Virolog y Stem Cells International

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Enzyme Research

Hindawiwwwhindawicom Volume 2018

International Journal of

MicrobiologyHindawiwwwhindawicom

Nucleic AcidsJournal of

Volume 2018

Submit your manuscripts atwwwhindawicom

Page 10: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

10 International Journal of Food Science

[11] HW Kim J B Kim S Poovan et al ldquoEffect of processing con-ditions on the content of cistrans carotene isomers as provita-min A carotenoids in Korean sweet potato varietiesrdquo Interna-tional Journal of Food Sciences and Nutrition vol 65 no 7 pp821ndash826 2014

[12] C Qian E A Decker H Xiao and D J McClements ldquoNano-emulsion delivery systems Influence of carrier oil on 120573-caro-tene bioaccessibilityrdquo Food Chemistry vol 135 no 3 pp 1440ndash1447 2012

[13] J C Spada L D F Marczak I C Tessaro and C P Z NorenaldquoMicroencapsulation of 120573-carotene using native pinhao starchmodified pinhao starch and gelatin by freeze-dryingrdquo Interna-tional Journal of Food Science amp Technology vol 47 no 1 pp186ndash194 2012

[14] G Zakynthinos and T Varzakas ldquoCarotenoids From plants tofood industryrdquo Current Research in Nutrition and Food Sciencevol 4 no 1 pp 38ndash51 2016

[15] R Liang Q Huang J Ma C F Shoemaker and F ZhongldquoEffect of relative humidity on the store stability of spray-driedbeta-carotene nanoemulsionsrdquo Food Hydrocolloids vol 33 no2 pp 225ndash233 2013

[16] C Saenz S Tapia J Chavez and P Robert ldquoMicroencapsula-tion by spray drying of bioactive compounds from cactus pear(Opuntia ficus-indica)rdquo Food Chemistry vol 114 no 2 pp 616ndash622 2009

[17] S AkhavanMahdavi SM Jafari E Assadpoor andDDehnadldquoMicroencapsulation optimization of natural anthocyaninswith maltodextrin gum Arabic and gelatinrdquo InternationalJournal of Biological Macromolecules vol 85 pp 379ndash385 2016

[18] N V N Jyothi P M Prasanna S N Sakarkar K S PrabhaP S Ramaiah and G Y Srawan ldquoMicroencapsulation tech-niques factors influencing encapsulation efficiencyrdquo Journal ofMicroencapsulation vol 27 no 3 pp 187ndash197 2010

[19] S M Jafari E Assadpoor Y He and B Bhandari ldquoEncapsu-lation efficiency of food flavours and oils during spray dryingrdquoDrying Technology vol 26 no 7 pp 816ndash835 2008

[20] S C Samantha A S Bruna R M Adriana B Fabio A RSandro and R C Aline ldquoDrying by spray drying in the foodindustry Micro-encapsulation process parameters and maincarriers usedrdquo African Journal of Food Science vol 9 no 9 pp462ndash470 2015

[21] T C Kha M H Nguyen P D Roach and C E StathopoulosldquoMicroencapsulation of Gac oil Optimisation of spray dryingconditions using response surface methodologyrdquo Powder Tech-nology vol 264 pp 298ndash309 2014

[22] E Janiszewska-Turak ldquoCarotenoids microencapsulation byspray drying method and supercritical micronizationrdquo FoodResearch International vol 99 pp 891ndash901 2017

[23] A Goncalves B N Estevinho and F Rocha ldquoDesign andcharacterization of controlled-release vitamin A microparticlesprepared by a spray-drying processrdquo Powder Technology vol305 pp 411ndash417 2017

[24] MOrdonez and AHerrera ldquoMorphologic and stability cassavastarch matrices for encapsulating limonene by spray dryingrdquoPowder Technology vol 253 pp 89ndash97 2014

