动物源食品中酰胺醇类药物及其代谢物残留检测超高效液相色谱-串联质谱法研究

Determination of Amphenicols and Metabolite Residues in Animal Derived Food by UPLC-MS/MS

关键词:  动物源食品  酰胺醇类药物  代谢物  残留  超高效液相色谱-串联质谱

Key words:  animal derived food  amphenicols  metabolite  residue  UPLC-MS/MS

摘要:

建立了动物源食品中酰胺醇类药物（氯霉素CAP、甲砜霉素TAP、氟苯尼考FF）及其代谢物（氟苯尼考胺FFA）残留检测的超高效液相色谱-串联质谱（UPLC-MS/MS）法。样品经氨化乙酸乙酯提取，正己烷脱脂，氨化乙酸乙酯反萃取，电喷雾正/负离子多反应监测（MRM）模式检测。四种药物在0.2~50 μg/L的系列浓度范围呈线性相关，样品中CAP的检测限为0.1 μg/kg，定量限为0.2 μg/kg；TAP、FF、FFA检测限为0.5 μg/kg，定量限为1.0 μg/kg。在0.2~5 μg/kg的添加浓度范围内平均回收均为80%~120%，变异系数均小于15%。结果表明该方法简单快速、灵敏度高、重复性好，适用于动物源食品中酰胺醇类及其代谢物残留检测。

Abstract:

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the determination of amphenicols(CAP, TAP, FF) and metabolite(FFA) residues in animal derived food.The samples were extracted by ammoniated ethyl acetate.The fat was removed by hexane. The solution after defatting were extracted by ammoniated ethyl acetate again.The 4 drugs were detected by electrospray ionization in the positive /negative ion multiple reaction mode. The calibration curves of the 4 drugs were linear over the concentration ranges of 0.2~50 μg/L.The limit of detection of CAP was 0.1 μg/kg,and the limit of quantification was 0.2 μg/kg. The limits of detection of TAP,FF and FFA were 0.5 μg/kg,and the limits of quantification were 1 μg/kg. The control samples were spiked in 0.2~5 μg/kg，and the average recoveries ranged from 70% to 120%. The coefficient of variation was less than 15%. This method can be applied for the determination of amphenicols and metabolite residues in animal derived food.