C190-E145A High-Performance Liquid Chromatograph Application Systems Prominence Application Systems
C190-E145A
High-Performance Liquid Chromatograph Application Systems
ProminenceApplication Systems
ProminenceHigh Performance Liquid Chromatograph
Shimadzu Corporation is a world leader in high-performance liquid chromatography
and Shimadzu HPLC systems are employed in a wide range of fields from medicine,
pharmaceuticals, and biochemistry to chemistry, the environment, and foods.
Shimadzu’s Prominence HPLC series handles all applications at an extremely high level
of performance.
Contents
Chemical Industry
Environment
Food components Additives Residual pesticides Fragrances
Plastics Solvents Paints Fiber and paper
Atmosphere Drinking water Soil Biofuels
Drug ingredients Antibiotics and antimicrobials
Herbal medicines, natural products Veterinary pharmaceuticals
Pharmaceuticals
FoodsFo
FFoo
CChPla
EEnA
DrDr
He
PPhh
P. 4
P. 6
P. 8
P. 10
P. 12
P. 14
Amino Acid Analysis System
Organic Acid Analysis System
Reducing Sugar Analysis System
Carbamate Analysis System
Iminoctadine Analysis System
Synthetic Antimicrobial Analysis System
P. 16
P. 18
P. 20
P. 22
P. 24
Bromate Analysis System
Cyanide Analysis System
Anionic Surfactant Analysis System
Aldehyde Analysis System
Other Application Systems
Prominence was developed to improve the efficiency of analytical work and enhance data reliability.
These HPLC systems offer outstanding functions and performance in comparison with conventional
instruments, including web-based control, high-speed sample injections, and highly sensitive detection.
Shimadzu’s application systems, based on the Prominence series, incorporate the company’s
instrument analysis experience cultivated jointly with customers.
4
+
Amino Acid Analysis System
Amino Acid Analysis by HPLC
System Characteristics
Mobile PhaseReaction ReagentDegassing UnitReservoir Switching ValveSolvent Delivery Unit (Mobile Phase)Solvent Delivery Unit (Reaction Reagent)MixerColumn for Ammonium TrapAutosamplerColumn OvenAnalysis ColumnReaction CoilFluorescence DetectorData ProcessorWaste
Flow Diagram
121
1 1 6
14
15
4
5
2
2
8 9 11
10
12
1213
6
3
3
7
Prominence Amino Acid Analysis System
Main ComponentsP/N Product Name Model
Li Type
228-45012-XX
228-45002-XX
228-45000-XX
228-18803-92
228-45567-91
228-45018-XX
228-45049-91
228-45060-99
228-45093-93
228-45041-91
228-45007-XX
228-15652-92
228-45010-XX
228-45148-XX
228-35327-XX
228-31170-92
228-18837-91
228-18837-92
228-14206-91
228-00821-91
228-21195-94
228-21195-95
228-21195-93
—
Na Type
Quantity
1
1
2
1
2
2
1
1
1
1
1
1
1
1
1
1
1
1
System Controller
Solvent Delivery Unit (for mobile phase)
Solvent Delivery Unit (for reaction reagent)
20AB Automatic Rinsing Kit
20AD Automatic Rinsing Kit*1
Degassing Unit
Reservoir Switching Valve
Option Box S (VP)
Gradient Mixer
Reservoir Tray
Autosampler
1.5 mL Glass Vial
Column Oven
Fluorescence Detector
Outlet Unit
Amino Acid Analysis Tubing Kit
Analysis Column (for Na type)
Analysis Column (for Li type)
Column for Ammonium Trap (for Na type)
Column for Ammonium Trap (for Li type)
Amino Acid Mobile Phase Kit, Na Type
Amino Acid Mobile Phase Kit, Li Type
Amino Acid Analysis Kit, OPA Reagent
LC Workstation
CBM-20A
LC-20AB
LC-20AD*1
DGU-20A3R*1
FCV-11ALS
Mixer 0.5-2.6 mL HP
SIL-20AC
CTO-20AC*2
RF-20AXS*3
Shim-pack Amino-Na
Shim-pack Amino-Li
Shim-pack ISC-30/S0504 Na
Shim-pack ISC-30/S0504 Li
LabSolutions LC Single LC*4
1
1
1
1
1
1
Conventionally, amino acid analyzers using a ninhydrin reagent have
been used to analyze amino acids. However, as HPLC has become
more widespread, methods using post-column fluorescence
derivatization based on the reaction between ortho-phthalaldehyde
(OPA) reagent and primary amines have been investigated.
Shimadzu created an HPLC amino acid analysis system that
incorporated post-column derivatization by OPA reagent in the late
1970s. However, due to the simultaneous detection of the secondary
amino acid proline, Shimadzu proposed the "non-switching flow"
method that continuously adds an oxidant (sodium hypochlorite) to
the column eluate to establish a highly sensitive amino acid analysis
system.
This is an automated amino acid analysis system that uses post-column fluorescence derivatization detection with Shimadzu's unique OPA/N-acetylcysteine as the reaction reagent.
The fluorescence detector (RF-20AXS) achieves previously unheard of sensitivity, with a water Raman S/N ratio of at least 2000.
Shimadzu's unique N-acetylcysteine (odorless solid) is used as the thiol-based reaction initiation. Compared with the conventional method using mercaptoethanol, it is easier to handle and achieves higher sensitivity for amino acids, such as proline.
The mobile phase and reaction reagent are provided as kits for worry-free analysis.
The PRR-2A peristaltic pump (228-45145) can also be selected to deliver the reaction reagent. In this case, only one DGU-20A5R degassing Unit (228-45019-XX) is used with Trans B-2 (200-45099-02).
CTO-20A (228-45009-XX) can be used with the Na type but not with the Li type.
RF-20A (228-45147-XX) can also be selected.
Separate printer and cables required.
*1:
*2:
*3:
*4:
1.2.3.4.5.6.7.8.9.
10.11.12.13.14.15.
5Application Systems
CHO COOH
H2N C
H
R1
R2
HS-R2
S
N
CHO
++
(N-acetyl-cysteine)
o-phthalaldehyde Amino acid
Fluorescent derivative
COOH
C
H R1
Detection Principle
Generally, 2-mercaptoethanol or ethanethiol is used
as the compound having a thiol group but these
compounds have the bad odor inherent with
sulfhydryl (SH) compounds. Conversely, the
N-acetylcysteine used by Shimadzu is odorless and
permits the highly sensitive detection of amino acids,
including proline.
Data
Analysis of Amino Acids by OPA/N-Acetylcysteine Post-Column Fluorescence Derivatization
The amino acid analysis systems include the Na type, which is mainly suitable for the analysis of protein hydrolyzed amino acids, and the Li
type which is suitable for the simultaneous analysis of free amino acids, such as modified amino acids and amino acid structural analogs.
Fig. 1 Chromatogram of a Mixture of 17 Amino Acid Standard Components(100 nmol/mL each, 10 µL injection volume, Na-type analytical conditions)
Related Documents:
: Shim-pack Amino-Na (100 mmL. × 6.0 mmI.D.): Shim-pack ISC-30/S0504Na (50 mmL. × 4.0 mmI.D.): Amino Acids Mobile Phase Kit (Na type), gradient elution: 0.4 mL/min: 60 °C: 10 µL: Amino Acid Regent Kit: 0.2 mL/min, each: 60 °C: RF-20Axs (Ex. 350 nm, Em. 450 nm): 25 °C
[Analytical Conditions (Na type)]
Column
Ammonia trap
Mobile phase
Mobile phase flow rateColumn temp.Injection volumeReaction reagentReaction reagent flow rateReaction temp.DetectionCell temp.
HPLC Application Report No. 26 "Principles and Applications of the Prominence Amino Acid Analysis System" (C190-E106)
Shimadzu HPLC Amino Acid Analysis System, Application Data Book (C190-E004)
Shimadzu HPLC Food Analysis Applications, Application Data Book (C190-E078)
0 10 20 30 5040 (min.)