[25] S-M Jafari K Mahdavi-Khazaei and A Hemmati-KakhkildquoMicroencapsulation of saffron petal anthocyanins with cressseed gum compared with Arabic gum through freeze dryingrdquoCarbohydrate Polymers vol 140 pp 20ndash25 2016

[26] M P Rascon C I Beristain H S Garcıa and M A Sal-gado ldquoCarotenoid retention and storage stability of spray-dried encapsulated paprika oleoresin using gum Arabic and

Soy protein isolate as wall materialsrdquo LWT- Food Science andTechnology vol 44 no 2 pp 549ndash557 2011

[27] GA Rocha C S Favaro-Trindade andC R F Grosso ldquoMicro-encapsulation of lycopene by spray drying Characterizationstability and application of microcapsulesrdquo Food and Bioprod-ucts Processing vol 90 no 1 pp 37ndash42 2012

[28] Q Shen and S Y Quek ldquoMicroencapsulation of astaxanthinwith blends of milk protein and fiber by spray dryingrdquo Journalof Food Engineering vol 123 pp 165ndash171 2014

[29] A M Goula and K G Adamopoulos ldquoA new technique forspray-dried encapsulation of lycopenerdquoDrying Technology vol30 no 6 pp 641ndash652 2012

[30] J Loksuwan ldquoCharacteristics of microencapsulated 120573-caroteneformed by spray drying with modified tapioca starch nativetapioca starch andmaltodextrinrdquoFoodHydrocolloids vol 21 no5-6 pp 928ndash935 2007

[31] A A Santana L E Kurozawa R A de Oliveira and K JPark ldquoInfluence of Process Conditions on the PhysicochemicalProperties of Pequi Powder Produced by Spray Dryingrdquo DryingTechnology vol 31 no 7 pp 825ndash836 2013

[32] D Troya D S Tupuna-Yerovi and J Ruales ldquoEffects of WallMaterials and Operating Parameters on Physicochemical Pro-perties Process Efficiency and Total Carotenoid Content ofMicroencapsulated Banana Passionfruit Pulp (Passiflora tri-partita var mollissima) by Spray-Dryingrdquo Food and BioprocessTechnology vol 11 no 10 pp 1828ndash1839 2018

[33] D C Montgomery Design and Analysis of Experiments JohnWiley amp Sons 8th edition 2012

[34] M do S M Rufino R Alves E de Brito et al MetodologiaCientıfica Determinacao da Atividade Antioxidante Total emFrutas pela Captura do Radical Livre ABTS ComunicadoTecnico (Embrapa Agroindustria Tropical Online) 2007

[35] N Nenadis L-F Wang M Tsimidou and H-Y Zhang ldquoEsti-mation of scavenging activity of phenolic compounds using theABTS∙+ assayrdquo Journal of Agricultural and Food Chemistry vol52 no 15 pp 4669ndash4674 2004

[36] C A Di Battista D ConstenlaM V Ramırez-Rigo and J PinaldquoThe use of Arabic gum maltodextrin and surfactants in themicroencapsulation of phytosterols by spray dryingrdquo PowderTechnology vol 286 pp 193ndash201 2015

[37] C A Schneider W S Rasband and K W Eliceiri ldquoNIH Imageto ImageJ 25 years of image analysisrdquo Nature Methods vol 9no 7 pp 671ndash675 2012

[38] S Shamaei S S Seiiedlou M Aghbashlo E Tsotsas and AKharaghani ldquoMicroencapsulation of walnut oil by spray dry-ing effects of wall material and drying conditions on physico-chemical properties of microcapsulesrdquo Innovative Food Scienceand Emerging Technologies vol 39 pp 101ndash112 2017

[39] L Medina-Torres R Santiago-Adame F Calderas et alldquoMicroencapsulation by spray drying of laurel infusions (Litseaglaucescens) with maltodextrinrdquo Industrial Crops and Productsvol 90 pp 1ndash8 2016

[40] S Beirao-da-Costa C Duarte A I Bourbon et al ldquoInulinpotential for encapsulation and controlled delivery of Oreganoessential oilrdquo Food Hydrocolloids vol 33 no 2 pp 199ndash2062013

