24 pesticide residues in vegetables were rapidly performed pilot study with online GPC-GC/MS and QuEnChERS method.Samples were extracted with acetonitrile,purification using dispersive solid-phase extraction method.All 0.1 mg/kg spiked level pesticides included in our studied samples,the average recovery were in range of 70%~120%,the limits of detection were in range of 0.0002~0.009 mg/kg,the linear range of 0.025~0.030 mg/L and RSD were 1.41%~1.98% to satisfy the agricultural chemicals residual analysis request.The method of QuEChERS make pre-treating method more simple,convenient and rapid,and GPC of online GPC-GC/MS system could effectively clean up interfered compounds that QuEChERS pre-treating method couldn't completely deal with,which detect more accurately in vegetables.This method has high sensitivity and good precision.%采用QuEChERS前处理方法和在线凝胶渗透色谱-气相色谱质谱联用仪(gel permeation chromatography-gas chromatography/mass spectrometry,GPC-GC/MS)快速测定蔬菜中24种多农药残留。样品经乙腈提取,净化采用分散固相萃取的方式,加标浓度为0.1 mg/kg,油麦菜样品中的24种农药回收率大部分在70%~120%,24种农药的检出限范围在0.000 2~0.009 mg/kg,线性范围0.025~0.30 mg/L,相对标准偏差在1.41%~10.05%,满足农药多残留的分析要求。实验表明,QuEChERS方法提取和净化使样品前处理更为简单、方便、快速,GPC-GC/MS系统中的GPC柱弥补了QuEChERS方法去除干扰物不彻底的问题,能更准确地检测出蔬菜中多农药残留,检测灵敏度高,重现性好。
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