色谱

色谱 ›› 2011, Vol. 29 ›› Issue (03): 228-233.DOI: 10.3724/SP.J.1123.2011.00228

• 研究论文 • 上一篇    下一篇

用于气相色谱和气相色谱-质谱测定植物样品中含氯有机污染物残留的样品前处理方法

佟玲, 杨佳佳, 吴淑琪*   

  1. 国家地质实验测试中心, 北京 100037
  • 收稿日期:2010-11-04 修回日期:2010-12-31 出版日期:2011-03-28 发布日期:2011-03-28
  • 通讯作者: 吴淑琪,研究员,主要研究方向为环境地球化学分析.
  • 基金资助:

    国家地质实验测试中心基本科研经费项目(No.2009CSJ03)和中国地质调查局地质调查工作项目(No.1212010816028).

Sample pretreatment for determination of chlorinated organic pollutants in plants by gas chromatography and gas chromatography-mass spectrometry

TONG Ling, YANG Jiajia, WU Shuqi*   

  1. National Research Center for Geoanalysis, Beijing 100037, China
  • Received:2010-11-04 Revised:2010-12-31 Online:2011-03-28 Published:2011-03-28

PDF

738

被引次数

30

摘要： 根据植物样品中的主要干扰物质,建立了用于气相色谱(GC)和气相色谱-质谱联用(GC-MS)测定植物样品中含氯有机污染物残留的样品前处理方法,有效提高了对植物样品中有机氯农药及多氯联苯检测的灵敏度。采用均质提取法对样品进行提取,考察了凝胶渗透色谱(GPC)和固相萃取(SPE)对提取液的净化效果。结果发现,采用GC测定目标物时,提取液需经GPC和SPE两次净化；而采用GC-MS测定目标物时,仅用SPE一次净化即可。该方法快速、经济、灵敏,适合多种植物样品中有机污染物残留分析的样品前处理要求。

关键词: 多氯联苯, 气相色谱, 气相色谱-质谱, 样品前处理, 有机氯农药, 植物

Abstract: The sample pretreatment methods for the determination of chlorinated organic pollutants in plants by gas chromatography (GC) and GC-mass spectrometry (MS) were established. The homogeneous extraction was used to extract the chlorinated organic pollutants from plants. The main interferences in the co-extract from several kinds of plant samples were recognized. The sensitivity of the analysis on organochlorine pesticides and polychlorinated biphenyls (PCB) in plant samples was effectively improved. The removal efficiency of the interferences from the extract by gel permeation chromatography (GPC) and solid-phase extraction (SPE) was investigated. The impurities such as fatty acids and phenols can be cleaned-up through a Carb/NH2 SPE column with 20 mL mixed solvent of hexane-ethyl acetate (8:2, v/v) in 3% toluene as the eluent, and the recoveries were higher than 74%. It was necessary to combine GPC with SPE as the clean-up method when the sample was determined by GC, and only the SPE as the clean-up method was used if a mass spectrometer was employed as a detector. The methods are rapid and sensitive, and can be used in the analysis of organic pollutant residues in plant samples efficiently.

Key words: organochlorine pesticides, plants, polychlorinated biphenyls (PCB), sample pretreatment, gas chromatography (GC), gas chromatography-mass spectrometry (GC-MS)