湖北农业科学 ›› 2019, Vol. 58 ›› Issue (7): 108-110.doi: 10.14088/j.cnki.issn0439-8114.2019.07.025

• 检测分析 • 上一篇    下一篇

加速溶剂萃取-GC-MS检测土壤中萘及其取代衍生物

张莉, 李科, 刘佳, 张辰凌   

  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:2018-10-15 出版日期:2019-04-10 发布日期:2019-12-03
  • 通讯作者: 张辰凌,高级工程师,主要从事有机分析研究,(电子信箱)zhangchenling2011@126.com。
  • 作者简介:张 莉(1965-),女,河北保定人,高级工程师,主要从事有机分析研究,(电话)0311-88017401(电子信箱)zhangli202004@126.com
  • 基金资助:
    中国地质调查局地调项目(12120115055301)

Determination of naphthalene and its derivatives by using accelerated solvent extraction coupled with gas chromatography-mass spectrometry

ZHANG Li, LI Ke, LIU Jia,ZHANG Chen-ling   

  1. Institute of Hydrogeology and Environmental Geology,Chinese Academy of Geological Sciences,Zhengding 050803,Hebei,China
  • Received:2018-10-15 Online:2019-04-10 Published:2019-12-03

摘要: 建立了土壤中萘及其取代衍生物的加速溶剂萃取方法。土壤经石英砂分散后,装入加速溶剂萃取仪萃取池中,以二氯甲烷-丙酮(V/V,1∶1)为溶剂,在炉温100 ℃、压力10.342 2 MPa条件下萃取10 min。萃取液经过K-D浓缩后,用氟罗里硅土小柱净化,用DB-5MS柱分离,以气相色谱-质谱定性定量检测。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64.0%~102.6%,相对标准偏差为7.6%~15.2%。

关键词: 土壤, 萘及取代衍生物, 加速溶剂萃取, 气相色谱-质谱

Abstract: A method that accelerated solvent extraction of naphthalene and its derivatives was carried out in this research. A soil sample, mixed with some silica sand, was placed in the extract cell. Objectives were extracted by dichloromethane-acetone(VV,1∶1) at extraction temperature of 100 ℃ and extraction pressure of 10.342 2 MPa for 10 min. The eluent was purfied using florisil silica column after concentrated by K-D. Then naphthalene and its derivatives were analyzed by gas chromatography-mass spectrometry using a DB-5MS column. Spiked recoveries of three concentrations ranged from 64.0%~102.6% with relative standard deviation 7.6%~15.2%(n=7).

Key words: soil, naphthalene and its derivatives, accelerated solvent extraction, GC-MS

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