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

作　　者：许甜甜 王继东 史陶中[1] 吴祥为[1] 马鑫[1] 唐俊[1] XU Tiantian;WANG Jidong;SHI Taozhong;WU Xiangwei;MA Xin;TANG Jun(College of Resources and Environment,Anhui Agricultural University,Hefei 230036,China)

机构地区：[1]安徽农业大学资源与环境学院,合肥230036

出　　处：《农药学学报》2024年第6期1191-1200,共10页Chinese Journal of Pesticide Science

基　　金：安徽省省级大学生创新创业训练计划项目(S202310364226,S202310364225)。

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0.38~1.42μg/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。An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLCMS/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 0.38~1.42μg/kg and the limits of quantification(LOQ)were 1.28~4.76μg/kg.The method is reliable and sensitive,and meets the requirements of pesticide residue analysis,and it can achieve the simultaneous detection of MCPAisooctyl 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 

分 类 号：O657.63[理学—分析化学]