色谱

色谱 ›› 2013, Vol. 31 ›› Issue (9): 878-884.DOI: 10.3724/SP.J.1123.2013.02012

• 研究论文 • 上一篇    下一篇

同位素稀释气相色谱/三重四极杆串联质谱法分析环境样品中的多氯萘

刘芷彤1, 张兵1, 王雯雯2, 刘国瑞1,3, 高丽荣1, 郑明辉1   

  1. 1. 中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京 100085;
    2. 安捷伦科技(中国)有限公司, 北京 100102;
    3. 香港浸会大学化学系, 香港九龙塘
  • 收稿日期:2013-02-06 修回日期:2013-03-25 出版日期:2013-09-28 发布日期:2013-09-02
  • 通讯作者: 郑明辉
  • 基金资助:

    国家自然科学基金项目(21107123,21007084).

Determination of polychlorinated naphthalenes in environmental samples by isotope dilution gas chromatography-triple quadrupole mass spectrometry

LIU Zhitong1, ZHANG Bing1, WANG Wenwen2, LIU Guorui1,3, GAO Lirong1, ZHENG Minghui1   

  1. 1. State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China;
    2. Agilent Technologies (China) Inc., Beijing 100102, China;
    3. Department of Chemistry, Hong Kong Baptist University, Kowloon Tong, Hong Kong SAR, China
  • Received:2013-02-06 Revised:2013-03-25 Online:2013-09-28 Published:2013-09-02

PDF

357

被引次数

22

摘要：

采用稳定同位素标记的多氯萘(PCNs)同类物为内标,建立了同位素稀释气相色谱/三重四极杆串联质谱技术测定环境样品中20种高关注的PCNs同类物的方法。结果表明:PCNs同类物的校正曲线在0.5~200 μg/L范围内线性良好(R2>0.99),检出限(LOD)为0.04~0.48 μg/L,相对标准偏差(RSD)小于15%。采用基质加标法评价该方法对实际环境样品中PCNs测定的回收率为45.2%~87.9%。为验证方法的适用性,以河流沉积物和再生铝冶炼排放的烟道气样品为对象,利用所建立的方法测定了20种PCNs同类物,并将结果与高分辨气相色谱/高分辨质谱方法的测定结果进行了比对,两种方法测定结果的RSD为0.5%~41.4%,表明所建立的同位素稀释气相色谱/三重四极杆串联质谱方法可用于实际环境样品中PCNs的定性、定量分析。

关键词: 持久性有机污染物, 多氯萘, 环境样品, 气相色谱-三重四极杆串联质谱

Abstract:

An isotope dilution gas chromatography combined with triple quadrupole mass spectrometry (GC-MS/MS) method was established for the analysis of twenty polychlorinated naphthalenes (PCNs) congeners in environmental samples. The linear correlation coefficients (R2) of calibration curves were greater than 0.99 in the concentration range of 0.5-200 μg/L for all the twenty PCN congeners. The average relative response factors (RRF) were calculated based on a seven-point calibration for the twenty PCN congeners. The relative standard deviations (RSDs) of all the congeners were below 15% (n=7). The limits of detection (LOD) of the established method ranged from 0.04 to 0.48 μg/L for the twenty PCN congeners. The recoveries of matrix spiked samples ranged from 45.2% to 87.9%, and the RSDs ranged from 0.4% to 21.2%. The sediment samples and stack gas samples collected from secondary aluminum smelting were analyzed by the established method. The obtained results were also compared with the data analyzed by high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS) method. The comparison indicated that the data of the established method was in good agreement with those of HRGC/HRMS method with the RSDs of 0.5%-41.4%. Consequently, the established GC-MS/MS method can be applied to the determination of PCNs in environmental samples.

Key words: environmental samples, gas chromatography-triple quadrupole mass spectrometry, persistent organic pollutants, polychlorinated naphthalenes

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