National food safety standard - Determination of 331 pesticides and their metabolite residues in plant-derived foods. Liquid chromatography-mass spectrometry
GB 23200.121-2021 National food safety standard - Determination of 331 pesticides and metabolites residues in foods of plant origin - Liquid chromatography-tandem mass spectrometry method
1 Scope
This document specifies the liquid chromatography-tandem mass spectrometry method for determination of 331 pesticides and metabolites (see Annex A) residues in foods of plant origin.
This document is applicable to determination of 331 pesticides and metabolites residues in foods of plant origin.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB 2763-2021 National food safety standard - Maximum residue limits for pesticides in food
GB/T 6682 Water for analytical laboratory use - Specification and test methods
3 Principle
The specimen is extracted with acetonitrile, and the extract is purified by dispersive solid-phase extraction, then determined by liquid chromatography-tandem mass spectrometer and quantified by the external standard method.
4 Reagents and materials
Unless otherwise specified, analytically pure reagents, and Class-I water as defined in GB/T 6682, are used for the purpose of this method.
4.1 Reagents
4.1.1 Acetonitrile (CH3CN, CAS No.: 75-05-8).
4.1.2 Acetonitrile (CH3CN, CAS No.: 75-05-8): chromatographically pure.
4.1.3 Methyl alcohol (CH3OH, CAS No.: 67-56-1): chromatographically pure.
4.1.4 Sodium chloride (NaCl, CAS No.: 7647-14-5).
4.1.5 Sodium acetate (CH3COONa, CAS No.: 127-09-3).
4.1.6 Acetic acid (CH3COOH, CAS No.: 64-19-7).
4.1.7 Anhydrous magnesium sulfate (MgSO4, CAS No.:7487-88-9).
4.1.8 Sodium citrate dihydrate (C6H5Na3O7• 2H2O, CAS No.: 6132-04-3).
4.1.9 Disodium hydrogen citrate sesquihydrate (C6H6Na2O7•1.5H2O, CAS No.: 6132-05-4).
4.1.10 Formic acid (HCOOH, CAS No.: 64-18-6): chromatographically pure.
4.1.11 Ammonium formate (HCOONH4, CAS No.:540-69-2).
4.2 Preparation of solutions
4.2.1 Acetonitrile-acetic acid solution (99+1, volume ratio): Measure 10 mL of acetic acid, add it to 990 mL of acetonitrile, and mix well.
4.2.2 Ammonium formate-formic acid aqueous solution (2 mmol/L): Weigh 0.1261 g of ammonium formate, dissolve it in a 0.01% formic acid aqueous solution, dilute to 1,000 mL, and shake well.
4.2.3 Ammonium formate-formic acid methanol solution (2 mmol/L): Weigh 0.1261 g of ammonium formate, dissolve it in a 0.01% formic acid methanol solution, dilute to 1,000 mL, and shake well.
4.3 Standards
Contents
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Apparatus
6 Preparation of specimens
7 Analytical procedures
8 Calculation of results
9 Precision
10 Miscellaneous
Annex A (Informative) Chinese and English names of 331 pesticides and their metabolites and method quantification limits in various matrices
Annex B (Informative) Comparative index of English and Chinese names of 331 pesticides and their metabolites
Annex C (Informative) Retention time, parent ion, daughter ion and ion pair mass spectrometry parameters of 331 pesticides and their metabolites
Annex D (Informative) Mass chromatograms of 331 pesticides and their metabolites under multiple reaction monitoring (MRM)
Annex E (Informative) Representation and calculation of precision
