超高效液相色谱-串联质谱法测定鸡肉中的4种聚醚类抗球虫药物残留  

Simultaneous determination of four polyethers coccidiostats in chicken muscles using ultra performance liquid chromatography tandem mass spectrometry

作　　者：毕言锋[1] 徐倩[1] 王树槐[1] 汪霞[1] 

机构地区：[1]中国兽医药品监察所,国家兽药残留基准实验室,北京100081

出　　处：《分析试验室》2009年第7期17-21,共5页Chinese Journal of Analysis Laboratory

基　　金："十一五"国家科技支撑计划"新兽药筛选与安全评价技术研究"(2006BAD31B09)项目资助

摘　　要：采用乙腈直接提取、石墨化碳黑固相萃取小柱净化、UPLC快速分离，串联质谱检测、成功建立了鸡肉中莫能菌素、马杜菌素、盐霉素、拉沙洛西等4种抗球虫药物的多残留检测方法。对样品提取、净化过程和仪器条件进行了优化改进，经Waters C18 column分离、正离子电喷雾电离模式测定，4种药物的检测限为0．2gg／kg，最低定量限为0．5μg／kg。选取0．5、1．0、2．0μg／kg3个质量分数进行空白添加回收率实验，回收率为71．9％～100．9％，批内RSD2．7％～15％，批间RSD为1．7％～10％。各项技术指标满足国内外法规的要求，适合大量样品中聚醚类抗球虫药物残留的确认检测。A method for the simultaneous analysis of four polyethers coccidiostats in chicken muscles was developed by ultra performance liquid chromatography-tandem mass spectrometry. The residues from chicken muscles were extracted with acetonitrile, and the extracting solutions were purified using supelclean ENVI-Carb SPE cartridges. The four residues were separated on a Waters ACQUITY UPLC^TM BEH C18 column, and detected by MS/MS with positive electrospray ionization mode. The limits of detection （LOD） for the four drugs were 0.2 μg/kg, and the limits of quantification （LOQ） were 0.5 μg/kg. At three spiking levels of 0.5, 1.0, 2.0 g/kg, average recoveries were between 71.9% and 100.9 %. Coefficients of variation for intrassay were between 2.7 % and 15 %, and coefficient of variations for interassay were between 1.7 % and 10%. The experiment results showed that the method was simple, rapid and was applicable to simultaneous confirmation of multi-residues of four polyethers coccidiostats in chicken muscles.

关 键 词：超高效液相色谱-串联四极杆质谱 聚醚类抗球虫药物 鸡肉 

分 类 号：O657.63[理学—分析化学]