1
2
3 4
5
6
7 8
9
1011
12
13
14
15
16
17
1. Asp2. Thr3. Ser4. Glu5. Pro6. Gly7. Ala8.( Cys)29. Val
10. Met11. Ile12. Leu13. Tyr14. Phe15. His16. Lys17. Arg
Peaks
6
Organic Acid Analysis System
Organic Acid Analysis by HPLC
System Characteristics
The analysis of organic acids by HPLC was previously performed using
absorption photometry to detect absorption of the carboxyl group
between 200 and 210 nm. However, some samples are difficult to
analyze by this method, which is susceptible to the effects of impurity
components in this short wavelength range. Conversely, the
electroconductivity detector offers the selective and highly sensitive
detection of ionic substances and is less obstructed by impurity
components than a UV detector. However, it is difficult to use directly
for high-sensitivity detection, as the background electrical
conductivity increases due to the acidic mobile phase and the organic
acid dissociation equilibrium shifts toward the undissociated side.
Consequently, Shimadzu established an organic acid analysis system
using a pH-buffered post-column method. The pH buffer solution is
continuously added to the column eluate to maintain the mixed
solution at near-neutral pH. This promotes dissociation of the organic
acids to enhance the detection sensitivity of the electroconductivity
detector.
Shimadzu's unique pH-buffered post-column method with electrical conductivity detection creates an organic acid analysis system with superior selectivity and sensitivity.
This system first separates the organic acids by ion exclusion chromatography and continuously adds pH buffer solution to the column eluate to maintain a near-neutral pH and detect the organic acids in a dissociated state by the electroconductivity detector.
CBM-20Alite (228-45011-XX) can also be selected. SCL-10AVP (228-45051-XX) is required for LCsolution Ver.1.23, or earlier.
Analysis with a single column is possible for some samples (separation components).
Always use a guard column.
Separate printer and cables required
*1:
*2:
*3:
*4:
64
53
2
131
12
1110
98
7
Mobile PhasepH Buffer SolutionDegassing UnitSolvent Delivery Unit (Mobile Phase)Solvent Delivery Unit (pH Buffer Solution)AutosamplerColumn OvenGuard ColumnAnalysis ColumnMixerElectroconductivity DetectorData ProcessorWaste
Flow Diagram
Main ComponentsP/N Product Name QuantityModel
228-45012-XX
228-45000-XX
228-45018-XX
228-45041-91
228-45007-XX
228-15652-92
228-45010-XX
228-45054-XX
228-35327-XX
228-21747-91
228-17893-91
228-17924-91
—
System Controller
Solvent Delivery Unit (for mobile phase/reaction reagent)
Degassing Unit
Reservoir Tray
Autosampler
1.5 mL Sample Vial (100 vials)
Column Oven
Electroconductivity Detector
Outlet Unit
Tubing ASSY J
Analysis Column
Guard Column
LC Workstation
CBM-20A*1
LC-20AD
DGU-20A3R
SIL-20AC
CTO-20AC
CDD-10A
Shim-pack SCR-102H
SCR-102H Guard Column*3
LabSolutions LC Single LC*4
1
2
1
1
1
1
1
1
1
1
2*2
1
1
VP
Prominence Organic Acid Analysis System
1.2.3.4.5.6.7.8.9.
10.11.12.13.
7Application Systems
Detection PrincipleA pH buffer is mixed with the column eluate to
maintain a near-neutral pH and detect most organic
acids in a dissociated state by the electroconductivity
detector.
CH3COOH CH3COO- Detector
pH buffer solution Buffer action maintainsnear-neutral pH
Column
20%
100%
pKa=4.8
3 4 5 6 7 8 (pH)
pH3 in columnAlmost no dissociation
pH7 at detector inletAlmost complete dissociation
Proportion of dissociated acetic acid
Data
Analysis of Organic Acid by pH-Buffered Post-Column Method with Electrical Conductivity Detection
Related Documents: HPLC Application Report No. 25 "Principles and Applications of the Prominence Organic Acid Analysis System" (C190-E105)
Shimadzu HPLC Food Analysis Applications, Application Data Book (C190-E078)
Permeation Packing
Weak repulsionStrong repulsion
Neutral Weak acid Strong acid
Fig. 1 Principle of Ion Exclusion Chromatography
<Separation>Column
Mobile phaseFlow rateColumn temp.Injection volume
<Detection>pH buffer solutionFlow rateDetectionCell temp.
: Shim-pack SCR-102H (300 mmL. × 8.0 mmI.D.) and Guard Column SCR-102H (50 mmL. × 6.0 mmI.D.) in series: 5 mmol/L p -TSA*
: 0.8 mL/min: 45 °C: 10 µL
: 5 mmol/L p -TSA, 20 mmol/L Bis-Tris, 100 µmol/L EDTA-4H: 0.8 mL/min: CDD-10AVP
: 48 °C
[Analytical Conditions]
* p -TSA: p -toluenesulfonic acid
Fig. 2 Analysis of Organic Acid Standard
Phosphoric acid(α-Ketogultaric acid)Citric acidPyruvic acidMalic acidSuccinic acidLactic acidFormic acid(Fumaric acid)Acetic acidLevulinic acidPyroglutamic acid
Peaks
(min.)
Fig. 3 Analysis of Beer
1.2.3.4.5.6.7.8.9.
10.11.12.
If the ion exclusion mode is used for organic acid analysis, an H+ cation
ion-exchange resin is used as the packing. The organic acid target
components are separated by the degree of Donnan exclusion between
the H+ ion-exchange group and mobile phase at the solid-phase surface.
In this mode, strong acids undergo electrostatic exclusion due to the
negative charge of the solid phase and cannot permeate inside the
packing pores. However, for weak acids such as organic acids, the size
of this charge determines how many of them can permeate the pores,
which results in differences (separation) in the elution time (Fig. 1). As
shown in the diagram, as citric acid and lactic acid have a large negative
charge (small pKa) and undergo greater electrostatic exclusion than
acetic acid, for example, they elute more rapidly. In principle, organic
acids elute sequentially in order from the lowest pKa, and they elute
completely by the elution position for neutral substances (position of
complete pore permeation). Fig. 2 and Fig. 3 show examples of the
analysis of an organic acid standard sample and an actual sample (beer).
(min.)
Phosphoric acidCitric acidPyruvic acidMalic acidSuccinic acidLactic acidFormic acidAcetic acidPyroglutamic acidCarbonic acid
Peaks1.2.3.4.5.6.7.8.9.
10.
8
Reducing Sugar Analysis System
Reducing Sugar Analysis by HPLC
System Characteristics
A refractive index detector is often used for the analysis of sugars by HPLC.
However, the refractive index detector suffers from limitations, such as
poor selectivity and ineffective gradient elution of multiple components and
is not suitable for the analysis of reducing sugars in samples with many
impurity components. Therefore, it is common to react the sugars
separated in the column with a reaction reagent and then use UV/VIS
absorbance detection to detect the generated products or derivatization
detection to detect fluorescence.
Shimadzu realized that arginine, which is a reducing sugar and basic amino
acid, is a substance that generates a fluorescent derivative when heated in
the presence of boric acid. It applied this reaction to a post-column reaction
system to establish the reducing sugar analysis system.
This system uses post-column fluorescence derivatization detection with Shimadzu's unique arginine reaction reagent.
The fluorescence detector (RF-20AXS) achieves previously unheard of sensitivity with a water Raman S/N ratio of at least 2000.
After separating the sugars using anion exchange chromatography, for example, the column eluate is continuously spiked with arginine/boric acid reagent and heated to cause a reaction. The fluorescent derivatives formed are detected by a fluorescence detector.
It permits highly selective and sensitive analysis of reducing sugars in samples that contain many impurity components.
*1:
*2:
*3:
Main Components
Mobile PhaseSolvent Delivery Unit (for Mobile Phase)Degassing UnitMixerAutosamplerColumn OvenGuard ColumnAnalysis ColumnReaction ReagentSolvent Delivery Unit (for Reaction Reagent)Chemical Reaction BoxReaction CoilCooling CoilFluorescence DetectorData ProcessorWaste
Flow Diagram
Prominence Reducing Sugar Analysis System
P/N Product Name QuantityModel
228-45012-XX
228-45002-XX
228-45000-XX
228-18803-92
228-45567-91
228-45019-XX
228-45093-93
228-45041-91
228-45007-XX
228-15652-92
228-45010-XX
228-45148-XX
228-35327-XX
228-45065-XX
228-41681-91
228-09699-91
228-00823-91
—
System Controller
Solvent Delivery Unit (for mobile phase)
Solvent Delivery Unit (for reaction reagent)
20AB Automatic Rinsing Kit
20AD Automatic Rinsing Kit
Degassing Unit
Gradient Mixer
Reservoir Tray
Autosampler
1.5 mL Glass Vial
Column Oven
Fluorescence Detector
Outlet Unit
Chemical Reaction Box
Tubing H-PO ASSY
Analysis Column
Guard Column
LC Workstation
CBM-20A
LC-20AB
LC-20AD
DGU-20A5R
Mixer 0.5-2.6 mL HP
SIL-20AC
CTO-20AC
RF-20AXS*1
CRB-6A
Shim-pack ISA-07/S2504*2
Shim-pack Guard Column ISA
LabSolutions LC Single LC*3
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
RF-20A (228-45147-XX) can also be selected.
