GB/T 8381.3-2023Determination of lincosamides in feeds—Liquid chromatography-tandem mass spectrometry (English PDF)

Foreword

This document complies with the provisions of GB/T 1.1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents" Drafting.

This document replaces GB/T 8381.3-2005 "Determination of Lincomycin in Feed". Compared with GB/T 8381.3-2005, except for the structure In addition to adjustments and editorial changes, the main technical changes are as follows.

a) Changed the scope of application (see Chapter 1, Chapter 1 of the 2005 edition);

b) The principle has been changed (see Chapter 4, Chapter 4 of the 2005 edition);

c) Reagents or materials have been changed (see Chapter 5, Chapter 5 of the 2005 edition);

d) Changes in instruments and equipment (see Chapter 6, Chapter 6 of the 2005 edition);

e) The test procedures have been changed (see Chapter 8, Chapter 8 of the 2005 edition);

f) Test data processing has been changed (see Chapter 9, 10.2 of the 2005 edition).

1 Scope

This document describes the liquid chromatography-tandem mass spectrometry determination of lincomycin, clindamycin, clindamycin phosphate, and pirinomycin in feed. method.

This document applies to lincomycin, clindamycin, clindamycin in compound feeds, concentrated feeds, concentrate supplements and additive premixed feeds Determination of protein phosphate and pirinomycin.

The detection limit of this document is 10µg/kg and the limit of quantification is 40µg/kg.

2 Normative reference documents

The contents of the following documents constitute essential provisions of this document through normative references in the text. Among them, the dated quotations For undated referenced documents, only the version corresponding to that date applies to this document; for undated referenced documents, the latest version (including all amendments) applies to this document.

GB/T 6682 Specifications and test methods for water used in analytical laboratories

GB/T 20195 Preparation of animal feed samples

3 Terms and definitions

There are no terms or definitions to be defined in this document.

4 Principles

The test substance in the sample was extracted with methanol-phosphate buffer solution, purified by a mixed strong cation exchange solid-phase extraction cartridge, and liquid chromatography- Detected by tandem mass spectrometer and quantified by external standard method.

5 Reagents or materials

Unless otherwise specified, use only analytically pure reagents.

5.1 Water. GB/T 6682, Level 1.

5.2 Formic acid. chromatographically pure.

5.3 Methanol. chromatographically pure.

5.4 Acetonitrile. chromatographically pure.

5.5 Hydrochloric acid solution. Pipette 0.9mL hydrochloric acid, dilute to 100mL with water, and mix well.

5.6 Phosphate buffer solution (pH 8.0). Weigh 11.411g of dipotassium hydrogen phosphate trihydrate, add 430mL of water to dissolve, and use hydrochloric acid solution (5.5) Adjust pH to 8.0±0.1, dilute to 500mL with water, and mix well.

5.7 Methanol-phosphate buffer solution. Take 800mL of methanol (5.3), add.200mL of phosphate buffer solution (5.6), and mix well.

5.8 Formic acid solution I. Take 1mL of formic acid (5.2), dilute to 100mL with water, and mix well.