湖北农业科学 ›› 2018, Vol. 57 ›› Issue (17): 88-92.doi: 10.14088/j.cnki.issn0439-8114.2018.17.023

• 检测分析 • 上一篇    下一篇

GC-MS/MS测定叠鞘石斛中乐果等三种农药残留的一测多评研究

唐志康1, 陈文秋2, 余敏灵2, 饶春梅3, 余马1, 侯大斌1, 舒晓燕1, 黄晶1   

  1. 1.西南科技大学生命科学与工程学院,四川 绵阳 621010;
    2.乐山市食品药品检验检测中心,四川 乐山 614000;
    3.乐山市农业科学研究院,四川 乐山 614000
  • 收稿日期:2018-03-30 出版日期:2018-09-10 发布日期:2020-04-02
  • 通讯作者: 侯大斌,男,教授,博士,(电话)0816-6089523(电子信箱)dbhou@126.com。
  • 作者简介:唐志康(1976-),男,四川井研人,副研究员,博士,主要从事中药资源研究与开发工作,(电话)0816-6089516(电子信箱)tzkyaan@126.com。
  • 基金资助:
    西南科技大学博士基金项目(17ZX7104); 四川乐山市科技局重点研发项目(16SZD047)

Study on the Simultaneous Measurement of Three Residual Level of Pesticides such as Dimethoate in Dendrobium aurantiacum Using GC-MS/MS

TANG Zhi-kang1, CHEN Wen-qiu2, YU Min-ling2, RAO Chun-mei3, Yu Ma1, HOU Da-bin1, SHU Xiao-yan1, HUANG Jing1   

  1. 1.School of Life Science and Engineering,Southwest University of Science and Technology,Mianyang 621010,Sichuan,China;
    2.Sichuan Leshan for Food and Drug control,Leshan 614000,Sichuan,China;
    3.Leshan Academy of Agricultural Sciences,Leshan 614000,Sichuan,China
  • Received:2018-03-30 Online:2018-09-10 Published:2020-04-02

摘要: 以叠鞘石斛(Dendrobium aurantiacum)为研究对象,样品采用乙腈提取,经Cleanert TPH专用净化柱净化。用GC-MS/MS测定样品,根据色谱相对保留时间和质荷比信息对样品进行定性分析,以乐果二级离子扫描峰(125.0/79.0)面积为参照峰,建立以乐果为对照品,测定叠鞘石斛中乐果等三种农药残留量的GC-MS/MS方法。结果表明,乐果、敌敌畏、毒死蜱进样量在0.1~1.0 ng与它们的色谱峰面积有较好的线性关系,最低检出限(以进样量计)分别为1.399×10-2、2.279×10-4、1.757×10-4 ng;平均回收率分别为95.4%、95.0%、94.7%。该一测多评方法简单快速,定量准确,适用于叠鞘石斛中乐果、敌敌畏、毒死蜱农药残留的同时测定。

关键词: GC-MS/MS, 叠鞘石斛(Dendrobium aurantiacum), 乐果, 敌敌畏, 毒死蜱

Abstract: To establish a quantitative method for the simultaneous measurement of the residual level of three pesticides in Dendrobium aurantiacum by GC-MS/MS. The samples were extracted by acetonitrile and purify by Cleanert TPH column. The samples were then tested by GC-MS/MS. Information on relative retention time and mass charge ratio was used for qualitative analysis. The peak area obtained by secondary ion MS of dimethoate(125.0/79.0) was used as the reference peak to establish a method using dimethoate as the reference substance to determinate there sidual quantity of three pesticides in Dendrobium aurantiacum by GC-MS/MS. When the injection quantity of the sample containing dimethoatea, dichlorvos and chlorpyrifosis in the range of 0.1~1.0 ng, there is a good linear relationship between the injection quantity and peak area. Limit of quantification(LOQ) of dimethoate, dichlorvos and chlorpyrifos are 1.399×10-2、2.279×10-4、1.757×10-4 ng; The average recovery rates of dimethoate, dichlorvos and chlorpyrifos are 95.4%, 95.0% and 94.7%. the method is simple, accurate, rapid and is appropriate for the quantification of residual quantity of dimethoate,dichlorvos and chlorpyrifos in Dendrobium aurantiacum.

Key words: GC-MS/MS, Dendrobium aurantiacum, dimethoate, dichlorvos, chlorpyrifos

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