198 FABAD J. Pharm. Sci., 31, 198-209, 2006 RESEARCH ARTICLE Decontamination of Cosmetic Products and Raw Materials by Gamma Irradiation Summary Decontamination of Cosmetic Products and Raw Materials by Gamma Irradiation In this study, we aimed to use gamma irradiation for decontamination of cosmetic products in order to achieve the acceptable microbiological limits. Cosmetic products and raw materials were irradiated (5-7.5-10 kGy) and physicochemical, microbiological and biological properties of these samples were evaluated in normal and stress storage conditions. It was found that the physicochemical properties of samples tested were changed after irradiation. No change was observed in skin irritation properties of all samples tested. Decontamination dose for all samples, excluding starch, was found to be about 5 kGy or below. Key Words: Decontamination by gamma radiation, cosmetic products, cosmetic raw materials. Received : 03.03.2008 Revised : 27.03.2008 Accepted : 29.05.2008 * Hacettepe University, Faculty of Pharmacy, Department of Radiopharmacy, 06100, Ankara,Turkey. ** Hacettepe University, Faculty of Pharmacy, Department of Pharmaceutical Microbiology, 06100, Ankara, Turkey. *** Hacettepe University, Faculty of Medicine, Department of Dermatology, 06100, Ankara, Turkey. **** Hacettepe University, Faculty of Engineering, Department of Physics Engineering, 06532, Ankara, Turkey. ° Corresponding author e-mail : [email protected]INTRODUCTION Gamma irradiation has an increasingly important role in the manufacture of cosmetic products [1]. The use of gamma rays is an alternative method for ster- ilization/decontamination of products and raw ma- terials [2]. However, one of the major problems of irradiation is the occurrence of new radicals during the process [3]. Irradiation is never a substitute for poor compliance to Good Manufacturing Practice (GMP) guidelines. In fact, it should be a part of GMP [4]. The gamma radiation process cannot make some- thing radioactive or leave any residual radioactivity. Microorganisms are killed either as a result of the destruction in a vital molecule or by chemical reaction of compounds resulting from radiation. The most widely used application of gamma radiation process- ing is in the control of microbial contamination levels [1]. Topically applied preparations must not contain mi- crobials exceeding the permissible limits. This is
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198
FABAD J. Pharm. Sci., 31, 198-209, 2006
RESEARCH ARTICLE
Decontamination of Cosmetic Products and Raw Materials by Gamma IrradiationSummary
Decontamination of Cosmetic Products andRaw Materials by Gamma Irradiation
In this study, we aimed to use gamma irradiation for decontamination of cosmetic products in order to achieve the acceptable microbiological limits. Cosmetic products and raw materials were irradiated (5-7.5-10 kGy) and physicochemical, microbiological and biological properties of these samples were evaluated in normal and stress storage conditions. It was found that the physicochemical properties of samples tested were changed after irradiation. No change was observed in skin irritation properties of all samples tested. Decontamination dose for all samples, excluding starch, was found to be about 5 kGy or below. Key Words: Decontamination by gamma radiation, cosmetic products, cosmetic raw materials.Received : 03.03.2008Revised : 27.03.2008Accepted : 29.05.2008
* Hacettepe University, Faculty of Pharmacy, Department of Radiopharmacy, 06100, Ankara,Turkey. ** Hacettepe University, Faculty of Pharmacy, Department of Pharmaceutical Microbiology, 06100, Ankara, Turkey.*** Hacettepe University, Faculty of Medicine, Department of Dermatology, 06100, Ankara, Turkey.**** Hacettepe University, Faculty of Engineering, Department of Physics Engineering, 06532, Ankara, Turkey.° Corresponding author e-mail : [email protected]
INTRODUCTION
Gamma irradiation has an increasingly important
role in the manufacture of cosmetic products [1]. The
use of gamma rays is an alternative method for ster-
ilization/decontamination of products and raw ma-
terials [2]. However, one of the major problems of
irradiation is the occurrence of new radicals during
the process [3]. Irradiation is never a substitute for
poor compliance to Good Manufacturing Practice
(GMP) guidelines. In fact, it should be a part of GMP
[4]. The gamma radiation process cannot make some-
thing radioactive or leave any residual radioactivity.
Microorganisms are killed either as a result of the
destruction in a vital molecule or by chemical reaction
of compounds resulting from radiation. The most
widely used application of gamma radiation process-
ing is in the control of microbial contamination levels
[1].
