湖北农业科学 ›› 2018, Vol. 57 ›› Issue (1): 112-114.doi: 10.14088/j.cnki.issn0439-8114.2018.01.029

• 检测分析 • 上一篇    下一篇

加速溶剂萃取-气相色谱-质谱法检测土壤中染料母体偶氮苯和咔唑

张莉, 左海英, 张永涛, 桂建业, 张辰凌, 张琳, 李晓亚   

  1. 中国地质科学院水文地质环境地质研究所监测中心,河北 正定 050803
  • 收稿日期:2017-09-29 出版日期:2018-01-10 发布日期:2020-01-02
  • 通讯作者: 李晓亚,高级工程师,主要从事有机分析研究,(电子信箱)lixiaoya0527@126.com。
  • 作者简介:张 莉(1965-),女,河北保定人,高级工程师,主要从事化学分析研究,(电话)15803311506(电子信箱)zhangli202004@126.com
  • 基金资助:
    中国地质调查局地调项目(12120115055301)

Analysis of Pro-dyes Azobenzene and Carbazole by Accelerated Solvent Extraction and Gas Chromatography-mass Spectrometry

ZHANG Li, ZUO Hai-ying, ZHANG Yong-tao, GUI Jian-ye, ZHANG Chen-ling, ZHANG Lin, LI Xiao-ya   

  1. Institute of Hydrogeology and Environmental Geology,Chinese Academy of Geological Sciences,Zhengding 050803,Hebei,China
  • Received:2017-09-29 Online:2018-01-10 Published:2020-01-02

摘要: 建立了土壤中染料母体偶氮苯和咔唑加速溶剂萃取-在线净化检测方法。土壤经石英砂分散后,装入底部有氟罗里硅土粉和石墨炭黑粉的萃取池中,以丙酮-正己烷(V/V,1∶1)为溶剂用加速溶剂萃取仪萃取并同时完成净化,用DB-5MS柱分离,以气相色谱-质谱定性定量检测。考察了萃取溶剂、萃取温度、分散剂、土壤TOC及净化剂等因素的影响,对空白土壤样品进行3种浓度水平的加标试验,其平均回收率为72.0%~113.7%,相对标准偏差在7.6%~15.8%。此方法用于土壤样品的检测,部分样品中有偶氮苯和咔唑检出。

关键词: 偶氮苯, 咔唑, 气相色谱-质谱, 土壤, 在线净化

Abstract: A method that accelerated solvent extraction and in situ purification of pro-dyes,namely azobenzene and carbazole,was carried out in this research. A soil sample,mixed with some silica sand,was placed in the extract cell with fluorine silica powder and graphitized carbon powder;two objectives were extracted by acetone-hexane(VV,1∶1),and in situ purified in the accelerated solvent extractor. Then they were analyzed by gas chromatography-mass spectrometry using a DB-5MS column. We studied the influence of extracting solvent,temperature,dispersing agent,TOC content. Difference of in situ and off situ purification as well as superiority of composite purification was also discussed in this study. Spiked recoveries of three concentrations ranged from 72.0%~113.7% with relative standard deviation 7.6%~15.8%. Real sample analysis was constructed by this method, and some azobenzene and carbazole were detected.

Key words: azobenzene, carbazole, Gas Chromatography-mass Spectrometry, soil, in situ purification

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