滤过型萃取柱-超高效液相色谱-串联质谱法同时测定水果中11种农药残留  

Simultaneous Determination of 11 Pesticide Residues in Fruits by Filtered Extraction Column-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王子剑[1] 赵劲松[1] 郭晓宇[1] 李倩[1] 郑天驰 商爱媛 范赛[2] WANG ZiJian;ZHAO Jingsong;GUO Xiaoyu;LI Qian;ZHENG Tianchi;SHANG Aiyuan;FAN Sai(Daxing Center for Disease Control and Prevention,Beijing 102600,China;Beijing Center for Disease Control and Prevention,Beijing 100013,China)

机构地区：[1]北京市大兴区疾病预防控制中心,北京102600 [2]北京市疾病预防控制中心,北京100013

出　　处：《分析测试技术与仪器》2023年第1期23-29,共7页Analysis and Testing Technology and Instruments

摘　　要：建立了超高效液相色谱-串联质谱测定水果中杀虫剂、杀菌剂、除草剂等11种常见农药的方法.水果样品经乙腈提取,提取液经滤过型萃取柱(m-PFC)净化,正离子多反应模式(MRM)监测,外标法定量.水果中11种农药的检出限为1~3µg/kg,在1.0~100.0 ng/mL的范围内线性关系良好,相关系数r不低于0.9969.在样品基质中分别添加5、20、50µg/kg的标准品进行加标回收试验,11种农药的平均回收率为88.9%~110.1%,相对标准偏差(RSD)为2.7%~8.5%(n=6).方法操作简单、灵敏度高,能够准确测定水果中11种农药残留.A method for the determination of 11 common pesticides in fruits,such as pesticides,fungicides and herbicides,was set up using the ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The fruit samples were extracted with acetonitrile,and the extracts were purified using a filtered extraction column(m-PFC),monitored by the positive ion multiple reaction mode(MRM),and quantified by the external standard method.The detection limits of 11 pesticides in fruits were 1~3µg/kg,with good linearity in the range of 1.0~100.0 ng/mL,with the correlation coefficient r not less than 0.9969.The standards of 5,20 and 50µg/kg were added to the sample matrix for spiked recovery tests.The average recoveries rate of 11 pesticides were 88.9%~110.1%,and the relative standard deviation(RSD)were 2.7%~8.5%(n=6).The method is simple and sensitive,and can accurately determine 11 pesticide residues in fruits.

关 键 词：农药残留 滤过型萃取柱 超高效液相色谱-串联质谱法 水果 

分 类 号：O657.63[理学—分析化学]