采用改进的 QuEChERS方法提取和净化鸡肉、鸡肝、猪肉、猪肝样品，建立了4类29种禁限用兽药残留的超高效液相色谱-串联质谱（ UPLC-MS／MS）检测方法。样品采用 McIlvaine缓冲液-乙腈提取，提取液酸化、盐析后取乙腈相，用十八烷基硅烷（C18）和氨基（NH2）吸附剂分散固相萃取净化，最后用电喷雾串联质谱仪在正离子多反应监测扫描（ MRM）模式下进行测定，基质外标法定量。解决了四环素类兽药难与其他类兽药同时检测的难题。29种兽药在各自的浓度范围内，浓度与峰面积线性关系良好，相关系数不小于0.993。在29种兽药的定量限（ LOQ）水平、20μg／kg和50μg／kg 3个添加水平下进行加标回收率试验，29种兽药的平均回收率在71.5％和93.2％之间，相对标准偏差在0.8％和7.7％之间。29种兽药的检出限为0.3~3.0μg／kg，金刚烷胺的定量限为1.0μg／kg，四环素类兽药的定量限为10.0μg／kg，其他兽药的定量限均为5.0μg／kg。该方法操作简便，净化效果好，灵敏度、准确度和精密度均符合多残留检测技术的要求，可为食品检验机构对动物组织中禁限用兽药残留的日常监控提供更方便、快捷的检测方法支持。
An ultra performance liquid chromatography-tandem mass spectrometric method, with modified QuEChERS method for sample preparation,was developed for the determination of the 4 kinds of 29 banned and restricted veterinary drugs in chicken muscle,chicken liver, porcine muscle and porcine liver samples. The drugs were extracted with McIlvaine buffer solu-tion and acetonitrile,then cleaned-up by modified QuEChERS method,and finally analyzed by ultra performance liquid chromatography-tandem mass spectrometry in multiple reaction moni-toring mode via positive electrospray ionization. The method was validated at three fortification levels( LOQ level,20 μg/kg and 50 μg/kg)in chicken muscle,chicken liver,porcine muscle and porcine liver samples. The validation results were as follows. The correlation coefficients of the standard calibration curves for the 29 veterinary drugs were all between 0. 993 and 0. 999 over their own concentration ranges. The average recoveries of the 29 drugs were between 71. 5% and 93. 2%,with the relative standard deviations( RSDs)between 0. 8% and 7. 7%. The limits of determination( S/N=3)of the drugs were between 0. 3 and 3. 0 μg/kg. The limits of quantification( S/N≥10 ) were 1. 0 μg/kg for amantadine,10. 0 μg/kg for the tetracycline drugs,and 5. 0 μg/kg for all the other drugs. It was indicated that the method developed is easy,sensitive,and has a good purification effect. The sensitivity,accuracy and precision of the method were all acceptable,and it can meet the requirements of the multiple residue analy-sis. So,this method can be further applied to investigate the veterinary drug residues in animal derived foods.
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