GB/T 21317-2007 in English

《GB/T 21317-2007动物源性食品中四环素类兽药残留量检测方法 液相色谱-质谱/质谱法与高效液相色谱法》由424-caiq（中国检验检疫科学研究院）归口，主管部门为国家市场监督管理总局。
本标准系首次发布。
本标准规定了动物源性食品中四环素类兽药残留量检测的制样方法、高效液相色谱检测方法和液相色谱-质谱／质谱确证方法。
本标准适用于动物肌肉、内脏组织、水产品、牛奶等动物源性食品中二甲胺四环素、土霉素、四环素、去甲基金霉素、金霉素、甲烯土霉素、强力霉素7种四环素类兽药残留量的高效液相色谱测定和二甲胺四环素、差向土霉素、土霉素、差向四环素、四环素、去甲基金霉素、差向金霉素、金霉素、甲烯土霉素、强力霉素10种四环素类药物残留量的液相色谱�仓势祝�质谱测定。

1 Scope

This standard specifies the sample preparation method, the high-performance liquid chromatography (HPLC) method for testing and the liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) method for confirmation for the determination of tetracyclines residues in food of animal origin.

This standard is applicable to the determination of 7 tetracyclines residues, namely minocycline, oxytetracycline, tetracycline, demeclocycline, chlortetracycline, methacycline and doxycycline, by the HPLC method, and that of 10 tetracyclines residues, namely minocycline, 4-epioxytetracycline, oxytetracycline, 4-epitetracycline, tetracycline, demeclocycline, 4-epichlortetracyc-line, chlortetracycline, methacycline and doxycycline, by the LC-MS/MS method, in food of animal origin such as animal muscle and offal, aquatic products and milk.

2 Normative reference

The following normative documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated references, subsequent amendments to (excluding any corrigendum), or revisions of, any of these publications do not apply. However, parties to agreements based on this standard are encouraged to investigate the possibility of applying the latest editions of the standards indicated below. For undated references, the latest edition of the document referred to applies.

GB/T 6682 Water for analytical laboratory use - Specification and test methods (GB/T 6682-1992, neq ISO 3696:1987)

3 Principle

The residues of tetracycline antibiotics in the specimen are first extracted with 0.1mol/L Na2EDTA-Mcllvaine buffer solution (pH=4.0±0.05), and then filtered and centrifuged to obtain the supernatant which is purified by HLB solid phase extraction column, and determined by HPLC or liquid chromatography-electrospray-mass spectrometry (LC-ES-MS), and quantified by external standard peak area method.

1 Scope
2 Normative reference
3 Principle
4 Reagents and materials
5 Apparatus
6 Sample preparation and storage
7 Determination procedures
8 Blank test
9 Calculation and expression of results
10 Lower determination limit, recovery rate and precision
Annex A (Informative) Reference MS conditions
Annex B (Informative) Multi-reaction monitoring (MRM) chromatograms and liquid chromatograms
Annex C (Informative) Test data on recovery rate and precision of the methods