超高效液相色谱-串联质谱法同时测定鸡肉中的二氯二甲吡啶酚、磺胺类和喹诺酮类药物残留  

Simultaneous determination of clopidol,sulfonamide and quinolone residues in chickens byultra performance liquid chromatography-tandem mass spectrometry

作　　者：宋伟[1] 胡艳云 韩芳 吕亚宁 郑屏 周芳芳[3] 陈晓妹[1] 邱静 周晓莹 

机构地区：[1]安徽出入境检验检疫局技术中心,安徽合肥230022 [2]食品安全分析与检测安徽省重点实验室,安徽合肥230022 [3]安徽农业大学茶与食品科技学院,安徽合肥230022

出　　处：《色谱》2013年第12期1161-1166,共6页Chinese Journal of Chromatography

基　　金：安徽省科技攻关项目(12010402c205)

摘　　要：采用超高效液相色谱-串联质谱（UPLC-MS/MS）在正离子模式下通过多反应监测（MRM）方式同时测定了鸡肉组织中二氯二甲吡啶酚、磺胺嘧啶、磺胺二甲基嘧啶、磺胺对甲氧嘧啶、磺胺甲氧哒嗪、诺氟沙星、氧氟沙星、环丙沙星、恩诺沙星等9种药物残留。试样经乙腈均质提取,冷冻离心脱脂,旋转蒸发浓缩,用流动相复溶后经乙腈饱和的正己烷除油,随后进行UPLC-MS/MS定性定量分析。该方法测定9种药物的检出限为0.1μg/kg,定量限为0.5μg/kg。在添加水平分别为0.5、1.0和2.0μg/kg时,9种药物的加标回收率为81.5%~97.6%,相对标准偏差（RSD）为2.1%~8.9%。该方法简便、准确,可作为鸡肉中9种药物残留检测的确证方法。An analytical method for the simultaneous determination of clopidol, sulfadiazine, sulfamethazine, sulfametoxydiazine, sulfamethoxypyridazine, norfloxacin, ofloxacin, cipro- floxacin, enrofloxacin in chickens by ultra performance liquid chromatography coupled with tandem quadrupole mass spectrometry （UPLC-MS/MS） in positive ion mode with multiple reac- tion monitoring （MRM） has been developed and validated. The samples were homogenized and extracted with acetonitrile. After defatted with high speed frozen centrifugation, the superna- tant solution was evaporated and the residue was dissolved with the mobile phase and defatted with n-hexane. It was then analyzed with UPLC-MS/MS. The limit of detection of this method was 0. 1 μg/kg, and the limit of quantification was 0.5μg/kg. The average recoveries （spiked at the levels of 0.5, 1. 0, 2.0 μg/kg） ranged from 81.5% to 97.5%, with the relative standard deviations between 2. 1% and 8.9%. The results demonstrated that the method is simple, accu- rate and suitable for the identification and quantification of these drug residues in chickens.

关 键 词：超高效液相色谱-串联质谱法 二氯二甲吡啶酚 磺胺 喹诺酮 鸡肉 多残留 

分 类 号：O658[理学—分析化学]