色谱

色谱

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土壤中多环芳烃和酞酸酯类有机污染物气相色谱-质谱测定方法中的质量控制与质量保证

张利飞1, 黄业茹1*, 史双昕1, 周丽1, 董亮1, 张烃1, 曾良子2, 米方卓2, 邵丁丁1   

  1. 1. 国家环境分析测试中心, 国家环境保护二恶英污染控制重点实验室, 北京 100029; 2. 北京科技大学土木与环境工程学院, 北京 100083
  • 收稿日期:2010-01-14 修回日期:2010-02-14 出版日期:2010-05-28 发布日期:1980-09-25
  • 通讯作者: 黄业茹

Quality assurance/quality control for the determination of polycyclic aromatic hydrocarbons and phthalate esters in soils using gas chromatography-mass spectrometry

ZHANG Lifei1, HUANG Yeru1*, SHI Shuangxin1, ZHOU Li1, DONG Liang1, ZHANG Ting1, ZENG Liangzi2, MI Fangzhuo2, SHAO Dingding1   

  1. 1. State Environmental Protection Key Laboratory of Dioxin Pollution Control, National Research Center for Environmental Analysis and Measurement, Beijing 100029, China; 2. Civil & Environment Engineering School, University of Science & Technology Beijing, Beijing 100083, China
  • Received:2010-01-14 Revised:2010-02-14 Online:2010-05-28 Published:1980-09-25
  • Contact: HUANG Yeru

PDF

771

被引次数

40

摘要： 建立了气相色谱-质谱(GC-MS)测定土壤中多环芳烃(PAHs)和酞酸酯类(PAEs)有机污染物的方法。样品经加速溶剂萃取和超声萃取处理后,通过固相萃取或凝胶渗透色谱法进行净化,在选择离子监测模式下进行定量。通过全程序空白、空白加标回收、清洁土壤基质加标回收及有证标准参考物质比对等方式,对所建立的方法进行严格的质量控制和保证。16种PAHs和7种PAEs的方法检出限分别为0.13～2.2 μg/kg和0.19～0.52 μg/kg,平均加标回收率分别为41.5%～116.9%和90.7%~107.1%。本研究所建立的土壤中PAHs和PAEs的GC-MS快速分析方法及其质量控制措施可以为全国性土壤污染状况调查数据的科学性和准确性提供技术保障。

关键词: 多环芳烃, 气相色谱-质谱法, 酞酸酯类化合物, 土壤 , 质量保证, 质量控制

Abstract: A method for the determination of polycyclic aromatic hydrocarbons (PAHs) and phthalate esters (PAEs) in soil samples by gas chromatography-mass spectrometry (GC-MS) was developed. After extracted by accelerated solvent extraction or ultrasonic extraction by dichloromethane-hexane (1:1, v/v) and dichloromethane-acetone (1:1, v/v), respectively, the extracts were cleaned up by solid phase extraction and/or gel permeation chromatography. Quality control and quality assurance procedures were carried out with the methods of whole procedure blank, blank spike recovery, clean soil matrix spike recovery, and the comparison with reference materials. The method detection limits were 0.13~2.2 μg/kg and 0.19~0.52 μg/kg and the average recoveries were 41.5%~116.9%和90.7%~107.1% for the PAHs and the PAEs, respectively. The results showed that the method can meet the technical requirements on the soil sample test and analysis in the national survey of soil pollution.

Key words: phthalate esters, polycyclic aromatic hydrocarbons, quality assurance, quality control, soil , gas chromatography-mass spectrometry (GC-MS)