Topically applied preparations must not contain mi-
crobials exceeding the permissible limits. This is
199
achieved through the decontamination and steriliza-
tion process [5]. In many cases, the offending organ-
isms in a cosmetic product are Escherichia coli (E.
coli) or Pseudomonas aeruginosa (P. aeruginosa).
Both are especially susceptible to radiation energy at
very low doses, which often means that the radiation
effect on the product is negligible [6]. Cosmetic prod-
ucts may be contaminated during manufacturing by
microorganisms existing in the environment or in the
raw materials. Raw materials, especially water, found
in most of the cosmetic preparations form an appro-
priate media for microbial growth. There is no certain
radiation dose level in pharmacopoeia and guidelines
for decontaminating cosmetic preparations and cos-
metic raw materials. However, acceptable microbio-
logical limits are recommended in guidelines for a
variety of cosmetic preparations. These limits are
between 102 and 103. Generally, the gamma radiation
dose preferred to achieve these levels ranges between
5 and 15 kGy. 60Co source, which is commonly used
for gamma irradiation, can be used for cosmetic raw
materials and finished products. Aiming at the reduc-
tion in microbiological content, the method does not
leave any residues that may be harmful to the em-
ployees or consumers. Gamma radiation can penetrate
the packaging materials and sealed packages contain-
ing the finished products, thus destroying the existing
microorganisms. Decontamination by gamma radia-
tion is gaining increasing attention in cosmetic pro-
duction.
MATERIALS and METHODS
Materials used in the experiments are coded in Table
1. A, B, and C were kindly provided from Colgate-
Palmolive, D from Canan Kozmetik, E, F, G, H, I, J,
K, L from Eczac›bafl›-Beiersdorf, M from Evyap, N,
O, P from Eczac›bafl›-Avon, R from Johnson & Johnson,
S, V, Y from Merck, T from Roquette Freres, and U
from Çapamarka.
Statistics
Physicochemical test results are given as the mean of
6 experiments; whereas, n = 3 was applied for biolog-
ical and microbiological tests. Kruskal-Wallis and
non-parametric Mann-Whitney U tests were used as
the significance tests and SPSS computer software
program was employed for analyses.
Irradiation Process
Irradiation was performed at room temperature using
a 60Co Gamma Cell 220 available at the Turkish Atomic
Energy Agency (TAEK) at a dose rate of 2.84 kGy h-
1. All samples in glass vials were irradiated at doses
of 5, 7.5, 10 kGy. Bioburden and irritation tests were
carried out for sample K.
Unirradiated samples were used as controls to detect
physicochemical, biological and microbiological
changes resulting from the action of ionizing radiation
on the cosmetic products and raw materials investi-
gated. Experiments performed on cosmetic samples
are summarized in Table 2.
Physicochemical Properties
All tests were performed on unirradiated samples
and samples irradiated at doses of 5, 7.5 and 10 kGy
(Table 2). Results were analyzed statistically.
Table 1. Codes of materials used
Cosmetic Cosmetic Cosmetic Raw
Code Product Code Product Code Materials
A Baby powder J Concealer S Talc
B Solid soap K Mascara T Wheat starch
C Solid soap L Eye pencil U Corn starch
D Liquid soap M Solid soap V Bentonite
E Baby powder N Redness Y Gelatin
F Lush on O Lip pencil
G Compact powder P Foundation
H Foundation R Baby powder
I Eye shadow
Table 2. Tests performed on cosmetic samples under normal conditions
COSMETIC PRODUCTS
Physicochemical Tests
Biological Test
- Irritation test
Microbiological Tests
- Bioburden
- Determination of decontamination dose
Solid and liquid soaps
- Organoleptic properties
- pH
- Viscosity
- Foam height
Other preparations
- Organoleptic properties
- Particle size
COSMETIC RAW MATERIALS
Physicochemical Tests
Biological Test
- Irritation test
Microbiological Tests
- Bioburden
- Determination of
decontamination dose
- Organoleptic properties
- Particle size
- ESR behavior
200
FABAD J. Pharm. Sci., 31, 198-209, 2006
-Organoleptic Properties: Solid and liquid soaps were
evaluated by their color, odor and general appearance.
-pH: [5% (w/v)] solutions of unirradiated and irradi-
ated soaps were prepared and pH of these solutions
were measured at room temperature (25°C) and at
40°C (Sesa Model 1400).
- Viscosity: Viscosities of unirradiated and irradiated
1% (w/v) soap solutions were measured by Brookfield
rheometer (DV-II model) at two different temperatures
of 25°C and 40°C.
