超高效液相色谱-串联质谱法测定动物源食品中7种药物残留

Determination of Seven Drugs in Animal Origin Food by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

关键词:  头孢类  大环内酯类  残留  液质联用

Key words:  cephalosporin  macrolide  residues  UPLC-MS/MS

摘要:

建立了猪肉、鸡肉、鸡蛋中阿奇霉素、克林霉素、罗红霉素、头孢氨苄、头孢匹林、头孢噻肟、头孢拉定7种药物残留的液相色谱-串联质谱法。采用乙腈∶水=15∶2的溶液作为提取液，经正己烷净化，UPLC-MS/MS测定。结果表明：以上七种药物在2～100 μg/L范围内线性关系较好，相关系数r均在0.998以上。在猪肉、鸡肉和鸡蛋组织中阿奇霉素、克林霉素、罗红霉素的检测限为0.5 μg/kg，定量限为1 μg/kg，头孢氨苄、头孢匹林、头孢噻肟、头孢拉定检测限为2 μg/kg，定量限为4 μg/kg。在4、8、20 μg/kg的添加浓度上进行回收率试验，阿奇霉素、克林霉素、罗红霉素回收率在80%～100%之间，头孢氨苄、头孢匹林、头孢噻肟、头孢拉定回收率在70%～90%之间。本方法批内相对标准偏差≤20%，批间相对标准偏差≤20%。

Abstract:

A method based on ulra performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was developed for determination of seven drugs in pork，chicken and egg. The analytes were extracted with acetonitrile-water(V/V,15∶2)，and were cleaned up by hexane.Quantification of the analytes was achieved by UPLC-MS/MS with multiple reaction monitoring (MRM) using external standard method. The results indicated that the calibration curves were good linear between the peak areas and concentrations of 7 drugs in the range of 2～100 μg/L, with correlation coefficients more than 0.998.The limits of detection and limits of quantification of azithromycin, clindamycin, roxithromycin in pork, chicken and egg tissue were 0.5 μg/kg and 1 μg/kg, the limits of detection and limits of quantification of cefalexin，cephapiriin，cefotaxime，cefradine in pork, chicken and egg tissue were 2 μg/kg and 4 μg/kg, respectively.The average recoveries of azithromycin，clindamycin，roxithromycin at three concentration levels of 4 μg/kg，8 μg/kg and 20 μg/kg ranged from 80% to 100%,and the average recoveries of cefalexin，cephapiriin，cefotaxime，cefradineranged ranged from 70% to 90%.The intra-and inter-RSDs were less than 20%.