This is a cation-exchange column. A ligand exchange column or normal-phase column may also be used.
Separate printer and cables required.
+
1.2.3.4.5.6.7.8.9.
10.11.12.13.14.15.16.
1
5
6
7
8
13
15
16
12
11
109
2
4
3
1
14
9Application Systems
Detection PrincipleThe column eluate is continuously spiked with a
arginine/boric acid reagent and heated to cause a
reaction that forms fluorescent derivatives of the
sugars, which are detected by a fluorescence detector.
Data
Analysis of Reducing Sugars by Arginine Post-Column Fluorescence Derivatization Detection
CH2 OH
H
OH H
OHH
H +O
OH
COOH
H2 NCH
(CH2)3
NH
Arginine
Sugar
Boric acid
Fluorescent derivative
Heating
C=NH
NH2
HO
Fig. 1 Analysis of 11 Sugar Standards Fig. 2 High-Sensitivity Analysis
<Separation>ColumnGuard columnMobile phase
Flow rateColumn temp.Injection volume
: Shim-pack ISA-07/S2504 (250 mmL. × 4.0 mmI.D.): Shim-pack Guard Column ISA (50 mmL. × 4.0 mmI.D.) : A : 0.1 mol/L Potassium borate buffer (pH8)
B : 0.4 mol/L Potassium borate buffer (pH9) A B Linear gradient elution: 0.6 mL/min: 65 °C: 10 µL
<Detection>Reaction reagentFlow rateReaction coilReaction temp.DetectionCell temp.
: 10 g/L Arginine, 30 g/L Boric acid: 0.5 mL/min: SUS, 10 mL. × 0.8 mm I.D.: 150 °C: RF-20Axs (Ex. 320 nm, Em. 430 nm): 25 °C
(min.)250 50
11
10
98
7
6
5
43
21
75(min.)250 50 75
1110
9876
54
321
SucroseCellobioseMaltoseLactoseRhamnoseRiboseMannoseArabinoseGalactoseXyloseGlucose
SucroseCellobioseMaltoseLactoseRhamnoseRiboseMannoseArabinoseGalactoseXyloseGlucose
[Analytical Conditions]
Peaks
Peaks
Related Documents: Shimadzu Application News No. L382 "Determination of Carbohydrates by Hydrophilic Interaction Chromatography with Post-column
Fluorometric Detection" (LAAN-A-LC-E162)
Shimadzu Application News No. L394 "Applications of Prominence RF-20AXS Fluorescence Detector (Part 3), Analysis of Saccharides Using
Post-Column Derivatization System" (LAAN-A-LC-E173)
Shimadzu HPLC Food Analysis Applications, Application Data Book (C190-E078)
1.2.3.4.5.6.7.8.9.
10.11.
1.2.3.4.5.6.7.8.9.
10.11.
Diverse types of sugars exist, such as monosaccharides,
polysaccharides, neutral sugars, amino sugars, and sugar alcohols,
and many of these have isomers. To analyze sugars by HPLC, it is
important to select the appropriate separation and detection
methods for the target sugar type.
The standard analytical conditions for anion exchange
chromatography are shown below. Fig. 1 shows the simultaneous
analysis of 11 sugar components (200 µmol/L each (sucrose only 2
mmol/L), 10 µL injection volume). Fig. 2 shows the chromatogram
for a sugar standard solution by high-sensitivity analysis (2 µmol/L
each (sucrose only 20 µmol/L), 10 µL injection volume). The glucose
absolute injection volume is 20 pmol (3.6 ng). It can be seen that
the glucose is detected with a satisfactory S/N ratio.
10
Carbamate Analysis System
Analysis of N-Methylcarbamate Pesticides by HPLC
System Characteristics
N-methylcarbamate pesticides are used as insecticides. The target value is
set according to the residual limit value in Japan's Positive List System for
Agricultural Chemical Residues in Foods and the water quality control
target setting items (agricultural chemicals) based on the Ministerial
Ordinance Concerning Water Quality Standards. The HPLC post-column
fluorescence derivatization method using ortho-phthalaldehyde (OPA) as
the reaction reagent is adopted as the analytical method for these
components.
N-methylcarbamate pesticides are separated by reverse-phase
chromatography, converted to methyl amines (primary amines) by alkaline
hydrolysis, reacted with OPA, and detected by a fluorescence detector.
This analysis system uses post-column fluorescence derivatization detection with OPA as the reaction reagent.
The fluorescence detector (RF-20AXS) achieves previously unheard of sensitivity with a water Raman S/N ratio of at least 2000.
It permits highly selective and sensitive analysis of N-methylcarbamate pesticides in foods and tap water.
Main Components
Mobile PhaseReaction ReagentDegassing UnitSolvent Delivery Unit (Mobile Phase)MixerAutosamplerColumn OvenAnalysis ColumnChemical Reaction BoxSolvent Delivery Unit (Reaction Reagent)Reaction Reagent Introduction CoilReaction CoilCooling CoilReaction Tube KitFluorescence DetectorData ProcessorWaste
Flow Diagram
P/N Product Name QuantityModel
228-45012-XX
228-45002-XX
228-45000-XX
228-45567-91
228-45019-XX
228-45093-93
228-45041-91
228-45007-XX
228-15652-92
228-45010-XX
228-45148-XX
228-35327-XX
228-45065-XX
228-33943-91
228-40511-92
(A-330)
—
System Controller
Solvent Delivery Unit (for mobile phase)
Solvent Delivery Unit (for reaction reagent)
20AD Automatic Rinsing Kit
Degassing Unit
Gradient Mixer
Reservoir Tray
Autosampler
1.5 mL Glass Vial
Column Oven
Fluorescence Detector
Outlet Unit
Chemical Reaction Box
Carbamate Analysis Tubing Kit
Analysis Column
Inline Filter*2
LC Workstation
CBM-20A
LC-20AB
LC-20AD
DGU-20A5R
Mixer 0.5-2.6 mL HP
SIL-20AC
CTO-20AC
RF-20AXS*1
CRB-6A
Shim-pack FC-ODS (75mm×4.6mmI.D.)
LabSolutions LC Single LC*3
1
1
2
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Prominence Carbamate Analysis System
*1:
*2:
*3:
RF-20A (228-45147-XX) can also be selected.
Upchurch semi-prep filter (Use to analyze residual pesticides in foods.)
Separate printer and cables required.
1.2.3.4.5.6.7.8.9.
10.11.12.13.14.15.16.17.
1 1
2
172
11
9
12 13
7
6
4
14 15
16
5
10
103
8
11Application Systems
Detection PrincipleN-methylcarbamate pesticides are separated in the
column and subjected to alkaline hydrolysis to create
methyl amines. These methyl amines are reacted with
ortho-phthalaldehyde (OPA) to form fluorescent
derivatives that are detected by a fluorescence detector.
Data
Analysis of N-Methylcarbamate Pesticides by OPA Post-Column Fluorescence Derivatization Detection
Fig. 1 shows an example of the high-sensitivity analysis of a standard mixture of eight N-methylcarbamate pesticides (5 µg/L each, 10 µL
injection volume). The absolute injection volume of each component is 50 pg.
