GC-MS/MS一测多评法测定木瓜中的5种农药残留

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英文篇名：Simultaneous determination of five residual pesticides in Chaenomelis Fructus by GC-MS/MS 作者：陈道华 ; 余敏灵 ; 陈文秋 ; 杨璐 英文作者：CHEN Daohua;YU Minling;CHEN Wenqiu;YANGLu;The Traditional Chinese Medicine Hospital of Chengdu Qingbaijiang;Leshan Food and Drug Control Inspection and Testing Center;Food and Drug Supervision and Inspection Team of Leshan; 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 英文关键词：GC-MS/MS;;Determination;;Chaenomelis Fructus;;Fungiclor;;Procymidone;;Alpha endosulfan;;Beta endosulfan;;Endosulfan sulfate;;Ipesticide residue;;Quantitative anlaysis multicomponents by single marker 中文刊名：HXYO 英文刊名：West China Journal of Pharmaceutical Sciences 机构：成都市青白江中医院;乐山市食品药品检验检测中心;乐山市食品药品监督稽查支队; 出版日期：2019-05-09 09:18 出版单位：华西药学杂志 年：2019 期：v.34 语种：中文; 页：HXYO201903016 页数：7 CN：03 ISSN：51-1218/R 分类号：73-79

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~(-4)ng,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 were8. 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.

引文

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