超高效液相色谱-串联质谱法测定鸡肉中9种大环内酯类抗生素

目的建立超高效液相色谱-串联质谱法测定9种大环内酯类抗生素药物的分析方法。方法采用响应面法优化净化方法。样品经1%甲酸-乙腈提取,提取液经50 mg C₁₈、80 mg N-丙基乙二胺(primary secondary amine,PSA)、100 mg MgSO₄净化,Waters ACQUITY UPLC HSS T₃色谱柱(2.1 mm×100 mm,1.8μm)进行分离,采用电喷雾正离子多反应监测扫描(multiple reaction monitoring,MRM)模式下进行测定,外标法定量。结果其中8种抗生素线性范围1~50 ng/mL,替米考星为5~50 ng/mL,相关系数(r²)在0.9910-0.9993之间。替米考星检出限为2.5μg/kg,定量限为10μg/kg,其余8种化合物检出限均为0.5μg/kg,定量限均为2μg/kg。在低(替米考星10μg/kg,其他2μg/kg)、中(替米考星20μg/kg,其他10μg/kg)、高(替米考星40μg/kg,其他20μg/kg)3个添加水平下进行加标回收实验,9种抗生素平均回收率在81.30%~105.30%之间,相对标准偏差在0.77%~2.41%之间(n=6)。结论该方法操作简单、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要求,解决了大环内酯抗生素检测提取过程过于繁琐的问题,可为食品抗生素残留检测提供更方便、更快捷的检测方法支持。

Determination of 9 macrolides antibiotics in chicken by ultra performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for the determination of 9 macrolide antibiotics by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).Methods The method was optimized by response surface methodology.Samples were extracted by 1%formic acid-acetonitrile,and the extract was purified by 50 mg C₁₈,80 mg primary secondary amine(PSA)and 100 mg MgSO₄.The chromatographic separation was performed on Waters ACQUITY UPLC HSS T₃(2.1 mm×100 mm,1.8μm)chromatographic column,monitored by electrospray positive ions multiple reaction monitoring scanning mode,and quantified by external standard method.Results The linear range of 8 antibiotics was 1-50 ng/mL,and tilmicosin was 5-50 ng/mL,and the correlation coefficient(r²)was 0.9910-0.9993.The limit of detection of tilmicosin was 2.5μg/kg,the limit of quantitative was 10μg/kg,the limits of detection of the other 8 compounds were 0.5μg/kg,and the limits of quantitative were 2μg/kg.The recovery experiment of 9 antibiotics was tested at 3 levels:low(tilmicosin 10μg/kg,others 2μg/kg),medium(tilmicosin 20μg/kg,other 10μg/kg)and high(tilmicosin 40μg/kg,others 20μg/kg).The average recoveries of 9 antibiotics ranged from 81.30%to 105.30%,and the relative deviation(n=6)was 0.77%-2.41%(n=6).Conclusion This method is simple,effective,sensitive,accurate and precise,which meets the requirements of multi-residue detection technology and can solve the problem that the detection and extraction process of macrolide antibiotics is too complicated,which can provide more convenient and faster detection method support for food safety detection.