建立了改良的QuEChERS结合高效液相色谱-串联质谱同时测定水产品中13种镇静剂类药物的分析方法。样品经氨化乙腈提取,增强型去除脂类基质吸附剂(Enhanced matrix removal-lipid,EMR-Lipid)净化,然后用高效液相色谱-串联质谱仪多反应监测模式检测,外标法定量。结果表明,13种镇静剂在0.5~40 μg/L浓度范围内均呈良好的线性关系,相关系数(r)均大于0.99,方法检出限为0.0103~0.1470 μg/kg,定量限为0.0340~0.4850 μg/kg。在3个不同添加水平下的平均回收率为70.7%~108.0%,RSD为1.4%~10.3%。本方法操作简单,灵敏度高,净化效果好,可用于水产品中13种镇静剂的快速分析。
A method was established for the simultaneous determination of 13 sedative residues in aquatic products using modified QuEChERS and high-performance liquid chromatography-tandem mass spectrometry.The samples were extracted with ammoniate acetonitrile,cleaned-up with EMR-Lipid.The analytes were detected in the multi-reaction monitoring(MRM)mode and quantified by the external standard method. The analytes were quantified by matrix-matched standard solutions with external standard method. The linear relationships of 13 sedatives were good and the correlation coefficients(r)were greater than 0.99. The limits of detection(LODs)and the limits of quantification(LOQs)for the analytes were in the range of 0.0103 to 0.1470 μg/kg and 0.0340 to 0.4850 μg/kg. The average recoveries of 13 sedatives spiked at three levels in blank samples ranged from 70.7% to 108.0% with the RSDs from 1.4% to 10.3%.The developed method is easy to operate,sensitive with good purification effect. It can be applied to the rapid determination of the 13 sedatives in aquatic products.