Related Documents:
Shimadzu Application News No. L343 "Analysis of N-Methylcarbamate Pesticides in Foods" (LAAN-A-LC-E054)
Shimadzu Application News No. L399 "Applications of the "Prominence RF-20AXS" Fluorescence Detector (Part 4), Analysis of Pesticides with a Postcolumn
Derivatization System" (LAAN-A-LC-E177)
[References]
"Notes on Enforcement of Ministerial Ordinance Concerning Water Quality Standards, Partial Revision of Water Supply Act Enforcement Regulations and Water
Quality Control" (Japanese Ministry of Health, Labour and Welfare; Health Service Bureau, Water Supply Div. Ordinance No. 1010001, October 10, 2003 [partial
revision, Ministry of Health, Labour and Welfare; Health Service Bureau, Water Supply Div. Ordinance 0217, No. 1, February 17, 2010]), "Exhibit 4 Test Methods of
Water Quality Control Target Setting Items"
"Test Methods for Pesticide Residues in Food and Animal Feed Additives or Ingredients of Pharmaceutical Products for Animals" (Japanese Ministry of Health,
Labour and Welfare Notification No. 0124001, January 24, 2005) (Appendix) [Final revision August 2, 2010]
Fig. 1 Chromatogram of a Standard Solution of 8 N-Methylcarbamate Pesticides (5 µg/L, 10 µL injection volume)
CHO
ROHRO
O
H3CNH2
H3CNH2
H3CHN
CHOR' OH-
OH-
CO3
S-R'
N-CH3SH
o-phthalaldehyde
(3-mercaptopropionic acid)
Fluorescent derivative
2-
100Methylamine
<Separation>ColumnMobile phaseTime program
Flow rateColumn temp.Injection volume
: Shim-pack FC-ODS (75 mmL. × 4.6 mmI.D.): A : Water, B : Methanol: B conc. = 14 % (0-4 min) 40 %(10 min) 45 % (17 min) → 50 % (20-26 min) → 14 % (26.01-35 min)
: 1.0 mL/min: 50 °C: 10 µL
<Detection>Reagent 1Flow rateReaction temp.Reagent 2
Flow rateReaction temp.DetectionCell temp.
: 50 mmol/L Sodium hydroxide : 0.5 mL/min: 100 °C: 120 mmol/L Sodium borate buffer (pH9) containing 0.25 mmol/L OPA and 0.25 mmol/L 3-Mercaptopropionic acid: 0.5 mL/min: 50 °C: RF-20AXS (Ex. 339 nm, Em. 445 nm): 25 °C
[Analytical Conditions]
21 3 4
5
6
7 8
1. Aldicarb sulfoxide2. Aldicarb sulfone3. Oxamyl4. Aldicarb5. Bendiocarb6. Carbaryl7. Ethiofencarb8. Fenobucarb (50 pg each)
0 5 10 15 20 (min.)25
Peaks
1)
2)
12
Iminoctadine Analysis System
Iminoctadine Analysis by HPLC
System Characteristics
Iminoctadine is a pesticide used as an insecticide. The target value (as
acetate) is set according to the residual limit value in Japan's Positive
List System for Agricultural Chemical Residues in Foods and the water
quality control target setting items (agricultural chemicals) based on
the Ministerial Ordinance Concerning Water Quality Standards. The
HPLC post-column fluorescence derivatization method using
ninhydrin as the reaction reagent is adopted as the analytical method
for iminoctadine.
Iminoctadine is separated by reverse-phase chromatography, reacted
by the aqueous sodium hydroxide solution and ninhydrin, and then
detected by a fluorescence detector.
This analysis system uses post-column fluorescence derivatization detection with ninhydrin as the reaction reagent.
The fluorescence detector (RF-20AXS) achieves previously unheard of sensitivity with a water Raman S/N ratio of at least 2000.
It permits highly selective and sensitive analysis of iminoctadine acetate in foods and tap water.
*1:*2:
RF-20A (228-45147-XX) can also be selected. Separate printer and cables required.
Mobile PhaseDegassing UnitSolvent Delivery Unit (Mobile Phase)AutosamplerColumn OvenAnalysis ColumnReaction ReagentSolvent Delivery Unit (Reaction Reagent)Reaction ChamberReaction CoilCooling CoilFluorescence DetectorData ProcessorWaste
Flow Diagram
Prominence Iminoctadine Analysis System
P/N Product Name QuantityModel
228-45012-XX
228-45000-XX
228-45567-91
228-45019-XX
228-45041-91
228-45007-XX
228-31600-91
228-45010-XX
228-45148-XX
228-35327-XX
228-45065-XX
228-46304-91
228-34937-91
—
System Controller
Solvent Delivery Unit (for mobile phase/reaction reagent)
20AD Automatic Rinsing Kit
Degassing Unit
Reservoir Tray
Autosampler
1 mL PP Vial
Column Oven
Fluorescence Detector
Outlet Unit
Chemical Reaction Box
Iminoctadine Analysis Tubing Kit
Analysis Column
LC Workstation
CBM-20A
LC-20AD
DGU-20A5R
SIL-20AC
CTO-20AC
RF-20AXS*1
CRB-6A
Shim-pack VP-ODS (150mm×4.6mmI.D.)
LabSolutions LC Single LC*2
1
3
2
1
1
1
1
1
1
1
1
1
1
1
Main Components
1.2.3.4.5.6.7.8.9.
10.11.12.13.14.
13
1
7
7
14
4
10
9
11
512
3
8
82
6
13Application Systems
Detection PrincipleIminoctadine is reacted with ninhydrin under alkaline
conditions to form fluorescent derivatives that are
detected by a fluorescence detector.
Data
Analysis of Iminoctadine by Post-Column Fluorescence Derivatization Detection Using Ninhydrin as the Reaction Reagent
Fig. 1 shows the chromatogram for iminoctadine triacetate solution (5 µg/L (3.3 µg/L as iminoctadine), prepared at mobile phase).
The water quality control target value for iminoctadine triacetate is 6 µg/L. The test method involves concentrating the sample 200 times.
However, the RF-20AXS permits direct detection with 10 µL injection volume, without sample concentration.
Related Documents:
Shimadzu Application News No. L312 " Analysis of Iminoctadine Triacetate in Drinking Water by HPLC" (LAAN-A-LC-E013)
Shimadzu Application News No. L399 "Applications of the "Prominence RF-20AXS" Fluorescence Detector (Part 4), Analysis of Pesticides with a Postcolumn
Derivatization System" (LAAN-A-LC-E177)
[References]
"Notes on Enforcement of Ministerial Ordinance Concerning Water Quality Standards, Partial Revision of Water Supply Act Enforcement Regulations and Water
Quality Control" (Japanese Ministry of Health, Labour and Welfare; Health Service Bureau, Water Supply Div. Ordinance No. 1010001, October 10, 2003
[partial revision, Ministry of Health, Labour and Welfare; Health Service Bureau, Water Supply Div. Ordinance 0217, No. 1, February 17, 2010]), "Exhibit 4 Test
Methods of Water Quality Control Target Setting Items"
"Test Methods for Pesticide Residues in Food and Animal Feed Additives or Ingredients of Pharmaceutical Products for Animals" (Japanese Ministry of Health,
Labour and Welfare Notification No. 0124001, January 24, 2005) (Appendix) [Final revision August 2, 2010]
Fig. 1 Chromatogram of Iminoctadine Triacetate (5 µg/L, 10 µL injection volume)
1. Iminoctadine triacetate
1
0 5 10 (min.)
<Separation>ColumnMobile phase
Flow rateColumn temp.Injection volume
: Shim-pack VP-ODS (150 mmL. × 4.6 mmI.D.): A : 30 mmol/L Lactate buffer (pH3.7) containing 100 mmol/L Sodium perchlorate, 10 mmol/L Sodium hydroxide B : Acetonitrile A / B = 17 / 5 ( v / v ): 0.6 mL/min: 50 °C : 10 µL
<Detection>Reagent 1Flow rateReagent 2Flow rateReaction temp.DetectionCell temp.
: 0.5 mol/L Sodium hydroxide : 0.2 mL/min: 3 g/L Ninhydrin solution: 0.1 mL/min : 90 °C: RF-20AXS (Ex. 395 nm, Em. 500 nm): 25 °C
[Analytical Conditions]
Iminoctadine triacetate
Fluorescent derivativeNinhydrin
NH2+
OH -
NH2ーCーNHー(CH2)8ーNH2+ー(CH2)8ーNHーCーNH2・〔3 CH3COO-〕
NH2+
Peaks
1)
2)
14
Synthetic Antimicrobial Analysis System
Analysis of Synthetic Antimicrobials by HPLC
System Characteristics
HPLC is widely used to analyze residual antimicrobials in meat and seafood
to ensure food safety. Many types of synthetic antimicrobials are used. They
are qualified through the simultaneous analysis of multiple components by
gradient elution and using the spectral information from a photodiode
array detector or MS detector.
