色谱

色谱

• 研究论文 • 上一篇    下一篇

气相色谱-电子轰击离子源质谱法分析卷烟和烟叶中29种农药的残留

邹西梅,林竹光*,彭淑女,陈招斌   

  1. Department of Chemistry and the Key Laboratory of Analytical Sciences of the Ministry of Education, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China
  • 收稿日期:2008-08-12 修回日期:2008-10-12 出版日期:2009-03-30 发布日期:1982-12-25
  • 通讯作者: 林竹光
  • 基金资助:
    国家基础科学人才培养基金项目(J0630429)

Determination of 29 pesticide residues in tobacco by gas chromatography-electron impact ionization mass spectrometry

ZOU Ximei, LIN Zhuguang*, PENG Shunü, CHEN Zhaobin   

  1. Department of Chemistry and the Key Laboratory of Analytical Sciences of the Ministry of Education, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China
  • Received:2008-08-12 Revised:2008-10-12 Online:2009-03-30 Published:1982-12-25
  • Contact: LIN Zhuguang

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790

被引次数

105

摘要： 开展了卷烟和烟叶中有机氯、有机磷和拟除虫菊酯3类29种农药残留的气相色谱-电子轰击离子源质谱(GC-EI/MS)的分析方法研究。优化与选择了卷烟和烟叶样品的前处理条件,样品经正己烷-丙酮(体积比为1∶1)混合提取剂超声提取、Florisil硅土和中性氧化铝双净化剂固相萃取柱净化、二氯甲烷-正己烷(体积比为95∶5)混合洗脱剂洗脱和浓缩后,以磷酸三苯酯(TPP)为内标物,采用GC-EI/MS的选择离子监测方式(SIM)进行定性和定量分析。当样品的加标水平为20,50,100 μg/kg时,加标回收率为70%～110%,相对标准偏差在2%～8%之间;除了甲氰菊酯、氯菊酯和溴氰菊酯的方法检出限(LOD)分别为1.85,1.74与2.54 μg/kg外,其余的26种农药的LOD均小于0.8 μg/kg;线性范围为5.0～500.0 μg/kg,相关系数都大于等于0.9994。此分析方法已成功地应用于卷烟和烟叶样品中3类29种痕量农药残留的分析

关键词: 拟除虫菊酯, 农药残留, 气相色谱-电子轰击离子源质谱, 烟草 , 有机磷, 有机氯

Abstract: A method was developed for rapid determination of 29 pesticide residues in tobacco based on gas chromatography coupled with electron impact ionization mass spectrometric detection (GC-EI/MS). After the optimization of different parameters, such as the extraction solvent, elution solvent, purificant, pesticides were extracted from tobacco with hexane-acetone (1∶1, v/v) in an ultrasonic bath, cleaned-up on a column, packed with Florisil and neutral alumina, eluted with dichloromethane-hexane (95∶5, v/v), and then determined by GC-EI/MS in the selected ion monitoring mode (SIM) with triphenyl phosphate (TPP) as internal standard. The recoveries were performed at 20, 50 and 100 μg/kg fortification levels for each pesticide, and the recoveries ranged from 70% to 110% with the relative standard deviations between 2% and 8%. The detection limits were less than 0.8 μg/kg for 26 pesticides except for the fenpropathrin, deltamethrin and permethrin. The method was linear over the range of 5.0-500.0 μg/kg with the correlation coefficients between 0.9994 to 0.9999. The method was successfully applied to the analysis of these pesticides in tobacco.

Key words: organochlorine, organophosphorous, pesticide residues, pyrethroid, tobacco , gas chromatography-electron impact ionization mass spectrometry (GC-EI/MS)