[41] R Santiago-Adame L Medina-Torres J A Gallegos-Infante etal ldquoSpray drying-microencapsulation of cinnamon infusions(Cinnamomum zeylanicum) with maltodextrinrdquo LWT- FoodScience and Technology vol 64 no 2 pp 571ndash577 2015

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

Hindawiwwwhindawicom

International Journal of

Volume 2018

Zoology

Hindawiwwwhindawicom Volume 2018

Anatomy Research International

PeptidesInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Journal of Parasitology Research

GenomicsInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawi Publishing Corporation httpwwwhindawicom Volume 2013Hindawiwwwhindawicom

The Scientific World Journal

Volume 2018

Hindawiwwwhindawicom Volume 2018

BioinformaticsAdvances in

Marine BiologyJournal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Neuroscience Journal

Hindawiwwwhindawicom Volume 2018

BioMed Research International

Cell BiologyInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Biochemistry Research International

ArchaeaHindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Genetics Research International

Hindawiwwwhindawicom Volume 2018

Advances in

Virolog y Stem Cells International

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Enzyme Research

Hindawiwwwhindawicom Volume 2018

International Journal of

MicrobiologyHindawiwwwhindawicom

Nucleic AcidsJournal of

Volume 2018

Submit your manuscripts atwwwhindawicom

Page 11: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

International Journal of Food Science 11

[42] R V Tonon C Brabet and M D Hubinger ldquoInfluence ofprocess conditions on the physicochemical properties of acai(Euterpe oleraceae Mart) powder produced by spray dryingrdquoJournal of Food Engineering vol 88 no 3 pp 411ndash418 2008

[43] M V Prince K Thangavel V Meda R Visvanathan and DAnanthakrishnan ldquoEffect of carrier blend proportion andflavorload on physical characteristics of nutmeg (Myristica frangransHoutt) oleoresin microencapsulated by spray dryingrdquo Interna-tional Food Research Journal vol 21 no 5 pp 2039ndash2044 2014

[44] D A Botrel S V Borges R V D B Fernandes et al ldquoApplica-tion of cashew tree gum on the production and stability ofspray-dried fish oilrdquo Food Chemistry vol 221 pp 1522ndash15292017

[45] J Poomkokrak C Niamnuy K Choicharoen and S Deva-hastin ldquoEncapsulation of soybean extract using spray dryingrdquoJournal of Food Science and Agricultural Technology (JFAT) vol1 pp 105ndash110 2015

[46] F Yu Z Li T Zhang Y Wei Y Xue and C Xue ldquoInfluence ofencapsulation techniques on the structure physical propertiesand thermal stability of fish oil microcapsules by spray dryingrdquoJournal of Food Process Engineering vol 40 no 6 Article IDe12576 2017

[47] D R S F Paim S D O Costa E HMWalter and R V TononldquoMicroencapsulation of probiotic jussara (Euterpe edulis M)juice by spray dryingrdquo LWT- Food Science and Technology vol74 pp 21ndash25 2016

[48] C Onwulata ldquoParticle Size Analysis of Food Powdersrdquo inEncapsulated and Powdered Foods pp 217ndash248 CRC Press2005

[49] I Tontul and A Topuz ldquoSpray-drying of fruit and vegetablejuices Effect of drying conditions on the product yield andphysical propertiesrdquo Trends in Food Science amp Technology vol63 pp 91ndash102 2017

[50] C C Ferrari S P M Germer and J M de Aguirre ldquoEffects ofSpray-Drying Conditions on the Physicochemical Properties ofBlackberry Powderrdquo Drying Technology vol 30 no 2 pp 154ndash163 2012

[51] E C Frascareli V M Silva R V Tonon and M D HubingerldquoEffect of process conditions on the microencapsulation ofcoffee oil by spray dryingrdquo Food and Bioproducts Processing vol90 no 3 pp 413ndash424 2012

