色谱 ›› 2013, Vol. 31 ›› Issue (11): 1081-1086.DOI: 10.3724/SP.J.1123.2013.05005

• 研究论文 • 上一篇    下一篇

超声波提取-气相色谱法测定土壤中21种酚类化合物

杨丽莉, 王美飞, 胡恩宇, 刘晶, 吴丽娟   

  1. 南京市环境监测中心站, 江苏 南京 210013
  • 收稿日期:2013-05-02 修回日期:2013-07-20 出版日期:2013-11-28 发布日期:2013-12-05
  • 通讯作者: 杨丽莉
  • 基金资助:

    国家环境保护标准制修订项目(2009-1045);南京市建设委员会科技项目(200717J).

Determination of 21 phenolic compounds in soil by ultrasonic extraction-gas chromatography

YANG Lili, WANG Meifei, HU Enyu, LIU Jing, WU Lijuan   

  1. Nanjing Environmental Monitoring Center, Nanjing 210013, China
  • Received:2013-05-02 Revised:2013-07-20 Online:2013-11-28 Published:2013-12-05

摘要:

建立了超声波提取-气相色谱法同时测定土壤中21种酚类化合物的分析方法。用二氯甲烷和正己烷混合溶剂提取土壤中的酚类化合物,提取液经碱性水溶液分配净化,去除非酸性有机杂质,再酸化萃取酚类化合物,浓缩后采用气相色谱-氢火焰离子化检测器进行检测,外标法定量。以10 g土壤样品计,酚类化合物的检出限为0.01~0.06 mg/kg。实际样品添加回收试验的回收率为62.9%~111.4%,相对标准偏差为4.3%~24.0%(n=6),准确度和精密度均较好。结果表明:该法操作方便,净化效果好,可用于土壤中多种酚类化合物的测定。

关键词: 超声波提取, 酚类化合物, 气相色谱法, 土壤

Abstract:

An effective method was developed to determine phenolic compounds in soil by ultrasonic extraction-gas chromatography (GC). The soil sample was extracted with methylene dichloride-hexane (2:1, v/v) for 3 min with the extraction temperature lower than 50 ℃ for 3 times. The extract was purified by alkaline aqueous solution (pH >12), and the phenolic compounds were dissolved in aqueous solution. After the organic solution was discarded, the aqueous solution was adjusted to pH<3 and subsequently extracted with methylene dichloride-ethyl acetate (4:1, v/v) twice. The analytes were determined by GC-FID and quantified by external standard method. The limits of quantification for all tested phenolic compounds were 0.01-0.06 mg/kg in about 10 g soil samples. The recoveries were between 62.9% and 111.4% with the relative standard deviations (RSDs) in the range of 4.3%-24.0% (n=6). The results showed that this method is sensitive, accurate, and suitable for the determination of the 21 phenolic compounds in soil.

Key words: gas chromatography (GC), phenolic compounds, soil, ultrasonic extraction

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