色谱

色谱 ›› 2010, Vol. 28 ›› Issue (12): 1137-1143.DOI: 10.3724/SP.J.1123.2010.01137

• 研究论文 • 上一篇    下一篇

固相萃取-三重串联四极杆气相色谱/质谱联用分析蔬菜中43种农药残留留

施家威*, 李继革, 王玉飞, 赵永纲   

  1. 宁波市疾病预防控制中心 宁波市毒物研究与控制重点实验室, 浙江 宁波 315010
  • 收稿日期:2010-08-10 修回日期:2010-10-08 出版日期:2010-12-28 发布日期:2010-08-28
  • 通讯作者: 施家威,硕士,主管技师,主要从事环境分析、理化分析研究. Tel: (0574)87274559, E-mail: shijw@nbcdc.org.cn.
  • 基金资助:

    宁波市重点实验室建设基金项目(2008A22002).

Analysis of 43 pesticide residues in vegetables using solid-phase extraction and gas chromatography-triple quadrupole mass spectrometry

SHI Jiawei*, LI Jige, WANG Yufei, ZHAO Yonggang   

  1. 宁波市疾病预防控制中心 宁波市毒物研究与控制重点实验室, 浙江 宁波 315010
  • Received:2010-08-10 Revised:2010-10-08 Online:2010-12-28 Published:2010-08-28
  • Contact: SHI Jia-Wei

PDF

812

被引次数

64

摘要： 建立了气相色谱/三重四极杆串联质谱同时分析蔬菜中43种农药残留的方法。采用乙腈提取样品中待测组分,经固相萃取法(SPE)净化后采用气相色谱/三重四极杆串联质谱在多反应监测(MRM)模式下进行外标法定量测定。分别对青菜进行3个水平(10、80、200 μg/kg)的加标回收试验,其回收率为62.2%～170.0%,其中36种农药的回收率为70.0%～120.0%。方法的相对标准偏差(RSD)小于18%,定量限(LOQ)为0.3～4.4 μg/kg。该分析方法背景干扰低,灵敏度高,适合蔬菜中多种农药及杀虫剂残留的测定。

关键词: 固相萃取, 农药残留, 气相色谱-串联质谱, 蔬菜

Abstract: A method for the simultaneous analysis of 43 pesticide residues in vegetables by gas chromatography coupled with triple quadrupole mass spectrometry (GC-QqQ-MS/MS) was developed and validated. The samples were extracted with acetonitrile, and then purified by solid-phase extraction (SPE). The detection of 43 pesticides was carried out by GC-QqQ-MS/MS in the multi-reaction monitoring (MRM) mode using external standard method. The overall recoveries determined at three spiked levels of 10, 80 and 100 μg/kg were 62.2%~170.0%, which in the recoveries of 36 pesticides were 70.0%~120.0%. The relative standard deviations (RSDs) were less than 18%. The limits of quantification (S/N≥10) were 0.3~4.4 μg/kg. The method possesses low background and high sensitivity. It can be applied to the routine analysis of the 43 pesticides in vegetables.

Key words: pesticide residues, solid-phase extraction, vegetables, gas chromatography-tandem mass spectrometry (GC-MS/MS)