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加压流体萃取-硅酸镁柱净化-气相色谱质谱法同时测定土壤中有机氯农药和多环芳烃

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刘彬, 闫强, 郭丽, 张明杰, 施敏芳, 贺小敏. 加压流体萃取-硅酸镁柱净化-气相色谱质谱法同时测定土壤中有机氯农药和多环芳烃[J]. 环境化学, 2019, (10): 2212-2221. doi: 10.7524/j.issn.0254-6108.2018112605
引用本文: 刘彬, 闫强, 郭丽, 张明杰, 施敏芳, 贺小敏. 加压流体萃取-硅酸镁柱净化-气相色谱质谱法同时测定土壤中有机氯农药和多环芳烃[J]. 环境化学, 2019, (10): 2212-2221. doi: 10.7524/j.issn.0254-6108.2018112605
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LIU Bin, YAN Qiang, GUO Li, ZHANG Mingjie, SHI Minfang, HE Xiaomin. Simultaneous determination of OCPs and PAHs in soil by GC-MSD with ASE and florisil SPE purification[J]. Environmental Chemistry, 2019, (10): 2212-2221. doi: 10.7524/j.issn.0254-6108.2018112605
Citation: LIU Bin, YAN Qiang, GUO Li, ZHANG Mingjie, SHI Minfang, HE Xiaomin. Simultaneous determination of OCPs and PAHs in soil by GC-MSD with ASE and florisil SPE purification[J]. Environmental Chemistry, 2019, (10): 2212-2221. doi: 10.7524/j.issn.0254-6108.2018112605
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加压流体萃取-硅酸镁柱净化-气相色谱质谱法同时测定土壤中有机氯农药和多环芳烃

  • 1. 湖北省环境监测中心站, 武汉, 430072;

  • 2. 黄石环境监测站, 黄石, 435000;

  • 3. 湖北省地质实验测试中心, 武汉, 430034

    • 通讯作者: 贺小敏, E-mail: 39208454@qq.com
  • 基金项目:

    2017年湖北省土壤污染防治专项资金（湖北省土壤污染网联评估与成因研究）资助.

Simultaneous determination of OCPs and PAHs in soil by GC-MSD with ASE and florisil SPE purification

  • 1. Hubei Environmental Monitoring Central Station, Wuhan, 430072, China;

  • 2. Huangshi Environmental Monitoring Station, Huangshi, 435000, China;

  • 3. Hubei Province Geological Experimental Testing Center, Wuhan, 430034, China

    • Corresponding author: HE Xiaomin, 39208454@qq.com
  • Fund Project: Supported by the 2017 Special Fund for Soil Pollution Control of Hubei Province(The Synthetic Evaluation and Cause Analysis of Soil Pollution in Hubei Province).

  • 摘要: 本研究通过对仪器定性定量、样品萃取和萃取液净化等环节的条件优化实验，建立了同时测定土壤中8种有机氯农药和15种多环芳烃的加压流体萃取-硅酸镁柱净化-气相色谱质谱分析方法.化合物方法检出限在0.4—3.2 μg·kg-1之间，测定下限在1.6—12.8 μg·kg-1之间；对化合物含量为0.1 mg·kg-1和0.5 mg·kg-1的土壤加标样品分别进行6次平行分析，回收率在61%—119%之间，测定结果的RSD在2.8%—21%之间；对相关土壤标准物质进行分析，测定结果均在化合物认定值与不确定度范围内.与其他方法相比，本法减少了萃取环节共萃物、降低了净化环节对干扰物的洗脱、有效排除了假阳性，且显著提高了工作效率.
    Abstract: A method for determination of OCPs and PAHs in soils by gas chromato- graphy/mass spectrometry with accelerated solvent extraction and florisil SPE purification was developed. The procedures of extraction and purification,as well as chromatographic and mass spectrometric parameters were optimized. Under the optimized conditions, the detection limits of target compounds were 0.4-3.2 μg·kg-1, and the quantitative lower limits were 1.6-12.8 μg·kg-1. The RSDs(n=6) of two concentration levels were 2.8%-21%, and the recoveries ranged from 61% to 119%. The determination results of soils standard reference materials were all satisfactory. Compared with other methods, the influence of interferent in extract liquid was less, the false positive was eliminated effectively and much higher operating efficiency was obtained in this method.
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  • 收稿日期:  2018-11-26

加压流体萃取-硅酸镁柱净化-气相色谱质谱法同时测定土壤中有机氯农药和多环芳烃

    通讯作者: 贺小敏, E-mail: 39208454@qq.com
  • 1. 湖北省环境监测中心站, 武汉, 430072;
  • 2. 黄石环境监测站, 黄石, 435000;
  • 3. 湖北省地质实验测试中心, 武汉, 430034
  • 收稿日期:  2018-11-26
基金项目:

2017年湖北省土壤污染防治专项资金（湖北省土壤污染网联评估与成因研究）资助.

摘要: 本研究通过对仪器定性定量、样品萃取和萃取液净化等环节的条件优化实验，建立了同时测定土壤中8种有机氯农药和15种多环芳烃的加压流体萃取-硅酸镁柱净化-气相色谱质谱分析方法.化合物方法检出限在0.4—3.2 μg·kg-1之间，测定下限在1.6—12.8 μg·kg-1之间；对化合物含量为0.1 mg·kg-1和0.5 mg·kg-1的土壤加标样品分别进行6次平行分析，回收率在61%—119%之间，测定结果的RSD在2.8%—21%之间；对相关土壤标准物质进行分析，测定结果均在化合物认定值与不确定度范围内.与其他方法相比，本法减少了萃取环节共萃物、降低了净化环节对干扰物的洗脱、有效排除了假阳性，且显著提高了工作效率.

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