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GB/T 22955-2008Determination of benzimidazoles residues in fugu, eel and baked eel - LC-MS-MS method (English PDF)

河豚鱼、鳗鱼和烤鳗中苯并咪唑类药物残留量的测定 液相色谱-串联质谱法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

December 31, 2008

Implementation date

May 1, 2009

Scope

GB/T 22955-2008 is the English-translated version of 河豚鱼、鳗鱼和烤鳗中苯并咪唑类药物残留量的测定 液相色谱-串联质谱法.

GB/T 22955-2008 prescribes a liquid chromatography-tandem mass spectrometry method for determining residues of benzimidazole drugs and their metabolites in puffer fish, eel and baked eel.

Clause 1 confines the method to those three matrices and names sixteen analytes, among them oxfendazole and fenbendazole with the metabolite oxfendazole sulfone, albendazole with albendazole 2-amino sulfone, albendazole sulfoxide and albendazole sulfone, mebendazole with amino mebendazole and hydroxy mebendazole, flubendazole with 2-amino flubendazole, and thiabendazole with 5-hydroxy thiabendazole and thiabendazole ester; the method detection limit is 0.010 mg/kg for every one of them.

Clause 3 sets out the principle: the sample is extracted with ethyl acetate under basic conditions, centrifuged and concentrated, the residue is dissolved in acetonitrile and 0.1 mol/L hydrochloric acid and defatted with n-hexane, the solution is cleaned up on an MCX solid phase extraction cartridge, and the test solution is then run on the liquid chromatograph-tandem mass spectrometer with quantification by external standard peak area.

Clause 4 lists the reagents and materials, including ethyl acetate, n-hexane, chromatographic-grade methanol and acetonitrile, anhydrous sodium sulfate ignited at 650 degrees C for four hours and kept in a desiccator, 2,6-di-tert-butyl-p-cresol and hydrochloric acid.

Reagents are analytical grade unless stated otherwise and the water meets GB/T 6682, while GB/T 6379.1 and GB/T 6379.2 are cited for the accuracy, trueness and precision of measurement methods.

Appendix A and Appendix B are both informative. The standard was proposed and is administered by the national quality supervision authority, and was drafted by the Qinhuangdao and Guangdong Entry-Exit Inspection and Quarantine Bureaus. It was issued on December 31, 2008 and has applied since May 1, 2009.

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Document preview — GB/T 22955-2008

National Standard of the People's Republic of China

ICS
67.050
Classification
X 04

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Foreword
  • 1 Scope
  • 2 Normative references
  • 3 Principle
  • 4 Reagents and materials

Foreword

The Standard Appendix A, Appendix B is an informative annex.

1 Scope

This standard specifies the puffer fish, eels and eel in the benzimidazole drug and metabolite residues in liquid chromatography - tandem mass spectrometry method.

This standard applies to liquid chromatography - tandem mass spectrometry puffer fish, eels and eel in oxfendazole, fenbendazole and their metabolites Was oxfendazole sulfone, albendazole and metabolites of albendazole 2-amino-sulfone, albendazole sulfoxide, albendazole sulfone, mebendazole and their representatives

Metabolite amino mebendazole, hydroxy mebendazole, flubendazole and its metabolites 2-flubendazole, thiabendazole and its metabolite 5-hydroxy Thiabendazole, thiabendazole ester, oxybenzone of residues oxazole.

The standard method detection limit. oxfendazole, fenbendazole, oxfendazole sulfone, albendazole, albendazole 2-amino-sulfone, albendazole Sulfoxide, albendazole sulphoxide, mebendazole, amino mebendazole, hydroxy mebendazole, flubendazole, 2-amino flubendazole, thiabendazole, serotonin Yl thiabendazole, thiabendazole ester, oxybenzone of azole are 0.010mg/kg.

2 Normative references

The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.

GB/T 6379.1 measurement methods and results of Accuracy (trueness and precision) - Part 1: General principles and definitions (GB/T 6379.1-2004, ISO 5725-1:1994, IDT)

GB/T 6379.2 measurement methods and results of Accuracy (trueness and precision) - Part 2: Determine the standard measurement method to repeat Of the basic methods of reproduction (GB/T 6379.2-2004, ISO 5725-2:1994, IDT)

GB/T 6682 analytical laboratory use specifications and test methods (GB/T 6682-2008, ISO 3696. 1987, MOD)

3 Principle

Specimen under basic conditions extracted with ethyl acetate, centrifugation, and concentrated, and the residue with acetonitrile -0.1mol L hydrochloric acid solution/dissolution, n-hexane Skimmed by MCX solid phase extraction cartridge. Sample solution for chromatography - tandem mass spectrometer, external standard peak area quantification.

4 Reagents and materials

Unless otherwise indicated, the reagents used were of analytical grade water as a water GB/T 6682 regulations.

4.1 Ethyl acetate.

4.2 n-hexane.

4.3 Methanol. chromatographically pure.

4.4 Acetonitrile. chromatography.

4.5 Anhydrous sodium sulfate. After 650 °C burning 4h, placed in the dryer set aside.

4.6 2,6-di-tert-butyl-p-cresol (BHT).

4.7 Hydrochloric acid.

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

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