-Foam Height: To determine the foam height, 5 ml of
unirradiated and irradiated 1% (w/v) soap solutions
were placed in tubes and vigorously shaken for 10
min at 280 rpm.min-1. Foam height was calculated as
the ratio of foam height to total height. The same
procedure was repeated at 25°C and 40°C.
-Mean Particle Size and Distribution: Unirradiated
samples and samples irradiated at doses of 5, 7.5 and
10 kGy were investigated. Mean particle sizes and
size distributions of cosmetic samples except soaps,
i.e. foundations, concealer, mascara, eye pencil and
lip pencil, were measured by laser diffraction method
(Sympatec Helos (H 0728) Particle Size Analyzer).
-ESR Behavior: Electron spin resonance (ESR) studies
were done on cosmetic raw materials before and
immediately after irradiation. These studies were
carried out using a Varian 9”E-LX Band ESR Spec-
trometer. Each spectrum was corrected for variation
using the amount of material in the ESR tube.
Microbiological Properties
The neutralization process of antimicrobial property
was not validated because the aim of this research
was to determine the bioburden of cosmetic raw
materials and products and to compare these findings
with the limits permitted legally. The purpose was to
find the reliability of cosmetic products and raw
materials available on the Turkish market and in
accordance with the guidelines.
In order to obtain these results, 1 g of cosmetic product
or raw material was used in the experimental part
and all samples were contaminated with Bacillus
pumilus spores (106 cfu.mL-1) at the beginning of the
study.
-Bioburden: In order to determine the microbial load
(bioburden) of samples, 1 g of each sample was
weighed in sterile vials and 1 ml of sterile distilled
water was then added. Each mixture was mixed for
1 min; 0.1 ml of samples were withdrawn from vials
and inoculated on plates with tryptic soy agar. All
plates were incubated for 24-48 h at 37°C followed
by counting the number of colonies with naked eye.
cfu.mL-1), in order to determine the decontamination
dose level. The samples were then irradiated at dif-
ferent dose levels of 2, 5, 7.5 and 10 kGy. Each sample
was mixed for 1 min; 0.1 ml of samples were with-
drawn from vials and inoculated on plate with tryptic
soy agar. All plates were incubated for 24-48 h at 37°C,
followed by counting the number of colonies with
naked eye.
Biological Properties
-Irritation Test: Possible irritation effects of unirradi-
ated and irradiated samples were evaluated using
occlusive patch test. Patches were applied to the
forearms of healthy volunteers. Patches were removed
24 h later, and forearms were washed with tap water.
Irritation was evaluated by a dermatologist using the
scores given in Table 3. The test was repeated 3 times
Table 3. Scoring of irritation
Erythema0 No evidence of erythema0.5 Minimal or doubtful erythema1 Slight, spotty and diffuse redness2 Moderate, uniform redness3 Strong uniform redness4 Hot rednessDryness0 No evidence of scaling0.5 Dry without scaling; appears smooth and tight1 Fine/mild scaling2 Moderate scaling3 Severe scaling with large flakesEdema- Absence of edema+ Presence of edema
201
per sample. In total, 18 healthy volunteers were used
for 22 samples.
5% (w/v) soap solutions were used for this test. 15
mg of samples A, E, F, G, H, I, N and R were weighed
and placed in the Finn chambers. One drop of samples
H and P were absorbed on special filter papers, and
then placed in the chamber. For sample K, 2 ml of
distilled water was added to the original package
and mixed for 2 min; then, one drop of mixture was
put on special filter paper and then placed in the
chamber. A certain amount of samples J, L and O
were placed in chambers. At the end of the test, the
score table (Table 3) [7] was used for evaluating the
results.
Stability Studies
In this part of the study, tests performed for samples
under normal environmental conditions were repeated
with samples stored in unsealed glass tubes for cos-
metic raw materials and in sealed glass tubes for
cosmetic products, at high temperature (40±2)ºC and
high relative humidity (75±5)% conditions over a
period of 3 months. Possible changes wer e investigat-
ed at accelerated conditions after irradiation. Exper-
imental studies carried out for this purpose are sum-
marized in Table 4.
- ESR Behavior: Peaks obtained in the ESR studies in
normal environmental conditions were also evaluated
in the samples at the end of the stability studies to
determine any radical formation.
RESULTS and DISCUSSION
Studies Carried Out Under Normal Conditions
Physicochemical Properties
Physicochemical properties of soaps treated with
gamma radiation are widely described, but not for
other cosmetics. Therefore, physicochemical tests
were applied to cosmetic products considering the
existing guidelines or other official sources. For those
properties not officially mentioned, particle size mea-
surements, organoleptic properties and ESR studies