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

    • 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0.38~1.42 μg/kg,定量限( LOQ) 为1.28~4.76 μg/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.

       

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