QuEChERS-液相色谱-串联质谱法测定蔬菜中105种农药残留  

Determination of 105 pesticide residues in vegetables by QuEChERS-liquid chromatography-tandem mass spectrometry

作　　者：邓慧芬 张建莹 黄科 钟恬恬 林丽敏 DENG Huifen;ZHANG Jianying;HUANG Ke;ZHONG Tiantian;LIN Limin(Food Inspection&Quarantine Center,Shenzhen Customs,Shenzhen 518045,China)

机构地区：[1]深圳海关食品检验检疫技术中心,广东深圳518045

出　　处：《色谱》2018年第12期1211-1222,共12页Chinese Journal of Chromatography

基　　金：原国家质检总局项目(2017IK271;2017IK262)~~

摘　　要：通过优化QuEChERS前处理方法并结合液相色谱-串联质谱(LC-MS/MS)技术建立了蔬菜中105种典型杀虫剂、杀菌剂、除草剂、植物生长调节剂的多残留测定方法。目标化合物使用乙腈提取,以150 mg乙二胺-N-丙基硅烷(PSA)、150 mg封端十八烷基键合硅胶吸附剂(EC-C18)、30 mg石墨化炭黑(GCB)作为基质提取液净化剂。实验结果表明,在0. 010～0. 200 mg/L范围内,105种目标化合物的线性相关系数(r)>0. 99,方法定量限为0. 010mg/kg;3个添加水平的回收率范围为68. 2%～108%,相对标准偏差(RSD)为1. 02%～11. 8%。该方法快速简便,净化效果好,可用于蔬菜中日常农药残留的测定。After optimization of the QuEChERS pretreatment method,combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS)technology,a multi-residue determination method was established for 105 typical insecticides,bactericides,herbicides,and plant growth regulators in vegetables.The target compounds were extracted by acetonitrile,purified with 150 mg primary secondary amine(PSA),150 mg EC-C18,and 30 mg graphitized carbon black(GCB)adsorbents.The standard curves of 105 target compounds were linear in the concentration range of 0.010-0.200 mg/L,with correlation coefficients(r)>0.99.The limit of quantification was 0.010 mg/kg,the recoveries were between 68.2%and 108%at three spiked levels,and the RSDs of the method were between 1.02%and 11.8%.The method is suitable for the rapid determination of the common pesticides in vegetables owing to its advantages of rapidity,simplicity,and better purification.

关 键 词：QUECHERS 液相色谱-串联质谱 农药残留 蔬菜 

分 类 号：O658[理学—分析化学]