微孔膜萃取辅助QuEChERS-LC-MS/MS测定鸡肉中磺胺和喹诺酮类兽药  

Determination of sulfanilamide and quinolone veterinary drugs in chicken with QuEChERS-LC-MS/MS assisted by microporous membrane extraction

作　　者：顾长瑜 王真 安彗心 周丽洋 雷正阳 王亚楠 刘熙媛 陈俐[2] 柯润辉 GU Changyu;WANG Zhen;AN Huixin;ZHOU Liyang;LEI Zhengyang;WANG Yanan;LIU Xiyuan;CHEN Li;KE Runhui(China Light Inspection and Certification Co.,Ltd.,Beijing 100016,China;Beijing University of Agriculture-Food Scinence and Engineering College;Beijing Technology and Business University)

机构地区：[1]中轻检验认证有限公司,北京100016 [2]北京农学院食品科学与工程学院 [3]北京工商大学

出　　处：《质量安全与检验检测》2024年第5期14-22,共9页QUALITY SAFETY INSPECTION AND TESTING

基　　金：现代农业产业技术体系北京市创新团队项目(BAIC06-2024)。

摘　　要：建立了聚四氟乙烯微孔滤膜萃取辅助QuEChERS法,结合高效液相色谱-串联质谱对鸡肉中磺胺类和喹诺酮类兽药残留进行快速测定的方法。样品经QuEChERS提取净化,ACQUITY UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7μm)分离,质谱采用ESI源,正离子模式下进行多重反应监测(MRM),外标法定量。结果表明,23种待测物质在各自线性范围内呈现良好的线性关系。相关系数均大于0.999,检出限为0.0008 mg/kg,定量限为0.002 mg/kg;在0.002~0.020 mg/kg加标水平下平均回收率为80.4%~110.4%,相对标准偏差(RSD,n=6)为2.7%~12.1%。该方法前处理简单高效,易于自动化,稳定性好,可以广泛应用于鸡肉中磺胺和喹诺酮类药物的检测。A method was developed for the rapid determination of sulfonamides and quinolones veterinary drug residues in chicken by polytetrafluoroethylene(PTFE)microporous membrane extraction-assisted QuEChERS method combined with ultra performance liquid chromatography-tandem mass spectrometry(LC-MS/MS).The sample was cleaned-up by QuEChERS extraction,separated on an ACQUITY UPLC BEH C18 column(50 mm×2.1 mm,1.7μm),and the mass spectrometry(MS)was performed by an ESI source with multiple reaction monitoring(MRM)in positive ionization mode,and quantified by external standard method.The results showed that the 23 substances to be measured exhibited good linearity within their respective linear ranges.The correlation coefficients were all greater than 0.999,and the limits of detection(LOD)were 0.0008 mg/kg and the limits of quantification(LOQ)were 0.002 mg/kg.The average recoveries at the spiked levels of 0.002-0.020 mg/kg ranged from 80.4%to 110.4%,and the relative standard deviations(RSD,n=6)were between 2.7%and 12.1%.The method is simple,efficient,easy to automate and stable,and can be widely used for the determination of sulfonamides and quinolones in chicken meat.

关 键 词：磺胺 喹诺酮 QUECHERS 膜萃取 高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS257.1[理学—化学]