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气相色谱-负化学源质谱法测定蔬菜中17种拟除虫菊酯类农药残留量

沈伟健 曹孝文 刘一军 张睿 范欣 赵增运 沈崇钰 吴斌

色谱2012,Vol.30Issue(11):1172-1177,6.
色谱2012,Vol.30Issue(11):1172-1177,6.DOI:10.3724/SP.J.1123.2012.07044

气相色谱-负化学源质谱法测定蔬菜中17种拟除虫菊酯类农药残留量

Determination of 17 pyrethroid pesticide residues in vegetables by gas chromatography-mass spectrometry with negative chemical ionization

沈伟健 1曹孝文 2刘一军 1张睿 1范欣 1赵增运 1沈崇钰 1吴斌1

作者信息

  • 1. 江苏出入境检验检疫局食品实验室,江苏南京210001
  • 2. 常州出入境检验检疫局,江苏常州213022
  • 折叠

摘要

Abstract

A method was established for the determination of 17 pyrethroid pesticide residues in vegetables using QuEChERS (quick, easy, cheap, effective, rugged and safe) clean-up method and gas chromatography-mass spectrometry (GC-MS) with negative chemical ionization (NCI). The pyrethroid pesticides in the sample were extracted with acetonitrile. After QuEChERS clean-up with a mixture of primary secondary amine and graphitized carbon black packings, the extract was analyzed by GC-NCI-MS in selected ion monitoring (SIM) mode. An isotope internal standard of cypermethrin was employed to the quantification. The limits of quantification ranged from 0. 02 to 5 jig/kg. The recoveries of the pyrethroid pesticides spiked in three different matrixes (peas, broccoli and Chinese onion green) at four spiked levels of 10, 20, 30 and 100 (ig/kg were from 71.0% to 139. 0%, and the relative standard deviations were less than 12. 8%. This method can be used as a conclusive evidence method of the 17 pyrethroid pesticide residues in vegetables.

关键词

气相色谱/负化学离子源质谱/拟除虫菊酯类农药/蔬菜

Key words

gas chromatography (GC) / negative chemical ionization mass spectrometry (NCI-MS) / pyrethroid pesticides/ vegetables

分类

化学化工

引用本文复制引用

沈伟健,曹孝文,刘一军,张睿,范欣,赵增运,沈崇钰,吴斌..气相色谱-负化学源质谱法测定蔬菜中17种拟除虫菊酯类农药残留量[J].色谱,2012,30(11):1172-1177,6.

基金项目

国家质量监督检验检疫总局科技计划项目(2011KJ39,2012KJ31)和科技部科技支撑项目(2011BAK10B04). (2011KJ39,2012KJ31)

色谱

OA北大核心CSCDCSTPCDMEDLINE

1000-8713

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