This is an analysis system that detects synthetic antimicrobials in foods using a photodiode array detector or MS detector.
It permits the simultaneous analysis of synthetic antimicrobials in meat and seafood.
Qualitative information can be obtained from a UV spectrum or MS spectrum.
*1:*2:
CBM-20Alite (228-45011-XX) can also be selected. Separate printer and cables required.
Prominence Synthetic Antimicrobial Analysis System(MS Detector)
Prominence Synthetic Antimicrobial Analysis System(Photodiode Array Detector)
228-45012-XX
228-45002-XX
228-45018-XX
228-35830-92
228-45041-91
228-45007-XX
228-15652-92
228-45010-XX
228-34937-94
225-13300-XX
225-25150-92
System Controller
Solvent Delivery Unit
Degassing Unit
Semi-Micro Gradient Mixer
Reservoir Tray
Autosampler
1.5 mL Glass Vial
Column Oven
Analysis Column
Mass Spectrometer
LCMS-2020 System package
CBM-20A
LC-20AB
DGU-20A3R
Mixer SUS
SIL-20AC
CTO-20AC
Shim-pack VP-ODS(150mm×2.0mm I.D.)
LCMS-2020
1
1
1
1
1
1
1
1
1
1
1
P/N Product Name QuantityModel
P/N Product Name QuantityModel
228-45012-XX
228-45002-XX
228-45018-XX
228-45093-93
228-45041-91
228-45007-XX
228-15652-92
228-45010-XX
228-45005-XX
228-34937-91
—
System Controller
Solvent Delivery Unit
Degassing Unit
Gradient Mixer
Reservoir Tray
Autosampler
1.5 mL Glass Vial
Column Oven
Photodiode Array Detector
Analysis Column
LC Workstation
CBM-20A*1
LC-20AB
DGU-20A3R
Mixer 0.5-2.6 mL HP
SIL-20AC
CTO-20AC
SPD-M20A
Shim-pack VP-ODS (150mm×4.6mmI.D.)
LabSolutions LC Multi LC-PDA*2
1
1
1
1
1
1
1
1
1
1
1
Main Components
Main Components
15Application Systems
Data
Analysis of Synthetic Antimicrobials Using a Photodiode Array Detector or MS Detector
Fig. 1 shows the simultaneous analysis of 19 synthetic antimicrobial standards using a photodiode array detector.
Fig. 2 shows the MS spectra and UV spectra (measured by a photodiode array detector) for four of the separated synthetic antimicrobials.
The MS detector and photodiode array detector achieve high selectivity and provide useful qualitative information from the simultaneous
analysis of multiple target compounds.
Fig. 2 Simultaneous Analysis of 19 Synthetic Antimicrobials
Related Document: Shimadzu HPLC Food Analysis Applications, Application Data Book (C190-E078)
Fig. 1 Simultaneous Analysis of 19 Synthetic Antimicrobials
[Analytical Conditions]
[Analytical Conditions]
ColumnMobile phase
Flow rateTemp.Detection
: STR ODS-II (150 mmL. × 4.6 mmI.D.): A : Water/Acetic acid = 100/0.3 (v/v) (containing 100 mmol/L NaClO4) B : Acetonitrile/Water/Acetic acid = 90/10/0.3 (v/v/v) (containing 100 mmol/L NaClO4) A/B Gradient elution: 2.0 mL/min: 40 °C: Photodiode Array SPD-M20A (190−600 nm)
ColumnMobile phase
Flow rateTemp.
: 0.2 mL/min: 40 °C
: Shim-pack VP-ODS (150 mmL. × 2.0 mmI.D.): A: Water/Acetic acid = 100/0.3 (v/v) B: Acetonitrile/Mobile phase A = 90/10 (v/v) A/B Gradient elution
0 10 20 30 (min.)
1
2
345
67
8
9
10
11
121314 15
16 17
18
19
Olaquindox (ODX)Clopidol (CLP)Sulfamerazine (SMR)Thiamphenicol (TP)Carbadox (CDX)Sulphadimidine (SDD)Furazolidone (FZ)Sulfamonomethoxine (SMMX)Trimethoprim (TMP)Ormetoprim (OMP)Oxolinic acid (OA)Sulfadimethoxine (SDMX)Sulfaquinoxaline (SQ)Morantel citrate (MRT)Nalidixic acid (NA)Pyrimethamine (PYR)Piromidic acid (PA)Difurazone (DFZ)Nicarbazin (NCZ)
Peaks1.2.3.4.5.6.7.8.9.
10.11.12.13.14.15.16.17.18.19.
16
Bromate Analysis System
Bromate Analysis by HPLC
System Characteristics
As the ozonation of tap water becomes more widespread, increasing
attention has been focused on the oxidative halogen acid byproducts, such
as bromates. Bromates must be measured at µg/L-level sensitivity.
Revisions to the Ministerial Ordinance Concerning Water Quality Standards
were announced on May 30, 2003 (Japanese Ministry of Health, Labour
and Welfare Ordinance No. 101, April 1, 2004), and the test method was
notified on July 22, 2003 (Japanese Ministry of Health, Labour and Welfare
Notification No. 261).
As the water quality control standard for bromate is 0.01 mg/L,
post-column ion chromatography is the designated test method.
The instrument must provide accuracy of CV10 % max. at one-tenth
concentration (0.001 mg/L (1 µg/L)).
This bromate analysis system measures bromates using ion chromatography with post-column absorption detection (tribromide ion method), based on the water quality test method.
Shimadzu's proven post-column reaction technique combined with a highly sensitive UV-VIS detector achieves sub-µg/L detection sensitivity.
The post-column unit is a kit containing the pipe components required for the tribromide ion method, which includes a mixing device (Japanese Patent No. 4082309) to effectively mix in the concentrated reaction reagent.
It can perform the simultaneous quantitation of oxidative halogen acids. It permits the simultaneous quantitation of iodate ions and chlorite ions as oxidative halogen acids.
Main Components
Mobile PhaseDegassing UnitSolvent Delivery Unit (Mobile Phase)AutosamplerColumn OvenAnalysis ColumnReaction ReagentSolvent Delivery Unit (Reaction Reagent)Reaction CoilUV-VIS DetectorData ProcessorWaste
1
7
7
12
49 9
5 10
3
8
82
6Flow Diagram
Prominence Bromate Analysis System
228-45012-XX
228-45000-XX
228-45089-XX
228-45567-91
228-45019-XX
228-45041-91
228-45075-XX
228-32651-18
228-45064-91
228-31537-91
228-45009-XX
228-45003-XX
228-33338-91
228-35327-XX
228-45350-91
228-46884-91
228-46884-93
—
System Controller
Solvent Delivery Unit (for mobile phase/reaction reagent)
Solvent Delivery Unit (for reaction reagent)
20AD Automatic Rinsing Kit
Degassing Unit
Reservoir Tray
Autosampler
Sample Loop 500 µL PEEK
Sample Cooler L
4 mL PP Vial
Column Oven
UV-VIS Detector
Inert Cell
Outlet Unit
Bromate Analysis Tubing Kit
Analysis Column
Guard Column
LC Workstation
CBM-20A
LC-20AD
LC-10Ai
DGU-20A5R
SIL-10Ai
CTO-20A
SPD-20A
For SPD-20A/20AV
Shim-pack IC-Bromate
Shim-pack IC-Bromate(G)
LabSolutions LC Single LC*
1
2
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
P/N Product Name QuantityModel
*: Separate printer and cables required.
1.2.3.4.5.6.7.8.9.
10.11.12.
11
17Application Systems
Data
Analysis of Bromates Using Post-Column Ion Chromatography
Fig. 1 shows an example of the analysis of an iodate ion standard solution (1 to 10 µg/L concentration, 200 µL injection volume).
Fig. 2 and Fig. 3 show examples of the analysis of 200 µL tap water and of tap water spiked to 5 µg/L bromate.
Highly sensitive detection is achieved at one-tenth the reference concentration value.
Detection PrincipleBromates are converted to tribromide ions through a
reaction with a potassium bromide/sulfuric acid solution.
These are detected through UV absorption at 268 nm.
