QuEChERS-超高效液相色谱-串联质谱法同时测定绿豆和赤小豆中10种农药及其代谢物残留研究  

Study on simultaneous determination of ten pesticides and metabolite residues in mung bean and red bean by QuEChERS-liquid chromatographytandem mass spectrometry

作　　者：陶波[1] 乔禹欣 陈国峰[1,2] 马诚义 马红 TAO Bo;QIAO Yuxin;CHEN Guofeng;MA Chengyi;MA Hong(School of Agriculture, Northeast Agricultural University, Harbin 150030, China;Safety and Quality Institute of Agricultural Products, Heilongjiang Acadamy of Agricultural Sciences, Harbin 150086, China)

机构地区：[1]东北农业大学农学院,哈尔滨150030 [2]黑龙江省农业科学院农产品质量安全研究所,哈尔滨150086

出　　处：《东北农业大学学报》2018年第11期26-34,41,共10页Journal of Northeast Agricultural University

基　　金：国家重点研发计划子课题(2016YFD0200507-6)

摘　　要：研究旨在建立绿豆和赤小豆中氟磺胺草醚、烯草酮、精喹禾灵等10种常用除草剂及其代谢物液相色谱-串联质谱检测方法。试验样品经乙腈溶液提取,25 mg乙二胺-N-丙基硅烷(Primary secondary amine,PSA)吸附剂净化,利用乙腈和0.1%甲酸水作为流动相梯度洗脱,C18色谱柱分离,动态多反应监测模式下定量分析液相色谱-三重四极杆串联质谱。结果表明,10种农药及其代谢物5～100μg·L^(-1)呈良好线性关系,相关系数(r)为0.9978～0.9999。3个加标水平下,10种农药及其代谢物平均回收率90.2%～110.0%,相对标准偏差小于7.3%。该方法简便、快速、灵敏度高,适用于绿豆和赤小豆中多种除草剂及其代谢物同时检测,对解决绿豆和赤小豆食品安全问题具有重要意义。The aim of this study was to establish a simple analytical method for the determination of ten pesticides and metabolite residues in mung bean and red bean by using dispersive solid phase extraction combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS).Samples were extracted with acetonitrile,cleaned up with 25mg PSA.Qualitative analyses of ten pesticides and metabolite residues were carried out in the multiple reaction monitoring(MRM)model after the chromatographic separation on a reversed phase C18column with gradient elution using a mobile phase composed of acetonitrile and 0.1% formic acid aqueous solution.The results showed that there was a good linearity for ten pesticides and metabolite residues in the range of 5-100μg·L^-1with a coefficient of determination(r)were in the range of 0.9978-0.9999.The recoveries of ten pesticides and metabolite residues in mung bean and red bean were in the range of 90.2%-110.0% at three spiked concentration levels,and the precision,as indicated by relative standard deviations(RSDs,n=5),was not more than7.3%.The method was simple,rapid and sensitive,and could meet the requirements for the determination of pesticides and metabolites residues in mung bean and red bean.It was of great significance to solve the food safety problems of mung bean and red bean.

关 键 词：超高效液相色谱-串联质谱 绿豆 赤小豆 农药 代谢物 

分 类 号：TQ457[化学工程—农药化工] S482[农业科学—农药学]