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
