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2~100μg/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0.5μg/kg,定量限为1μg/kg,头孢氨苄、头孢匹林、头孢噻肟、头孢拉定检测限为2μg/kg,定量限为4μg/kg。在4、8、20μg/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%。
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%.
出处
《中国兽药杂志》
2014年第8期51-54,共4页
Chinese Journal of Veterinary Drug