GB/T 22260-2023Determination of anabolic steroids 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 22260-2008 "Determination of methyltestosterone in feed by high performance liquid chromatography tandem mass spectrometry" and is consistent with Compared with GB/T 22260-2008, in addition to structural adjustments and editorial changes, the main technical changes are as follows.

a) Increased detection limit (see Chapter 1);

b) The principle has been changed (see Chapter 4, Chapter 3 of the 2008 edition);

c) Changed the extraction and purification of the sample (see 8.1, 8.2, 7.1, 7.2 of the 2008 edition);

d) The reference conditions for liquid chromatography and mass spectrometry have been changed (see 8.3.1 and 8.3.2, 7.3.1 and 7.3.2 of the 2008 edition);

e) Changed the qualitative and quantitative requirements for liquid chromatography-tandem mass spectrometry (see 8.3.4 and 8.3.5, 7.3.3 of the 2008 edition);

f) Changed the test data processing (see Chapter 9, 8.1 of the 2008 edition);

g) Changed precision (see Chapter 10, Chapter 9 of the 2008 edition).

1 Scope

This document describes a method for the liquid chromatography-tandem mass spectrometry determination of protein anabolic hormones in feed.

This document is applicable to testosterone, methane and alpha in compound feeds, concentrated feeds, concentrate supplements, additive premixed feeds and mixed feed additives.

Basetestosterone, Boldirone, Meandrosterone, Androstenedione, Dehydroepiandrosterone, Nandrolone, Nandrolone Propionate, Stanozolol, Melengestrol Acetate, Progesterone Determination.

The detection limit of methyltestosterone, stanozolol and melengestrol acetate in this document is 0.005mg/kg, and the detection limit of testosterone, bodiron, mestandrostenone and androstene is 0.005mg/kg.

The detection limit of diketone, dehydroepiandrosterone, nandrolone, nandrolone propionate, and progesterone is 0.02 mg/kg; methyltestosterone, stanozolol, and melengestrol acetate The limit of quantification for ketones is 0.01mg/kg, and the determination of testosterone, bodiron, meandrosterone, androstenedione, dehydroepiandrosterone, nandrolone, nandrolone propionate, and progesterone. The amount limit is 0.05mg/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 protein anabolic hormones in the sample were extracted with acetonitrile, purified by the adsorbent, and then detected with a liquid chromatography-tandem mass spectrometer using the internal standard method. Quantitative.

5 Reagents or materials

5.1 Water. GB/T 6682, Level 1.

5.2 Acetonitrile. chromatographically pure.

5.3 Formic acid. chromatographically pure.

5.4 50% acetonitrile solution. Take 50mL of acetonitrile (5.2), add water to dilute to 100mL, and mix well.

5.5 0.01% formic acid solution. Take 100µL of formic acid (5.3), add water to dilute to 1000mL, and mix well.

5.6 Standard stock solution (1mg/mL). Accurately weigh testosterone, methyltestosterone, bodiron, mestandrosterone, androstenedione, dehydroepiandrosterone, nodrol 0.01g each of nandrolone propionate, stanozolol, melengestrol acetate, and progesterone (accurate to 0.00001g) were placed in a 10mL brown container.