C190-E145A Prominence Application Systems · Prominence Application Systems. ... Reaction Coil...

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


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


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.


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)


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


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



20AB Automatic Rinsing Kit

20AD Automatic Rinsing Kit

Degassing Unit

Gradient Mixer

Reservoir Tray

Autosampler

1.5 mL Glass Vial

Column Oven


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


1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1


This is a cation-exchange column. A ligand exchange column or normal-phase column may also be used.


+

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


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


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


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)


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


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.


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


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




Degassing Unit

Gradient Mixer

Reservoir Tray

Autosampler

1.5 mL Glass Vial

Column Oven


Outlet Unit


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.)


1

1

2

1

1

1

1

1

1

1

1

1

1

1

1

1

1

Prominence Carbamate Analysis System

*1:

*2:

*3:


Upchurch semi-prep filter (Use to analyze residual pesticides in foods.)


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


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)


2-

100Methylamine

<Separation>ColumnMobile phaseTime program


: 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


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


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.


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


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



Degassing Unit

Reservoir Tray

Autosampler

1 mL PP Vial

Column Oven


Outlet Unit


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.)


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


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


: 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


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


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



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


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


LabSolutions LC Multi LC-PDA*2

1

1

1

1

1

1

1

1

1

1

1

Main Components

Main Components


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



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


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




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


*: Separate printer and cables required.

1.2.3.4.5.6.7.8.9.

10.11.12.

11


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)


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


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


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



Degassing Unit

Reservoir Tray

Autosampler

Sample Loop 500 µL PEEK

Sample Cooler L

4 mL PP Vial

Column Oven

UV-VIS Detector

Outlet Unit


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.


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)


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


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 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


Degassing Unit

Reservoir Tray

Autosampler

1.5 mL Glass Vial

Column Oven


Analysis Column

LC Workstation

CBM-20A*1

LC-20AD

DGU-20A3R

SIL-20AC

CTO-20AC

RF-20AXS*2



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


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




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


0 5 10 15 20 (min.)

1. C102. C113. C124. C135. C14

Peaks

1)

2)

22

Aldehyde Analysis System

Aldehyde Analysis by HPLC


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


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.)


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.


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.


*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


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


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



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


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


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


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


(The system in the photograph includes the optional kit to handle round-bottomed recovery flasks.)

Prominence A

pplication Systems

Company names, product/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its affiliates, whether or not they are used with trademark symbol “TM” or “®”.Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own.

For Research Use Only. Not for use in diagnostic procedures. The contents of this publication are provided to you “as is” without warranty of any kind, and are subject to change without notice. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication.

© Shimadzu Corporation, 2013www.shimadzu.com/an/Printed in Japan 3655-10311-30ANS

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