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超高效液相色谱-串联质谱法检测蔬菜中除虫菊素残留
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作者单位
李凌云,许晓敏,林桓,钱洪,黄晓冬,刘广洋,郑姝宁,徐东辉,裴志国 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 
基金项目: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)
中文摘要: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0.01 mg/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。
中文关键词:农药残留  蔬菜  除虫菊素  超高效液相色谱-串联质谱
 
Detection of Pyrethrins in Vegetables by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract: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.
Key Words:pesticide residues  vegetable  pyrethrins  ultra high performance liquid chromatography-tandem mass spectrometry
引用本文:李凌云,许晓敏,林桓,钱洪,黄晓冬,刘广洋,郑姝宁,徐东辉,裴志国.超高效液相色谱-串联质谱法检测蔬菜中除虫菊素残留[J].分析测试学报,2018,37(1):98-102.
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