改进的QuEChERS-气相色谱-串联质谱法测定鲜烟叶中27种农药残留  

Determination of 27 pesticide residues in fresh tobacco leaves with modified-QuEChERS by gas chromatography-tandem mass spectrometry

作　　者：艾小勇[1,2] 任志芹 袁飞[1] 原保忠[2] 张元[1] 李伟青[1] 张峰[1] 

机构地区：[1]中国检验检疫科学研究院,北京100123 [2]华中农业大学植物科技学院,湖北武汉430070 [3]河北农业大学理学院,河北保定071001

出　　处：《广东农业科学》2015年第17期96-101,共6页Guangdong Agricultural Sciences

基　　金：国家重大仪器设备开发专项(2012YQ 14000806);国家质检总局质检公益性行业科研专项(201310134;201410088-02);国家质检总局科技计划项目(2013IK202)

摘　　要：建立了鲜烟叶中27种农药的气相色谱-串联质谱（GC—MS／MS）检测方法。样品以乙腈为提取溶剂，对鲜烟叶中27种农药进行提取，采用N-丙基乙二胺（PSA）、c18和石墨化碳黑（GCB）3种复合吸附剂净化，采用GC—MS／MS在多反应监测（MRM）模式下进行检测，基质匹配外标法定量。结果显示，27种农药在10～1000μg／kg范围内，线性相关系数（r2）均大于0．995，检出限（LOD）为0．4～2．9μg／kg，定量限（LOQ）为1．4～9．6μg／kg，在3个添加水平下的回收率为71．8％～108．1％，相对标准偏差（RSD）为3．2％～11．8％。该方法前处理简单快速，准确度和精密度均符合农药多残留检测技术的要求，适用于鲜烟叶中27种农药残留的快速筛查和测定。A GC-MS/MS method was established for simuhaneous determination of 27 pesticides in fresh tobacco leaves. Using acetonitrile as extraction solvent and including a cleanup step with primary secondary amine （ PSA ） , graphitized carbon black （ GCB ） and C18 to reduce the high matrix effect found in these products. The samples were quantified using external standard with the matrix matched standard calibration curve method. Good linearities of two suckercides were observed in the range of 10-1 000 tXg/kg with correlation coefficients more than 0.995. The limits of detection （ LOD ） and the limits of quantification （ LOQ ） for 27 pesticides were 0.4-2.9μg/kg and 1.4-9.6 g/kg, respectively. The average recoveries at three spiked concentration levels ranged from 71.8% to 108.1%. The repeatabilities expressed as relative standard deviations （ RSD ） ranged from 3.2% to 11.8%. The method was suitable for the determination of 27 pesticide residues in fresh tobacco leaves.

关 键 词：QUECHERS 复合吸附剂 农药残留 鲜烟叶 气相色谱-串联质谱 

分 类 号：TQ450.263[化学工程—农药化工]