农药学学报2024,Vol.26Issue(6) :1191-1200.DOI:10.16801/j.issn.1008-7303.2024.0096

超高效液相色谱-串联质谱法同时测定玉米中2甲4氯异辛酯及其代谢物2甲4氯残留

Simultaneous determination of MCPA-isooctyl and its metabolite MCPA in maize by ultra-performance liquid chromatography-tandem mass spectrometry

许甜甜 王继东 史陶中 吴祥为 马鑫 唐俊
农药学学报2024,Vol.26Issue(6) :1191-1200.DOI:10.16801/j.issn.1008-7303.2024.0096

超高效液相色谱-串联质谱法同时测定玉米中2甲4氯异辛酯及其代谢物2甲4氯残留

Simultaneous determination of MCPA-isooctyl and its metabolite MCPA in maize by ultra-performance liquid chromatography-tandem mass spectrometry

许甜甜 1王继东 1史陶中 1吴祥为 1马鑫 1唐俊1
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作者信息

  • 1. 安徽农业大学资源与环境学院,合肥 230036
  • 折叠

摘要

建立了同时测定玉米(鲜食玉米、玉米籽粒、玉米秸秆)中2甲4氯异辛酯及其代谢物2甲4氯残留的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法.样品用盐酸酸化后经乙腈提取,NH2-SPE柱净化,采用多反应监测(MRM)模式,UPLC-MS/MS测定,外标法定量.结果表明:在添加水平为0.01~0.5 mg/kg时,2甲4氯异辛酯及2甲4氯的平均回收率为82%~107%,相对标准偏差为0.81%~8.9%.方法的检出限(LOD)为0.38~1.42yg/kg,定量限(LOQ)为1.28~4.76μg/kg.该方法正确度高、灵敏性好,符合农药残留分析的要求,可以实现2甲4氯异辛酯及其代谢物2甲4氯残留的同时检测.

Abstract

An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed for the simultaneous determination of MCPA-isooctyl and its metabolite MCPA residues in maize(fresh maize,maize kernel and maize stover).The samples were acidified with hydrochloric acid,extracted with acetonitrile,cleaned-up by NH2-SPE column,analyzed by UPLC-MS/MS in multiple reaction monitoring(MRM)mode,and quantified by external standard method.The results showed that the average recoveries of MCPA-isooctyl and MCPA were in the range of 82%~107%at the spiked levels of 0.01~0.5 mg/kg with the relative standard deviations(RSDs)of 0.81%~8.9%.The limits of detection(LOD)of the method were 0.38~1.42 μg/kg and the limits of quantification(LOQ)were 1.28~4.76 μg/kg.The method is reliable and sensitive,and meets the requirements of pesticide residue analysis,and it can achieve the simultaneous detection of MCPA-isooctyl and its metabolite MCPA in corn.

关键词

2甲4氯异辛酯/2甲4氯/玉米/超高效液相色谱-串联质谱/残留

Key words

MCPA-isooctyl/MCPA/maize/UPLC-MS/MS/residue

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出版年

2024
农药学学报
中国农业大学

农药学学报

CSTPCD北大核心
影响因子:0.879
ISSN:1008-7303
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