[52] M R Islam Shishir F S Taip N A Aziz R A Talib and M SHossain Sarker ldquoOptimization of spray drying parameters forpink guava powder usingRSMrdquo Food Science andBiotechnologyvol 25 no 2 pp 461ndash468 2016

[53] T Lundstedt E Seifert L Abramo et al ldquoExperimental designand optimizationrdquoChemometrics and Intelligent Laboratory Sys-tems vol 42 no 1-2 pp 3ndash40 1998

[54] D A Botrel S V Borges R V d B Fernandes et al ldquoEvaluationof spray drying conditions on properties of microencapsulatedoregano essential oilrdquo International Journal of Food Science ampTechnology vol 47 no 11 pp 2289ndash2296 2012

[55] N K Mohammed C P Tan Y A Manap A M Alhelli andA S M Hussin ldquoProcess conditions of spray drying micro-encapsulation of Nigella sativa oilrdquo Powder Technology vol 315pp 1ndash14 2017

[56] S Murali A Kar A S Patel J Kumar D Mohapatra and SK Dash ldquoEncapsulation of rice bran oil in tapioca starch-soyaprotein isolate complex using spray dryingrdquo Indian Journal ofAgricultural Sciences vol 86 no 8 pp 984ndash991 2016

[57] R V De Barros Fernandes G R Marques S V Borges and DA Botrel ldquoEffect of solids content and oil load on the microen-capsulation process of rosemary essential oilrdquo Industrial Cropsand Products vol 58 pp 173ndash181 2014

[58] R V Tonon R B Pedro C R F Grosso and M D HubingerldquoMicroencapsulation of Flaxseed Oil by Spray Drying Effect ofOil Load andType ofWallMaterialrdquoDrying Technology vol 30no 13 pp 1491ndash1501 2012

[59] T V Huynh N Caffin G Dykes and B Bhandari ldquoOpti-mization of the microencapsulation of lemon myrtle oil usingresponse surface methodologyrdquo Drying Technology vol 26 no3 pp 357ndash368 2008

[60] G A Reineccius ldquoThe spray drying of food flavorsrdquo DryingTechnology vol 22 no 6 pp 1289ndash1324 2004

[61] K Muzaffar and P Kumar ldquoParameter optimization for spraydrying of tamarind pulp using response surface methodologyrdquoPowder Technology vol 279 pp 179ndash184 2015

[62] I L Nunes and A Z Mercadante ldquoEncapsulation of lycopeneusing spray-drying and molecular inclusion processesrdquo Brazil-ian Archives of Biology and Technology vol 50 no 5 pp 893ndash900 2007

[63] J K Rutz C D Borges R C Zambiazi C G Da Rosa andM M Da Silva ldquoElaboration of microparticles of carotenoidsfrom natural and synthetic sources for applications in foodrdquoFood Chemistry vol 202 pp 324ndash333 2016

[64] P Roccia M L Martınez J M Llabot and P D RibottaldquoInfluence of spray-drying operating conditions on sunfloweroil powder qualitiesrdquo Powder Technology vol 254 pp 307ndash3132014

[65] AA Santana L C Paixao R AOliveira andV R Telis ldquoInflu-ence of process conditions on the physicochemical propertiesof jussara pulp (Euterpe edulis) powder produced by spraydryingrdquo Brazilian Journal of Food Technology vol 21 2018

[66] A Can Karaca O Guzel and M M Ak ldquoEffects of processingconditions and formulation on spray drying of sour cherry juiceconcentraterdquo Journal of the Science of Food and Agriculture vol96 no 2 pp 449ndash455 2016

[67] M Jayasundera B Adhikari R Adhikari and P Aldred ldquoTheeffect of protein types and low molecular weight surfactants onspray drying of sugar-rich foodsrdquo Food Hydrocolloids vol 25no 3 pp 459ndash469 2011

