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超高效液相色谱-串联质谱法快速检测菜豆及土壤中的灭蝇胺残留
引用本文:徐军,张盈,董丰收,刘新刚,郭紫兰,郑永权.超高效液相色谱-串联质谱法快速检测菜豆及土壤中的灭蝇胺残留[J].农药学学报,2012,14(6):654-658.
作者姓名:徐军  张盈  董丰收  刘新刚  郭紫兰  郑永权
作者单位:1.中国农业科学院 植物保护研究所,北京 100193
基金项目:国家自然科学基金资助项目(31171879;31000863).
摘    要:建立了采用超高效液相色谱-串联质谱仪(UPLC-MS/MS)快速检测分析菜豆及其土壤中灭蝇胺残留的方法。样品经5 mmol/L的乙酸铵-乙腈溶液V(乙酸铵):V(乙腈)=1:4]提取、定容,N-丙基乙二胺(PSA)净化后用UPLC-MS/MS在正离子模式下以多反应监测扫描方式进行测定,外标法定量。结果表明:在0.05~1 mg/kg添加水平范围内,灭蝇胺在菜豆和土壤中的平均回 收率为80.1%~95.2%,相对标准偏差(RSD)为1.9%~9.1%,检出限(LOD)为3.8~5.9 μg/kg,定量限(LOQ)为50 μg/kg。该方法操作简单、灵敏度高、定量准确且测定浓度范围宽,适用于菜豆及土壤中灭蝇胺的残留分析。

关 键 词:超高效液相色谱-串联质谱    灭蝇胺    残留    菜豆    土壤
收稿时间:2012/8/22 0:00:00
修稿时间:2012/9/27 0:00:00

Determination of cyromazine residues in common bean and soil using ultraperformance liquid chromatography-tandem mass spectrometry
XU Jun,ZHANG Ying,DONG Fengshou,LIU Xingang,GUO Zilan and ZHENG Yongquan.Determination of cyromazine residues in common bean and soil using ultraperformance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Pesticide Science,2012,14(6):654-658.
Authors:XU Jun  ZHANG Ying  DONG Fengshou  LIU Xingang  GUO Zilan and ZHENG Yongquan
Institution:1.Institute of Plant Protection, Chinese Academy of Agricultural Science, Beijing 100193, China2.College of Bio-Safety Science & Technology, Hunan Agricultural University, Changsha 410128, China
Abstract:A rapid method for determination of cyromazine residues in common bean(Phaseolus vulgaris) and soil was established based on ultraperformance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The sample was extracted with 5 mmol/L solution of ammonium acetate and acetonitrile V(acetate):V(acetonitrile)=1:4] and then purified by primary secondary amine(PSA).The cyromazine residues were analyzed by UPLC-MS/MS under multiple reaction monitoring mode and quantified with external standards.Average recoveries of cyromazine in common bean and soil at three levels(0.05,0.5 and 1 mg/kg) ranged from 80.1% to 95.2% with relative standard deviations from 1.9% to 9.1%.Limits of detection of cyromazine were 3.8-5.9 μg/kg,while limits of quantification were 50 μg/kg.The method is simple and suitable for the routine and confirmation analysis of cyromazine residue.
Keywords:ultraperformance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  cyromazine  residue  common bean(Phaseolus vulgaris)  soil
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