GB/T 21312-2007 in English

《GB/T 21312-2007动物源性食品中14种喹诺酮药物残留检测方法 液相色谱-质谱/质谱法》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。
本标准规定了动物源性食品中14种喹诺酮药物残留量检测的制样方法和高效液相色谱-质谱/质谱检测方法。本标准适用于猪肉、猪肝、猪肾、牛奶、鸡蛋等动物源性食品中恩诺沙星、诺氟沙星、培氟沙星、环丙沙星、氧氟沙星、沙拉沙星、依诺沙星、洛美沙星、吡哌酸、萘啶酸、奥索利酸、氟甲喹、西诺沙星、单诺沙星14种喹诺酮类兽药残留量的液相色谱-质谱/质谱法测定和确证。

1 Scope

This standard specifies the sample preparation method and high performance liquid chromatography tandem mass spectrometry method for analysis of fourteen quinolones in food of animal origin.

This standard is applicable to the determination and confirmation for analysis of fourteen quinolones (enrofloxacin, norfloxacin, pefloxacin, ciprofloxacin, ofloxacin, sarafloxacin, enoxacin, lomefloxacin, pipemidic acid, nalidixic acid, oxolinic acid, flumequine, cinoxacin, danofloxacin) in food of animal origin (e.g., pork, pig liver, pig kidney, milk and eggs) by high performance liquid chromatography tandem mass spectrometry.

2 Normative references

The following normative documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated reference, subsequent amendments (excluding corrections) to, 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 most recent editions of the standards indicated below. For undated references, the latest edition applies.

GB/T 6682 Water for analytical laboratory use—Specification and test methods (GB/T6682-1992, neq ISO 3696: 1987)

3 Method summary

The quinolone antibiotics in the samples are extracted with 0.1mol/L EDTA-Mcllvaine buffer solution (pH4.0). After filtration and centrifugation, the supernatant is purified by HLB solid phase extraction column. It is determined by high performance liquid chromatography tandem mass spectrometry and quantified by negative sample matrix plus external standard method.

1 Scope
2 Normative references
3 Method summary
4 Sample preparation method
5 Reagents and materials
6 Apparatus
7 Extraction and purification
8 Determination of high performance liquid chromatography tandem mass spectrometry
9 Blank test
10 Calculation and expression of results
11 Detection limit, quantitation limit and recovery rate
Annex A (Informative) Reference mass spectrometry conditions
Annex B (Informative) Reference liquid phase conditions
Annex C (Informative) Daughter ion scanning mass spectrum of 14 quinolones
Annex D (Informative) Chromatograms for standard solutions of 14 quinolones
Annex E (Informative) Recovery rate and relative standard deviations of 14 quinolones in five matrices