Tribromide ion method
BrO3-+5Br-+6H+
Br2+Br- Br3-
3Br2+3H2O
Fig. 1 Chromatogram of Bromate Standard
Fig. 2 Analysis of Tap Water
Fig. 3 Analysis of Tap Water Spiked to 1 µg/L Bromate
<Separation>ColumnGuard columnMobile phaseFlow rateColumn temp.Injection volume
: Shim-pack IC-Bromate (150 mmL. × 4.0 mmI.D.): Shim-pack IC-Bromate (G) (10 mmL. × 4.6 mmI.D.): 12 mmol/L NaHCO3 + 0.6 mmol/L Na2CO3
: 1.0 mL/min: 40 °C: 200 µL
<Detection>First reaction Reaction reagent Flow rate Reaction temp.Second reaction Reaction reagent Flow rate Reaction temp.Detection
: 1.5 mol/L KBr + 1.0 mol/L H2SO4
: 0.4 mL/min: 40 °C
: 1.2 mmol/L NaNO2
: 0.2 mL/min.: 40°C: SPD-20A (268 nm) (Lamp: D2)
[Analytical Conditions]
0 1 2 3 4 5 6 7(min.)
BrO3-
0 1 2 3 4 5 6 7(min.)
BrO3-
0 1 2 3 4 5 6 7(min.)
BrO3-
18
Cyanide Analysis System
Cyanide Analysis by HPLC
System Characteristics
Cyanide compounds are toxic substances that have been detected in
industrial effluent and groundwater. They are target substances for control
and inspection under the Ministerial Ordinance Concerning Water Quality
Standards. Revisions to the Ministerial Ordinance Concerning Water Quality
Standards were announced on May 30, 2003 (Japanese Ministry of Health,
Labour and Welfare Ordinance No. 101, April 1, 2004), and the test
method was notified on July 22, 2003 (Japanese Ministry of Health, Labour
and Welfare Notification No. 261, partially revised on February 17, 2010).
Post-column ion chromatography is the designated test method. The
instrument must provide accuracy of CV 10 % max. at one-tenth
concentration (0.001 mg/L (1 µg/L)).
This is a highly sensitive analysis system for cyanide ions and cyanogen chloride. It uses ion chromatography with post-column absorption detection (4-pyridinecarboxylic acid-pyrazolone method), based on the water quality test method.
It permits the highly sensitive simultaneous analysis of cyanide and cyanogen chloride by chemical form.
A column oven with cooling function offers thermal recycling to use the reaction heat from the reaction at the second stage for the reaction at the first stage.
High sensitivity. Limit of detection (SN ratio = 3): 0.0001 mg/L (CN- converted value). Easily achieves measurements at one-tenth the reference concentration (0.01 mg/L). The unique, high-performance column permits analysis of a sample in less than ten minutes.
Main Components
*: Separate printer and cables required.
Mobile PhaseDegassing UnitSolvent Delivery Unit (Mobile Phase)AutosamplerColumn OvenAnalysis ColumnReaction ReagentSolvent Delivery Unit (Reaction Reagent)Reaction Coil 1Reaction Coil 2Reaction ChamberCooling CoilUV-VIS DetectorData ProcessorWaste
1
7
7
15
14
49
10
11
12
5 13
3
8
82
6Flow Diagram
Prominence Cyanide Analysis System
P/N Product Name QuantityModel
228-45012-XX
228-45000-XX
228-45567-91
228-45019-XX
228-45041-91
228-45075-XX
228-32651-18
228-45064-91
228-31537-91
228-45010-XX
228-45004-XX
228-35327-92
228-45065-XX
228-45352-91
228-18837-91
228-18837-93
—
System Controller
Solvent Delivery Unit
20AD Automatic Rinsing Kit
Degassing Unit
Reservoir Tray
Autosampler
Sample Loop 500 µL PEEK
Sample Cooler L
4 mL PP Vial
Column Oven
UV-VIS Detector
Outlet Unit
Chemical Reaction Box
Cyanide Analysis Tubing Kit
Analysis Column
Guard Column
LC Workstation
CBM-20A
LC-20AD
DGU-20A5R
SIL-10Ai
CTO-20AC
SPD-20AV
CRB-6A
Shim-pack Amino-Na
Shim-pack IC-CN(G)
LabSolutions LC Single LC*
1
3
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1.2.3.4.5.6.7.8.9.
10.11.12.13.14.15.
19Application Systems
Data
Analysis of Cyanide Ions and Cyanogen Chloride by Post-Column Ion Chromatography
Detection PrincipleCyanide and cyanogen chloride are separated by ion
chromatography, reacted with chloramine-T to create
cyanogen chloride, and then reacted with
4-pyridinecarboxylic acid-pyrazolone.
The blue reaction products from this reaction are
measured by absorbance at 638 nm wavelength.
Related Document:
Fig. 1 Chromatogram of Cyanide Ion and Cyanogen Chloride Standards
Fig. 2 Calibration Curves for Cyanide Ion and Cyanogen Chloride Standards Fig. 3 Analysis of Tap Water Spiked to 1 µg/L Cyanide Ions
Fig. 1 shows the analysis reproducibility for a cyanide
standard solution (1 µg/L concentration, 100 µL
injection volume). Excellent reproducibility is achieved
at one-tenth the reference concentration value (0.01
mg/L). Fig. 2 shows the calibration curves in the
concentration range from 0.5 to 100 µg/L.
Fig. 3 shows the analysis of a tap water sample
spiked to 1 µg/L cyanide ions. Due to effects of the
residual chlorine in the tap water, most cyanide ions
are detected after conversion to cyanogen chloride.
200 40 60 80 100 (μg/L) 200 40 60 80 100 (μg/L)
Pea
k A
rea
<Separation>Column
Mobile phaseFlow rateColumn temp.Injection volume
: Shim-pack Amino-Na (100 mmL. × 6.0 mmI.D.): 10 mmol/L Tartrate (Na) buffer: 0.6 mL/min: 40 °C: 100 µL
<Detection>First Reaction Reaction Reagent Flow rate Reaction Temp.Second Reaction Reaction Reagent Flow rate Reaction Temp.Detection
: 100 mmol/L Phosphate buffer containing 1.8 mmol/L Chloramine T: 0.5 mL/min: 40 °C
: 14.4 mmol/L 1-Phenyl-3-methyl-5-pyrazolone + 48.3 mmol/L 4- Pyridinecarboxylate (Na): 0.5 mL/min: 100 °C: SPD-20AV (638 nm) (Lamp: W)
[Analytical Conditions]
Pea
k A
rea
10 2 3 4 5 6 7 8(min.)
10 2 3 4 5 6 7 8 (min.)
(Spiked)
(Not spiked)
Blue compound (λmax = 638 nm)
Chloramine-T
4-pyridinecarboxylic acid
1-phenyl-3-methyl-5-pyrazolone
Shimadzu Application News No. L301 "Analysis of Cyanide Ion and Cyanogen Chloride by Post-column Ion Chromatography" (LA190-019A)
20
Anionic Surfactant Analysis System
Analysis of Anionic Surfactant by HPLC
System Characteristics
Of the many types of surfactant available, anionic surfactants are widely used in our
everyday lives as the major component of synthetic detergents. Because they do not
break down in the sewage system, they exist in environmental water. Revisions to
the Ministerial Ordinance Concerning Water Quality Standards were announced on
May 30, 2003 (Japanese Ministry of Health, Labour and Welfare Ordinance No. 101,
April 1, 2004), and the test method was notified on July 22, 2003 (Japanese Ministry
of Health, Labour and Welfare Notification No. 261, partially revised on February 17,
2010). The water quality standard is set at a total of 0.2 mg/L max. for five anionic
surfactants. HPLC is adopted as the test method. HPLC offers highly sensitive analysis
of anionic surfactants after only simple concentration pretreatment.
Anionic surfactant analysis system based on the water quality test method.
The fluorescence detector (RF-20AXS) achieves previously unheard of sensitivity with a water Raman S/N ratio of at least 2000.
The grouping and group calibration curve functions permit quantitation by calculating the total peak area of multiple isomers with different alkyl chains.
The system using a MS detector can obtain more qualitative information for all types of surfactant.
Main Components
Main Components
Detection PrincipleThe water quality control standard for the target anionic
surfactants is set at a total of 0.2 mg/L for five anionic surfactants.
Each component includes isomers with different alkyl chains. They
can be separated by a reverse-phase column and detected by a
fluorescence detector.
*1:*2:*3:
CBM-20Alite (228-45011-XX) can also be selected. RF-20A (228-45147-XX) can also be selected. Separate printer and cables required.
