分散固相萃取-在线凝胶色谱串联质谱法快速检测鲜浙贝母中17种农药残留

Determinnation of 17 pesticide residues in fresh Fritillaria thunbergii by QuEChers cleanup and GPC-GC/MS

目的：建立简便、快速测定鲜浙贝母中17种农药多残留的检测方法。方法：以1%醋酸乙腈溶液作为提取剂,PSA（Primary Second amine）为分散净化剂,采用在线凝胶色谱-气相质谱联用,在离子监测模式下进行检测,并用外标法进行定量。结果：17种农药在0.0156~1.042mg/L范围内线性关系良好,3个添加水平的平均回收率都在80%~120%之间。相对标准偏差在5.12%~10.53%之间;检测限在1.83~9.13μg/L范围内。结论：该方法可以满足鲜贝母中多种农药残留的检测要求,具有简便、快速、灵敏度高、重现性好的特点。

Objective：To established a simple and quick method for the determination of 17 pestidues in fresh Fritillaria thunbergii.Methods：Pesticides were extracted with acetic acid 1% in acetonitrile and cleaned up by dispersive solid phase extraction using primary second amine,detected by Online GPC-GC/MS under selective ion monitoring mode and quantified by external standard method.Results：Good liner were obtained ranging 0.0156～1.042mg/L.The average recoveries of 17 pesticides in three levels were 80～120% with relative standard deviation（RSD） below10.53%.The limits of detection（LODs） were 1.83～9.13μg/L.Conclusion： The simplicity,quicik,sensitive and good reproduction quality made it be well suitable for the analysis of multi-pesticides in fresh Fritillaria thunbergii.