[68] S Y Chong and C W Wong ldquoProduction of Spray-DriedSapodilla (Manilkara zapota) Powder from Enzyme-AidedLiquefied Pureerdquo Journal of Food Processing and Preservationvol 39 no 6 pp 2604ndash2611 2015

[69] L Franceschinis D M Salvatori N Sosa and C ScheborldquoPhysical and Functional Properties of Blackberry Freeze- andSpray-Dried PowdersrdquoDryingTechnology vol 32 no 2 pp 197ndash207 2014

[70] Y Y Hee C P Tan R Abdul Rahman NMohdAdzahanW TLai and G H Chong ldquoInfluence of different wall materials onthe microencapsulation of virgin coconut oil by spray dryingrdquoInternational Journal of Food Engineering vol 11 no 1 pp 61ndash69 2015

[71] T C Kha M H Nguyen and P D Roach ldquoEffects of spraydrying conditions on the physicochemical and antioxidantproperties of the Gac (Momordica cochinchinensis) fruit arilpowderrdquo Journal of Food Engineering vol 98 no 3 pp 385ndash3922010

[72] G Miravet M Alacid J M Obon and J A Fernandez-LopezldquoSpray-drying of pomegranate juice with prebiotic dietary

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

Hindawiwwwhindawicom

International Journal of

Volume 2018

Zoology

Hindawiwwwhindawicom Volume 2018

Anatomy Research International

PeptidesInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Journal of Parasitology Research

GenomicsInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawi Publishing Corporation httpwwwhindawicom Volume 2013Hindawiwwwhindawicom

The Scientific World Journal

Volume 2018

Hindawiwwwhindawicom Volume 2018

BioinformaticsAdvances in

Marine BiologyJournal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Neuroscience Journal

Hindawiwwwhindawicom Volume 2018

BioMed Research International

Cell BiologyInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Biochemistry Research International

ArchaeaHindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Genetics Research International

Hindawiwwwhindawicom Volume 2018

Advances in

Virolog y Stem Cells International

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Enzyme Research

Hindawiwwwhindawicom Volume 2018

International Journal of

MicrobiologyHindawiwwwhindawicom

Nucleic AcidsJournal of

Volume 2018

Submit your manuscripts atwwwhindawicom

Page 12: Microencapsulation of -Carotene by Spray Drying: Effect of ...downloads.hindawi.com/journals/ijfs/2019/8914852.pdfMicroencapsulation of -Carotene by Spray Drying: Effect of Wall Material

12 International Journal of Food Science

fibrerdquo International Journal of Food Science amp Technology vol51 no 3 pp 633ndash640 2016

[73] S K Tumwesigye J CMontanez J COliveira andM J Sousa-Gallagher ldquoNovel Intact Bitter Cassava Sustainable Develop-ment and Desirability Optimisation of Packaging Filmsrdquo Foodand Bioprocess Technology vol 9 no 5 pp 801ndash812 2016

Hindawiwwwhindawicom

International Journal of

Volume 2018

Zoology

Hindawiwwwhindawicom Volume 2018

Anatomy Research International

PeptidesInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Journal of Parasitology Research

GenomicsInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawi Publishing Corporation httpwwwhindawicom Volume 2013Hindawiwwwhindawicom

The Scientific World Journal

Volume 2018

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The Scientific World Journal

Volume 2018

Hindawiwwwhindawicom Volume 2018

BioinformaticsAdvances in

Marine BiologyJournal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Neuroscience Journal

Hindawiwwwhindawicom Volume 2018

BioMed Research International

Cell BiologyInternational Journal of

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Biochemistry Research International

ArchaeaHindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Genetics Research International

Hindawiwwwhindawicom Volume 2018

Advances in

Virolog y Stem Cells International

Hindawiwwwhindawicom Volume 2018

Hindawiwwwhindawicom Volume 2018

Enzyme Research

Hindawiwwwhindawicom Volume 2018

International Journal of

MicrobiologyHindawiwwwhindawicom

Nucleic AcidsJournal of

Volume 2018

Submit your manuscripts atwwwhindawicom