快速过滤净化-UPLC-MS/MS同时测定畜禽肉中12种兽药残留

Simultaneous Determination of 12 Veterinary Drugs in Livestock and Poultry Meat by Rapid Filter Purification Couple with Ultra Performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS)

采用功能化聚苯乙烯/苯聚合物为填料的快速过滤净化柱萃取畜禽肉中的兽药,再结合超高效液相色谱-串联质谱(UPLC-MS/MS)高通量分析,建立了一种可同时测定12种兽药残留的方法。通过正交试验设计筛选前处理的最佳条件,样品经pH 4.0的EDTA-Mcllvaine缓冲液提取,按压式固相过滤柱快速净化,UPLC-MS/MS检测,外标法定量。结果表明,12种兽药在较宽的线性范围内拟合良好,相关系数均大于0.99,方法检出限0.3~3μg/kg,定量限1.0~10μg/kg。在3个不同添加水平下,猪肉、鸡肉、牛肉样品中的回收率分别为82.8%~110.4%、80.2%~108.4%、75.8%~107.1%,RSDs为0.51%~10.23%。该方法用于市售猪肉中的兽药检测,其中恩诺沙星、环丙沙星、金霉素、土霉素、四环素和强力霉素被检测出,与国标方法的测定结果相一致。该方法简单、快速、准确,适合多种兽药残留的同步筛查和准确定量。

Based on a rapid filtration column with functional polystyrene/benzene polymer as filler,a method was developed for simultaneous determination of 12 kinds of veterinary drugs in livestock and poultry meat,combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).An orthogonal experimental design was used to determine the optimal conditions of sample pretreatment.The target analytes were extracted from the samples by EDTA-Mcllvaine buffer solution with pH 4.0,quickly purified by pressing solid phase filter column,analyzed by UPLC-MS/MS,and quantified by external standard method.The proposed method showed a good linear relationship with correlation coefficients(R 2)greater than 0.99.The limits of detection(LODs)and limits of quantitation(LOQs)of the method were ranged from 0.3 to 3μg/kg and from 1.0 to 10μg/kg.At three spiked levels,the recoveries of 12 kinds of veterinary drugs in pork,chicken and beef samples were 82.8%~110.4%,80.2%~108.4%,75.8%~107.1%,respectively,and relative standard deviations(RSDs)were between 0.51%~10.23%.The developed method was successfully applied to veterinary drugs analysis in pork samples,which were bought from local markets.Six compounds of enrofloxacin,ciprofloxacin,chlortetracycline,oxytetracycline,tetracycline and doxycycline were detected,and the detection values were consistent with National Standard method.The method was suitable for simultaneous screening and rapid quantification for veterinary drug residues with the advantages of easy accessibility,rapid detection and accuracy.