色谱

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

• 研究论文 • 上一篇    下一篇

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   

  1. 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
  • 收稿日期:2012-07-26 修回日期:2012-09-19 出版日期:2012-11-28 发布日期:2012-11-21
  • 通讯作者: 沈伟健,高级工程师. Tel: (025)52345193, E-mail: swj9722418@yahoo.com.cn.
  • 基金资助:

    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).

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

SHEN Weijian1*, CAO Xiaowen2, LIU Yijun1, ZHANG Rui1, FAN Xin1, ZHAO Zengyun1, SHEN Chongyu1, WU Bin1   

  1. 1. Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 2. Changzhou Entry-Exit Inspection and Quarantine Bureau, Changzhou 213022, China
  • Received:2012-07-26 Revised:2012-09-19 Online:2012-11-28 Published:2012-11-21

PDF

675

被引次数

33

摘要： 建立了气相色谱-负化学源质谱检测蔬菜中17种拟除虫菊酯类农药残留量的方法。样品中的目标物经乙腈提取后,用乙二胺-N-丙基甲硅烷(PSA)和石墨化炭黑填料进行分散固相萃取净化,气相色谱-负化学源质谱选择离子监测模式测定,同位素内标法定量。在甜豌豆、绿花菜和大葱基质中均未见干扰所有农药测定的现象。17种拟除虫菊酯类农药的定量限均为0.02～5 μg/kg。在10、20、30和100 μg/kg等4个添加水平下,所有农药的回收率均为71.0%～139.0%,相对标准偏差≤12.8%。该方法可作为蔬菜中17种菊酯类农残检测的确证方法。

关键词: 负化学离子源质谱, 拟除虫菊酯类农药, 气相色谱, 蔬菜

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 μg/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 μg/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.

Key words: negative chemical ionization mass spectrometry (NCI-MS), pyrethroid pesticides, vegetables, gas chromatography (GC)