QuEChERS法-液相色谱-串联质谱法测定蔬菜中7种农药及其代谢物的残留量  

Determination of 7 Pesticide and Metabolite Residues in Vegetables Using QuEChERS and Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王建华[1] 葛敏敏 张慧丽[2] 林洪[2] 汤志旭[1] 李立[3] WANG Jianhua;GE Minmin;ZHANG Huili;LIN Hong;TANG Zhixu;LI Li(Inspection and Quarantine Technical Center, Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China;College of Food Science and Engineering, Ocean University of China, Qingdao 266100, China;Chinese Academy of Inspection and Quarantine, Beijing 100176, China)

机构地区：[1]山东出入境检验检疫局检验检疫技术中心,山东青岛266002 [2]中国海洋大学食品科学与工程学院,山东青岛266100 [3]中国检验检疫科学研究院,北京100176

出　　处：《食品科学》2017年第20期235-241,共7页Food Science

基　　金：公益性行业(质检)科研专项(201410177;201210012)

摘　　要：样品经乙腈提取,C_(18)吸附剂和石墨化碳黑分散固相萃取净化,液相色谱-三重四极杆串联质谱在动态多反应监测模式下检测,基质匹配标准曲线外标法进行定量,建立了蔬菜中7种农药及其代谢物的多残留分析方法。在10、20μg/kg 7种农药及其添加物添加水平下,农药及其代谢物的平均回收率为71.9%~117.8%,相对标准偏差为0.8%~9.6%,定量限为0.2~10μg/kg。该方法简便、快速、灵敏,适用于蔬菜中多种农药及其代谢物的同时检测。A method was developed for the simultaneous determination of7pesticide and metabolite residues in vegetables by employing quick,easy,cheap,effective,rugged and safe(QuEChERS)extraction coupled with liquid chromatography triple quadrupole mass spectrometry(LC-MS/MS).Samples were extracted with acetonitrile,and then the extract was purified by dispersive solid phase extraction(SPE)using graphite carbon black(GCB)and C18sorbent.The analytes were monitored by liquid chromatography-tandem triple quadrupole mass spectrometry in the dynamic multiple reaction monitoring(DMRM)mode,and quantification was carried out by the external standard method with matrix-match standard solution.The recoveries at spiked levels of10and20μg/kg were in the range from71.9%to117.8%and the precision,expressed as relative standard deviation(RSD,n=3),ranged from0.8%to9.6%under the selected conditions.The limits of quantification(LOQs)were in the range of0.2-10μg/kg.The method proved to be simple,fast,sensitive and useful for the analysis of the7pesticides and their metabolite residues in vegetables.

关 键 词：液相色谱-串联质谱 蔬菜 农药及其代谢物 

分 类 号：S859.7[农业科学—临床兽医学]