超高效液相色谱-串联质谱法检测蔬菜中除虫菊素残留  

Detection of Pyrethrins in Vegetables by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李凌云[1] 许晓敏[1] 林桓[1] 钱洪[1] 黄晓冬[1] 刘广洋 郑姝宁[1] 徐东辉[1] 裴志国[2] LI Ling-yun;XU Xiao-min;LIN Huan;QIAN Hong;HUANG Xiao-dong;LIU Guang-yang;ZHENG Shu-ning;XU Dong-hui;PEI Zhi-guo(Key Laboratory of Vegetables Quality and Safety Control,Ministry of Agriculture,Key Laboratory of Biology and Genetic Improvement of Horticultural Crops,Ministry of Agriculture,Institute of Vegetables and Flowers,Chinese Academy of Agricultural Sciences,Beijing 100081,China;State Key Laboratory of Environmental Chemistry and Ecotoxicology,Research Center for Eco-Environmental Sciences,Chinese Academy of Sciences,Beijing 100085,China)

机构地区：[1]中国农业科学院蔬菜花卉研究所,农业部蔬菜质量安全控制重点实验室,农业部园艺作物生物学与种质创制重点实验室,北京100081 [2]中国科学院生态环境研究中心,环境化学与生态毒理学国家重点实验室,北京100085

出　　处：《分析测试学报》2018年第1期98-102,共5页Journal of Instrumental Analysis

基　　金：国家蔬菜产品质量安全风险评估项目(GJFP2017002);国家重点研发计划项目(2016YFD0200200)

摘　　要：建立了蔬菜中除虫菊素的超高效液相色谱-串联质谱(UPLC-MS/MS)快速检测技术。采用乙腈提取,盐析后无需净化,直接进样分析,正离子多反应监测(MRM)模式测定。结果表明,6种除虫菊素的线性关系良好,相关系数为0.999 5~0.999 9,在0.05、0.1、0.5 mg/kg 3个加标水平下,6种物质的平均回收率为73.9%~109.3%,相对标准偏差(RSDs)为0.4%~7.7%;除虫菊素Ⅰ、除虫菊素Ⅱ的定量下限为0.01mg/kg,瓜叶菊素Ⅰ、瓜叶菊素Ⅱ、茉酮菊素Ⅰ和茉酮菊素Ⅱ的定量下限为0.05 mg/kg,定量下限均指除虫菊素总量。结果表明该方法简便、快速、灵敏度高,适用于蔬菜中除虫菊素的快速检测分析。An analytical method was successfully developed for the rapid detection of pyrethrins in vegetables using ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).Vegetable samples were extracted with acetonitrile.After salting out,the solvent extracts were determined by UHPLC-MS/MS without further cleanup steps.The positive ion mode and multiple reaction monitoring(MRM)mode were used to identify and quantify pyrethrins in vegetables.Results showed that all six compounds had good linearity in their respective concentration ranges with the correlation coefficients of 0.999 5-0.999 9.Their average recoveries at spiked levels of 0.05,0.1,0.5 mg/kg ranged from 73.9%to 109.3%with relative standard deviations(RSDs)of 0.4%-7.7%.The limits of quantitation(LOQs)were 0.01 mg/kg for pyrethrinⅠand pyrethrinⅡ,and 0.05 mg/kg for cinerinⅠ,cinerinⅡ,jasmolinⅠand jasmolinⅡ.Both LOQs referred to total pyrethrins.Results showed that this method was simple,rapid and sensitive,and was suitable for the rapid determination of pyrethrins in vegetables.

关 键 词：农药残留 蔬菜 除虫菊素 超高效液相色谱-串联质谱 

分 类 号：O657.7[理学—分析化学] O657.63[理学—化学]