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

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

中文关键词:  鸡肉  响应面分析法  超高效液相色谱-串联质谱法  大环内酯类抗生素

英文关键词:chicken  response surface analysis  ultra performance liquid chromatography-tandem mass spectrometry  macrolide antibiotics

中文摘要:

      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, 1.8 μm)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2.5 μg/kg, 定量限为10 μg/kg, 其余8种化合物检出限均为0.5 μg/kg, 定量限均为2 μg/kg。在低(替米考星10 μg/kg, 其他2 μg/kg)、中(替米考星20 μg/kg, 其他10 μg/kg)、高(替米考星40 μg/kg, 其他20 μg/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。

英文摘要:

      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, 1.8 μm) 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 2.5 μg/kg, the limit of quantitative was 10 μg/kg, the limits of detection of the other 8 compounds were 0.5 μg/kg, and the limits of quantitative were 2 μg/kg. The recovery experiment of 9 antibiotics was tested at 3 levels: low (tilmicosin 10 μg/kg, others 2 μg/kg), medium (tilmicosin 20 μg/kg, other 10 μg/kg) and high (tilmicosin 40 μg/kg, others 20 μg/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.