UPLC-MS/MS测定葡萄籽提取物中78种农药残留  

Determination of 78 pesticide residues in grape seed P.E using UPLC-MS/MS

作　　者：孔祥虹 黄江锐 何强 郝开拓 

机构地区：[1]陕西出入境检验检疫局,西安710068

出　　处：《分析试验室》2012年第5期38-43,共6页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局科研项目(2009IK285);国家公益性行业科研项目(201010040)资助

摘　　要：建立了超高效液相色谱串联质谱法(UPLC-MS/MS)检测葡萄籽提取物中78种农药残留物的分析方法。样品用乙腈振荡提取,经乙二胺-N-丙基甲硅烷(PSA)和石墨化炭(GCB)固相萃取柱串联净化,乙腈-甲苯(V/V3:1)洗脱,洗脱液浓缩至约0.5 mL后,于45℃下氮气吹干,1.0 mL乙腈定容,UPLC-MS/MS测定,外标法定量。葡萄籽提取物中,78种农药在0.001～0.2μg/mL范围内线性关系均良好;所有农药的方法定量限(LOQ)均低于17.0μg/kg;在5,25,50μg/kg的添加水平下,葡萄籽提取物中78种农药的平均回收率处于72.6%～113.5%之间,相对标准偏差不大于11%。方法适用于葡萄籽提取物中78种农药残留的快速筛查测定。A multiresidue analytical method was developed for the determination of 78 pesticides in grape seed P.E using ultra performance liquid chromatography coupled with tandem mass spectrometry（UPLC-MS/MS）.The pesticide residues were extracted from grape seed P.E by acetonitrile,cleaned-up by ethylenediamine-N-propyl silyl（PSA） and graphite carbon（GCB）,and then eluted with acetonitrile-toluene（3：1,V/V）.The eluate was concentrated to about 0.5 mL with a rotary evaporator,dried with nitrogen at 45 ℃.All the 78 pesticides showed good linearity in the range of 0.001-0.2 mg /L,and the limits of quantification（LOQs,S /N≥10） were all less than 17.0 μg/kg.The average recoveries of all the pesticides were in the range of 72.6% to 113.5% at three spiked levels of 5,25 and 50 μg/kg in grape seed P.E,with the relative standard deviations（RSDs） were lower than 11%.

关 键 词：超高效液相色谱串联质谱 葡萄籽提取物 农药残留 

分 类 号：O657.63[理学—分析化学]