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GB/T 18932.19-2003Method for the determination of chloramphenicol residues in honey -- LC-MS-MS method (English PDF)

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Issued by

General Administration of Quality Supervision, Inspection and Quarantine of the People’s Republic of China

Level / Type

National · Recommended

Issue date

December 26, 2003

Implementation date

June 1, 2004

Scope

GB/T 18932.19-2003 (Method for the determination of chloramphenicol residues in honey -- LC-MS-MS method) is available as an English-translated PDF.

GB/T 18932.19-2003 — This Part of GB/T 18932 specifies the method for the determination of chloramphenicol residues in honey - LC-MS-MS method. This Part is applicable to the determination of chloramphenicol residues in honey. The method detection limit of this Part. chloramphenicol is 0.10 µg/kg.

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Document preview — GB/T 18932.19-2003

National Standard of the People's Republic of China

ICS: 67.180.10
Classification: X 31

Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People’s Republic of China

Foreword...3
1 Scope...4
2 Normative References...4
3 Principles...4
4 Reagents & Materials...5
5 Instruments...5
6 Sample preparation and storage...6
7 Determination steps...6
8 Calculation of results...8
9 Precision...9

Foreword

This Part of GB/T18932 is modified on the basis of adopting the Canadian

Standard ACC-062-V1.0 "Method for the determination of chloramphenicol

residues in honey - LC-MS method". The main modified contents are as follows.

- Purification column is modified from C18 solid phase extraction column to

Oasis HLB solid phase extraction column;

- Eluent is modified from acetonitrile + water (3+7) to ethyl acetate;

- Single quadrupole mass-spectrometry detector is modified to tandem

quadrupole mass-spectrometry detector;

- Internal standard method is modified to the external standard method.

Appendix A and Appendix B of this Part are informative.

This Part was proposed by Qinhuangdao Entry - Exit Inspection and Quarantine

Bureau of the People's Republic of China.

This Part shall be under the jurisdiction of National Federation of Supply and

Marketing Cooperatives.

The drafting organization of this Part. Qinhuangdao Entry - Exit Inspection and

Quarantine Bureau of the People's Republic of China.

Main drafters of this Part. Pang Guofang, Cao Yanzhong, Zhang Jinjie, Jia

Guangqun, Fan Chunlin, Li Xuemin, Liu Yongming and Shi Yuqiu.

This Part was issued for the first time.

Method for the determination of chloramphenicol

residues in honey - LC-MS-MS method

1 Scope

This Part of GB/T 18932 specifies the method for the determination of

chloramphenicol residues in honey - LC-MS-MS method.

This Part is applicable to the determination of chloramphenicol residues in

honey.

The method detection limit of this Part. chloramphenicol is 0.10 µg/kg.

2 Normative References

The following standards contain the provisions which, through reference in this

Part of the GB/T18932, constitute the provisions of this Part. For dated

references, all subsequent amendments (excluding corrections) or revisions do

not apply to this Part. However, the parties who enter into agreement based on

this Part are encouraged to investigate whether the latest versions of these

standards are applicable. For undated reference documents, the latest versions

apply to this Part.

GB/T 6379 Precision of test methods - Determination of repeatability and

reproducibility for a standard test method by inter-laboratory tests (GB/T

6379-1986,neq IS05725.1981)

3 Principles

Use ethyl acetate to extract the sample. After the extract is concentrated,

dissolve it in water.

4 Reagents & Materials

4.1 Water. Grade-1 water specified by GB/T 6682.

4.2 Methanol. chromatographic pure.

4.3 Acetonitrile. chromatographic pure.

4.4 Ethyl acetate. chromatographic pure.

4.5 Acetonitrile + water (1+7). measure 20 mL of acetonitrile and mix it with 140

mL of water.

4.7 Chloramphenicol reference material. purity >= 99%.

4.8 Chloramphenicol standard stock solution. 0.1 mg/mL. Accurately weigh an

adequate amount of chloramphenicol reference material (4.7), and use

methanol to make 0.1 mg/mL standard stock solution. Store the stock solution

in the refrigerator at 4°C; it shall be used for two months.

5 Instruments

5.1 Liquid chromatography - tandem quadrupole mass spectrometer. equipped

with electrospray ionization source.

5.2 Analytical balances. 2 balances of which the sensitivity is 0.1 mg and 0.01

g respectively.

5.3 Automatic concentrator or equivalent.

5.4 Nitrogen blowing instrument.

5.10 Centrifuge.

5.11 Graduated centrifuge tube. 10 mL, the accuracy is 0.1 mL.

5.12 Pipette. 10 mL.

5.13 Centrifuge tube. 50 mL with stopper.

6 Sample preparation and storage

6.1 Sample preparation

Evenly stir the non-crystallized laboratory sample. For crystallized sample, in a

enclosed circumstance, place it in the water bath at not more than 60°C; warm

it; oscillate it till it is totally melted;

6.2 Sample storage

Store the sample at room temperature.

7 Determination steps

7.1 Extraction

Weigh 5 g of sample, accurate to 0.01 g. Place it into a 50 mL stoppered

centrifuge tube; add 5 mL of water. Quickly mix it in the liquid mixer for 1 min till

it is completely dissolved.

7.2 Purification

Pour the extract (7.1) into a liquid reservoir that is connected to Oasis HLB

column (4.6) in the lower. The solution flows through the Oasis HLB solid phase

extraction column at the flow rate <= 3 mL/min.

7.3 Determination

7.3.1 Liquid chromatography conditions

7.3.2 Mass-spectrometry conditions

321/194 -20

7.3.3 LC-MS-MS determination

Respectively inject the chloramphenicol standard working solutions (4.9) under

LC-MS-MS conditions. Take the peak area as ordinates, and take working

solution concentration (ng/mL) as abscissa; draw the seven-point standard

working curve.

7.4 Parallel test

Follow the previous steps to carry out the parallel test for the same sample.

7.5 Blank test

Follow the previous steps, except weighing the sample.

8 Calculation of results

The result is calculated according to equation (1).

9 Precision

The precision data in this Part is determined in accordance with the provisions

of GB/T 6379.The repeatability and reproducibility values are calculated in 95%

confidence.

9.1 Repeatability

Under conditions of repeatability, the content of chloramphenicol in honey is

between 0.19g/kg~4.0µg/kg. The absolute difference between two independent

test results obtained shall not exceed the repeatability limit (r). The repeatability

limit of this Part is calculated according to equation (2).

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 9 pages — is available in the English PDF.

Referenced standards

Normative references

GB/T18932 · GB/T 6379

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