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GC-MS/MS一测多评法测定木瓜中的5种农药残留

Simultaneous determination of five residual pesticides in Chaenomelis Fructus by GC-MS/MS
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摘要 目的建立气相色谱-串联质谱法(GC-MS/MS)测定木瓜中五氯硝基苯、腐霉利、α-硫丹、β-硫丹、硫丹硫酸酯等农药残留的一测多评方法。方法采用Cleanert TPH净化柱净化、乙腈提取。采用串联质谱测定,根据色谱峰的相对保留时间及质荷比信息进行定性分析,以五氯硝基苯(m/z 294.8/236.8)的二级离子扫描峰面积为参照峰,建立以五氯硝基苯为对照品,测定木瓜中5种农药残留量的GC-MS/MS方法。结果0.1~1 ng五氯硝基苯、腐霉利、α-硫丹、β-硫丹、硫丹硫酸酯与其峰面积有较好的线性关系,检出限(以进样量计)分别为8.68×10^-5、1.37×10^-4、8.35×10^-4、2.65×10^-4、1.66×10^-4ng,平均回收率分别为96.9%、99.1%、98.7%、97.4%、97.8%。结论所用的一测多评方法简单快速,定量准确,适用于同时测定木瓜中五氯硝基苯、腐霉利、α-硫丹、β-硫丹、硫丹硫酸酯等农药的残留。 OBJECTIVE To establish a quantitative method for the simultaneous measurement of the residual level of fungiclor,procymidone,alpha endosulfan,beta endosulfan and endosulfan sulfate in Chaenomelis Fructus by GC-MS/MS.METHODS The samples were extracted using acetonitrile and then purified by Cleanert TPH column,then tested by GC-MC/MS.Information on relative retention time and mass charge ratio were used for qualitative analysis.The peak area obtained by secondary ion MS of fungiclor(m/z 294.8/236.8)was used as a reference peak to establish a method using fungiclor as another reference substance to determine the five residual pesticides in C.Fructus by GC-MS/MS.RESULTS When samples with contents in the range of 0.1-1.0 ng were injected,there existed a good linear relationship between the injection quantity and peak area.Limit of detections(LODs)of fungiclor,procymidone,alpha endosulfan,beta endosulfan and endosulfan sulfate were 8.68×10^-5,1.37×10^-4,8.35×10^-4,2.65×10^-4,and 1.66×10^-4 ng respectively.The average recovery rates were 96.9%,99.1%,98.7%,97.4%and 97.8%respectively.CONCLUSION The developed method is simple,accurate and rapid,which is appropriate for the quantification of residual quantity of fungiclor,procymidone,alpha endosulfan,beta endosulfan and endosulfan sulfate in C.Fructus.
作者 陈道华 余敏灵 陈文秋 杨璐 CHEN Daohua;YU Minling;CHEN Wenqiu;YANGLu(The Traditional Chinese Medicine Hospital of Chengdu Qingbaijiang,Chengdu,Sichuan,610031 P.R.China;Leshan Food and Drug Control Inspection and Testing Center,Leshan,Sichuan,614000 P.R.China;Food and Drug Supervision and Inspection Team of Leshan,Leshan,Sichuan,614000 P.R.China)
出处 《华西药学杂志》 CAS CSCD 2019年第3期275-281,共7页 West China Journal of Pharmaceutical Sciences
关键词 气相色谱-串联质谱 含量测定 木瓜 五氯硝基苯 腐霉利 α-硫丹 β-硫丹 硫丹硫酸酯 农药残留 一测多评 GC-MS/MS Determination Chaenomelis Fructus Fungiclor Procymidone Alpha endosulfan Beta endosulfan Endosulfan sulfate Ipesticide residue Quantitative anlaysis multicomponents by single marker
作者简介 陈道华,从事医院药学工作;通信作者:余敏灵,Email:89729204@qq.com.
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