CnH2n+1
SO3Na
n = 10: sodium decylbenzenesulfonaten = 11: sodium undecylbenzenesulfonaten = 12: sodium dodecylbenzenesulfonaten = 13: sodium tridecylbenzenesulfonaten = 14: sodium tetradecylbenzenesulfonateSO3Na n = 14: sodium tetradecylbenzenesulfonate
Prominence Anionic Surfactant Analysis System (Fluorescence Detector)
228-45012-XX
228-45000-XX
228-45018-XX
228-45041-91
228-45007-XX
228-15652-92
228-45010-XX
228-45148-XX
228-34937-92
—
System Controller
Solvent Delivery Unit
Degassing Unit
Reservoir Tray
Autosampler
1.5 mL Glass Vial
Column Oven
Fluorescence Detector
Analysis Column
LC Workstation
CBM-20A*1
LC-20AD
DGU-20A3R
SIL-20AC
CTO-20AC
RF-20AXS*2
Shim-pack VP-ODS (250mm×4.6mmI.D.)
LabSolutions LC Single LC*3
1
1
1
1
1
1
1
1
1
1
Prominence Anionic Surfactant Analysis System (MS Detector)
228-45012-XX
228-45002-XX
228-45018-XX
228-35830-92
228-45041-91
228-45007-XX
228-15652-92
228-45010-XX
228-34937-94
225-13300-XX
225-25150-92
System Controller
Solvent Delivery Unit
Degassing Unit
Semi-Micro Gradient Mixer
Reservoir Tray
Autosampler
1.5 mL Glass Vial
Column Oven
Analysis Column
Mass Spectrometer
LCMS-2020 System Packcage
CBM-20A
LC-20AB
DGU-20A3R
Mixer 100 µL HP
SIL-20AC
CTO-20AC
Shim-pack VP-ODS (150mm×2.0mm I.D.)
LCMS-2020
1
1
1
1
1
1
1
1
1
1
1
P/N Product Name QuantityModel
P/N Product Name QuantityModel
21Application Systems
Data
Analysis of Anionic Surfactants Conforming to the New Water Quality Test Method
Related Document: Shimadzu Application News No. L392 "Applications of the Prominence RF-20AXS Fluorescence Detector (Part 1)
High Sensitivity Analysis of Anionic Surfactants, tert-Butylhydroquinone, and Amitrole" (LAAN-A-LC-E171)
[References]
Japanese Ministry of Health, Labour and Welfare Ordinance No. 101 (May 30, 2003), [Partial revision of Ministry of Health, Labour and Welfare Ordinance No.
135 (November 14, 2007)]
Japanese Ministry of Health, Labour and Welfare Notification No. 261 (July 22, 2003), [Partial revision of Ministry of Health, Labour and Welfare Notification
No. 56 (February 17, 2010)]
Fig. 1 Chromatogram of a Standard Mixture of Five Anionic Surfactant Components(0.04 mg/L each, total 0.2 mg/L, no concentration)
Fig. 3 Mass Spectra of Alkylphenyl Polyoxyethylene SulfateFig. 2 Mass Chromatogram of Alkylphenyl Polyoxyethylene Sulfate
Fig. 1 shows the results for a 20 µL injection volume of a mixture of five anionic surfactant components equivalent to the reference concen-
tration (0.04 mg/L each, total 0.2 mg/L). This test method is prescribed as injecting the sample into the HPLC after pretreatment to concen-
trate the sample 250 times. However, using the RF-20AXS permits analysis by direct sample injection, without sample concentration.
Analysis of Anionic Surfactants by LCMS
Fig. 2 shows the mass chromatogram of alkylphenyl polyoxyethylene sulfate, a commonly used anionic surfactant. Fig. 3 shows its mass spectra. Using a mass
spectrometer as the detector permits simple separation and quantitation by m/z of impurities in samples and of isomers with different carbon numbers.
ColumnMobile phase
Flow rateColumn temp.Injection volumeDetectionCell temp.
: Shim-pack VP-ODS (250 mmL. × 4.6 mmI.D.): Water/Acetonitrile=35/65 containing 0.1 mol/L Sodium perchlorate: 1.0 mL/min: 40 °C: 20 µL: RF-20Axs (Ex. 221 nm, Em. 284 nm): 30 °C
[Analytical Conditions]
0 5 10 15 20 (min.)
1. C102. C113. C124. C135. C14
Peaks
1)
2)
22
Aldehyde Analysis System
Aldehyde Analysis by HPLC
System Characteristics
The partial revision of the Japanese Air Pollution Control Law displays a list of
chemical atmospheric contaminants. The list includes aldehydes, including
formaldehyde and acetaldehyde, as substances requiring priority action.
According to the revision to the Japanese Ordinance on Prevention of Hazards
due to Specified Chemical Substances, the interior environment of indoor
workplaces that manufacture or handle aldehydes must be measured every six
months.
A known method for measuring aldehydes in air is to derivatize the aldehydes
in the captured air sample with 2,4-dinitrophenylhydrazine (2,4-DNPH), and to
then analyze them by HPLC. Generally, this derivatization reaction is performed
at the time the air sample is captured. This is achieved by passing the air
through an absorbent presoaked in 2,4-DNPH.
This system analyzes the products of derivatization by 2,4-dinitrophenylhydrazine (2,4-DNPH) of aldehydes and ketones in indoor air or the ambient atmosphere.
Main Components
Detection PrincipleCarbonyl compounds, such as aldehydes and ketones,
react with 2,4-dinitrophenylhydrazine to form
dinitrophenylhydrazone.
These are detected through UV absorption at 360 nm.
Reaction of carbonyl compounds with 2,4-DNPH
O
CR1 R2
CR1 R2
NH2
H2O
NO2
NO2
H+
NH
N
NO2
NO2
NH
Carbonyl compound
2,4-dinitrophenylhydrazineDNPH derivative (hydrazone)
Prominence Aldehyde Analysis System
228-45012-XX
228-45002-XX
228-45018-XX
228-45093-93
228-45041-91
228-45007-XX
228-15652-92
228-45010-XX
228-45003-XX
228-40511-92
—
System Controller
Solvent Delivery Unit
Degassing Unit
Gradient Mixer
Reservoir Tray
Autosampler
1.5 mL Glass Vial
Column Oven
UV-VIS Detector
Analysis Column
LC Workstation
CBM-20A*1
LC-20AB
DGU-20A3R
Mixer 0.5-2.6 mL HP
SIL-20AC
CTO-20AC
SPD-20A
Shim-pack FC-ODS (75mm×4.6mmI.D.)
LabSolutions LC Single LC*2
1
1
1
1
1
1
1
1
1
1
1
*1:*2:
CBM-20Alite (228-45011-XX) can also be selected. Separate printer and cables required.
P/N Product Name QuantityModel
3 mg 20 mg 300 mg 2 g
Semi-micro Analytical Semi-preparative Preparative
0.001 0.01 0.1 1 10 100
10 mL/min
20 mL/min
23
Data
Analysis of Aldehydes in the Environment by HPLC
Related Document: HPLC Application Report No. 21 "Analysis of Aldehydes in the Environment by High-Performance Liquid Chromatography" (C190-E103)
Fig. 1 shows the construction of an air sampler containing DNPH solid-phase cartridges. An ozone scrubber is inserted in front of the DNPH
cartridges to prevent decomposition of the derivatives due to ozone. Atmospheric air is monitored by an accumulating flowmeter as it is
drawn in at a constant flow rate.
Derivatives are eluted from the cartridge by passing acetonitrile through the cartridge.
The captured and derivatized aldehydes and ketones are analyzed
by HPLC. Fig. 2 and Fig. 3 show the chromatograms measured by
isocratic elution for aldehyde standards and for aldehydes sampled
from the atmosphere, respectively. Fig. 4 and Fig. 5 show the
respective analyses by gradient elution. Satisfactory separation and
detection are achieved for aldehydes in atmospheric air. Fig. 1 Sampling of Aldehydes from Air Using DNPH Cartridges
Ozone ScrubberDNPH Cartridges
Pump IntegratingFlowmeter
[Analytical Conditions (Isocratic)]
ColumnMobile phase
Time program
Flow rateTemp.Detection
: Shim-pack FC-ODS (75 mmL. × 4.6 mmI.D.): A : Water / Tetrahydrofuran (8/2, v/v) B : Acetonitrile: B conc. = 20 % (0 min) → 60 % (14 min) → 20 % (14.01 -20 min): 1.2 mL/min: 40 °C: SPD-20A (365 nm)
ColumnMobile phaseFlow rateTemp.Detection
: Shim-pack FC-ODS (75 mmL. × 4.6 mmI.D.): Water / Acetonitrile (55/45, v/v): 1.0 mL/min: 40 °C: SPD-20A (360 nm)
[Analytical Conditions (Gradient)]
0 5 10(min.)
