液相色谱-串联质谱法测定动物源性食品中5种镇静剂药物残留量

Determination of 5 kinds of sedative drug residues in animal-derived foods by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱法  动物源性食品  镇定剂  残留量

英文关键词:high performance liquid chromatography-tandem mass spectrometry  animal-derived foods  sedative  residue

中文摘要:

      目的 建立液相色谱-串联质谱法同时测定动物源性食品中5种镇静剂残留量的方法。方法 样品用乙腈提取后, 经过Oasis HLB固相萃取柱净化后收集, 用乙腈-0.1%甲酸水溶液为流动相, Waters ACQUITY UPLC?BEH C18色谱柱分离进行液相色谱梯度洗脱, 质谱多反应监测式进行检测, 内标法定量。结果 5种镇静剂的线性关系良好, 相关系数r≥0.9991, 其检出限为0.07~0.11 μg/kg, 样品的加标回收率为94.5%~110.4%, 相对标准偏差(relative standard deviation, RSD)为3.76%~6.33%。结论 该方法样品处理后基质干扰小, 检测灵敏度高, 结果稳定、可靠, 适用于动物源性食品中5种镇静剂药物残留的检测。

英文摘要:

      Objective To establish a simultaneous detection method of 5 kinds of sedative residues in animal-derived foods by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile and collected after purification by Oasis HLB solid phase extraction column. The sample solution was separated by Waters ACQUITY UPLC?BEH C18 chromatographic column, with liquid chromatography gradient elution using acetonitrile-0.1% formic acid solution as the mobile phase. Results Five kinds of sedatives had good linear relationships with the correlation coefficients r≥0.9991. Detection limits were 0.07-0.11 μg/kg. The average recoveries for 5 kinds of sedatives were 94.5%-110.4%, and relative standard deviations (RSDs) of testing results were 3.76%-6.33%. Conclusion The method is accurate and sensitive with little background, which is suitable for determination of 5 kinds of sedative residues in animal-derived foods.