全自动固相萃取结合气相色谱-串联质谱法快速测定石斛中62种常用农药残留  

Automatic QuEChERS-GC-MS/MS method for rapid determination of residues of 62 common pesticides in Dendrobium

作　　者：曹桂红[1] 刘璐 许波[1] 茅向军[1] 李志 王兴宁 CAO Gui-hong;LIU Lu;XV Bo;MAO Xiang-jun;LI Zhi;WANG Xing-ning(Guizhou Provincial Institute for Food and Drug Control,Guiyang 550023,China;Guiyang Customs Comprehensive Technology Center,Guiyang 550023,China)

机构地区：[1]贵州省食品药品检验所,贵州贵阳550023 [2]贵阳海关综合技术中心,贵州贵阳550023

出　　处：《化学研究与应用》2024年第5期1127-1136,共10页Chemical Research and Application

基　　金：贵州省科技计划项目(黔科合NY字[2022]3005号)资助;海关总署科研项目(2022HK132)资助。

摘　　要：建立全自动QuEChERS方法结合气相色谱-串联质谱技术检测石斛中62种常用农药残留的分析方法。样品经全自动QuEChERS样品制备系统涡旋、振动和离心处理,HP-5MS色谱柱分离,选择分时间段的多反应监测模式进行数据采集及定性定量分析,内标法定量。62种农药在5~500ng·mL^(-1)范围内线性关系良好,相关系数(r^(2))大于0.99;3个加标水平下(0.01mg·kg^(-1)、0.05mg·kg^(-1)和0.1mg·kg^(-1)),平均回收率为65.6%~109.3%,相对标准偏差(RSD)为2.4%~15.1%;定量限均低至0.01mg·kg^(-1)。该方法简便、快速、灵敏、准确性高,适用于石斛中62种常用农药残留的快速检测。A method for the determination of 62common pesticide residues in dendrobium was established by using automatic QuEChERS method and gas chromatography tandem mass spectrometry(GC-MS/MS).Samples were processed by vortexing,shaking and centrifugation in a fully automated QuEChERS sample preparation system,separated by HP-5 MS column,selected in multiple reaction monitoring mode over time periods for data acquisition and qualitative and quantitative analysis,and quantified by internal standard.the results showed that 62 pesticides were linear in the range of 5-500 ng mL^(-1)with correlation coefficients(r^(2))greater than 0.99;at the three spiked levels(0.0lmg·kg^(-1),0.05mg·kg^(-1)and 0.1 mg·kg^(-1)),the average recoveries ranged from 65.6%to 109.3%,and the relative standard deviations(RSD)ranged from 2.4%to 15.1%;The limits of quantification were all as low as 0.01 mg kg^(-1).This method is simple,rapid,sensitive,and accurate,It is suitable for the rapid detection of 62 common pesticide residues in dendrobium.

关 键 词：气相色谱-串联质谱 全自动QuEChERS 农药残留 石斛 

分 类 号：O657.7[理学—分析化学]