0 5 10 (min.) 0 5 10 (min.)
(C)
(D)
1. Formaldehyde2. Acetaldehyde3. Acetone
Peaks
Chromatogram of Aldehyde Standards
Analysis of Environmental Air (A) and Indoor Air (B)
Fig. 4 Chromatogram of 13 Aldehyde Standards Fig. 5 Analysis of Laboratory Air (C) and Procedural Blank (D)
FormaldehydeAcetaldehydeAcetoneAcroleinPropionaldehydeCrotonaldehyde2-butanoneMethacroleinn-butyraldehydeBenzaldehydeValeraldehydem-tolualdehydeHexaldehyde
Peaks1. Formaldehyde2. Acetaldehyde3. Acetone5. Propionaldehyde7. 2-butanone
Peaks
Fig. 2 Fig. 3
1.2.3.4.5.6.7.8.9.
10.11.12.13.
0 5 10(min.)
1. Formaldehyde2. Acetaldehyde
Peaks
Application Systems
24
Other Application Systems
Preparative HPLC SystemShimadzu preparative HPLC systems offer high-purity preparation, high-speed
preparation, and enhanced economy. Shimadzu has achieved a sales record of
over 2000 preparative HPLC systems around the world. Through application of
technologies and experience acquired through operations across a diverse
range of scales and fields, these systems have been developed to offer all the
functions demanded for preparative HPLC.
High-Pressure Gradient Analysis / Preparative System
Large-Scale Preparative System
Simple Semi-Preparative Recycle System
Bio-Chemical Analysis/Preparative System (Inert LC System)
Main Components (High-pressure gradient analysis / preparative system)
Main Components (Semi-preparative recycle system (manual injector))
*1:
*2:
Separate sample vials, sample racks, collection tubes, preparative racks, sample loops, etc. are also required.
Separate printer and cables required.
*3:
*4:
*5:
Separate sample vials, sample racks, collection tubes, preparative racks, sample loops, etc. are also required.
Connect to one detector such as the SPD-20A or the RID-10A differential refractive index detector.
Separate PC, printer and cables required.
QuantityModelColumn Scales and Product Range
Maximum load guideline (single injection, 25 cm-long column)
Flow rate mL/min
3 mg3 mg3 mg 20 mg20 mg 300 mg300 mg 2 g2 g20 mg 300 mg 2 g
Semi-microSemi-micro AnalyticalAnalytical Semi-preparativeSemi-preparative PreparativePreparativeSemi-micro Analytical Semi-preparative Preparative
2 mmI.D.
0.0010.001 0.010.01 0.10.1 1 1010 1001000.001 0.01 0.1 1 10 100
5 mmI.D. 20 mmI.D. 50 mmI.D.
LC-20AT
LC-6AD
LC-20AP
10 mL/min10 mL/min10 mL/min
20 mL/min20 mL/min20 mL/min
150 mL/min
LC-6AD Recycle Preparative System
LC-20AP Gradient Analysis / Preparative Switching System
228-45012-XX
228-45150-XX
228-20600-91
228-20601-91
228-45163-41
228-45041-91
228-45057-XX
228-32210-91
228-45079-91
228-45005-XX
228-34189-91
228-13000-95
228-45070-XX
228-24105-91
228-45116-91
—
System Controller
Solvent Delivery Unit
Gradient Mixer (preparative)
Gradient Mixer (analytical)
Reservoir Switching Valve
Reservoir Tray
Autosampler
Manual Injector
Column Holder
Photodiode Array Detector
Preparative Cell
Manual Column Switching Valve
Fraction Collector
Fraction Collector Head with FRC Valve
Large-Volume Kit for FRC
LC Workstation
CBM-20A
LC-20AP
Mixer 14 mL
Mixer 4.5 mL
FCV-230AL
SIL-10AP*1
Rheodyne7725 1
SPD-M20A
Preparative Flow Cell (0.5 mm)
FRC-10A*1
LabSolutions LC Multi LC-PDA*2
1
2
1
1
1
1
1
1
1
1
1
1
1
1
1
P/N Product Name QuantityModel
228-45012-XX
228-45068-XX
228-31103-91
228-28711-92
228-45041-91
228-45203-41
228-45060-91
228-45013-31
228-21217-95
228-32210-91
228-45003-XX
228-23405-91
228-45070-XX
228-24105-91
228-45192-91
System controller
Solvent delivery unit
Interface board
6AD recycle kit
Reservoir tray
Column holder
Optional box, VP
High-pressure flow line switching valve
Rotor Assy, 3-Port Valve
Manual injector
UV-VIS detector
Preparative cell
Fraction collector
Fraction collector head with valve
Software for Prominence Recycling Preparative HPLC Systems
CBM-20A
LC-6AD
PC-31L
Column holder, SLIM
FCV-20AH
Rheodyne7725*3
SPD-20A*4
Preparative cell with variable optical path length (0.5 mm)
FRC-10A*3
Recycle-Assist*5
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
P/N Product Name QuantityModel
25Application Systems
Main Components
*1:*2:*3:
CBM-20Alite (228-45011-XX) can also be selected. Select according to the measured molecular weight range. Separate printer and cables required.
*4:*5:
If no column oven is required, select the column holder (228-45079-91). Upchurch semi-preparative filter
GPC SystemMolecular weight distribution measurements by gel permeation
chromatography (GPC) are widely used to evaluate the properties of synthetic
polymers. The Prominence GPC system is designed specifically to provide
superior data reliability and ease of use.
3 mg 20 mg 300 mg 2 g
Semi-micro Analytical Semi-preparative Preparative
0.001 0.01 0.1 1 10 100
10 mL/min
20 mL/min
Prominence GPC System
Prominence GPC Clean-Up System
P/N Product Name QuantityModel
228-45012-XX
228-45000-XX
228-45018-XX
228-45041-91
228-45119-XX
228-48258-91
228-15652-92
228-45009-XX
228-45095-XX
—
—
223-05687-92
System Controller
Solvent Delivery Unit
Degassing Unit
Reservoir Tray
Autosampler
Vespel Needle Seal
1.5 mL Glass Vial
Column Oven
Refractive Index Detector
Analysis Column
LC Workstation
GPC Software
CBM-20A*1
LC-20AD
DGU-20A3R
SIL-20AHT
1.5 mL Glass Vial
CTO-20A
RID-10A
Shim-pack GPC Series*2
LCsolution Single*3
LCsolution GPC Software
1
1
1
1
1
1
1
1
1
—
1
1
Main Components
GPC Clean-Up SystemThis is a pretreatment system for GPC cleanup that conforms to the pesticide
test method in the Japanese Ministry of Health, Labour and Welfare
Ordinance. It effectively separates and automatically fractions pesticide
components from lipids and pigments in agricultural product extracts.
228-45051-31
228-45001-XX
228-45018-XX
228-45041-91
228-45057-XX
228-21280-92
228-45009-XX
228-45070-XX
228-24105-91
228-45116-91
228-45003-XX
228-23406-91
(406-762)
(406-763)
(A-330)
223-04500-31
—
System Controller
Solvent Delivery Unit
Degassing Unit
Reservoir Tray
Autosampler
15 mL Glass Reagent Vial (30 vials)
Column Oven*4
Fraction Collector
Fraction Collector Head with Valve
Large-Volume Kit
UV-VIS Detector
Preparative Cell
Preparative Column
Guard Column
Pre-Column Filter*5
Data Processor
Optical Fiber Cable (2 m)
SCL-10AVP
LC-20AT
DGU-20A3R
SIL-10AP
CTO-20A
FRC-10A
SPD-20A
Shodex CLNpak EV-2000 AC
Shodex CLNpak EV-G AC
C-R8A Chromatopac
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
P/N Product Name QuantityModel
(The system in the photograph includes the optional kit to handle round-bottomed recovery flasks.)
Prominence A
pplication Systems
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