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冰川冻土 ›› 2023, Vol. 45 ›› Issue (1): 267-276.doi: 10.7522/j.issn.1000-0240.2023.0020

• 冰冻圈技术 • 上一篇    下一篇

基于气相色谱-四级杆串联飞行时间质谱联用法测定积雪中28种多氯联苯

郝琳瑶1(), 步小敏1, 牟臻1, 浦伟2, 王鑫1,2, 付晓丽1()   

  1. 1.天津大学 地球系统科学学院,天津 300072
    2.兰州大学 大气科学学院,甘肃 兰州 730000
  • 收稿日期:2022-01-17 修回日期:2022-05-25 出版日期:2023-02-28 发布日期:2023-02-25
  • 通讯作者: 付晓丽 E-mail:haolinyao@tju.edu.cn;fuxiaoli@tju.edu.cn
  • 作者简介:郝琳瑶,硕士研究生,主要从事积雪中持久性有机污染物研究. E-mail: haolinyao@tju.edu.cn
  • 基金资助:
    国家自然科学基金项目(42025102)

Determination of 28 kinds of polychlorinated biphenyls in snow based on gas chromatography-quadrupole tandem time-of-flight mass spectrometry

Linyao HAO1(), Xiaomin BU1, Zhen MU1, Wei PU2, Xin WANG1,2, Xiaoli FU1()   

  1. 1.School of Earth System Science,Tianjin University,Tianjin 300072,China
    2.College of Atmospheric Sciences,Lanzhou University,Lanzhou 730000,China
  • Received:2022-01-17 Revised:2022-05-25 Online:2023-02-28 Published:2023-02-25
  • Contact: Xiaoli FU E-mail:haolinyao@tju.edu.cn;fuxiaoli@tju.edu.cn

摘要:

多氯联苯(PCBs)是一类典型持久性有机污染物(POPs),在环境中长期存留并通过多种环境介质进行远距离迁移,对环境安全及人类健康具有严重危害。已有研究表明PCBs在大气中广泛存在,但在积雪中PCBs的浓度极低,大量积雪样品采集给分析研究带来困难。为了探究积雪中PCBs的含量及分布特征,本研究首先建立了基于气相色谱-四级杆串联飞行时间质谱(GC-QTOF/MS)测定积雪中28种PCBs的方法,利用优化高分辨气质联用仪参数,在较少样品量(1~2 L)情况下实现积雪中PCBs的定量分析。通过比较PCBs在不同离子源下的定性定量参数,最终发现电子轰击离子源最优,并进一步对发射电流进行优化,提高了仪器灵敏度。结果表明:28种PCBs标准样品在0.05~10 μg·L-1浓度范围内线性关系良好,相关系数为0.993~0.999;在低、中、高三种不同浓度水平下,28种PCBs回收率为60.2%~103.2%,相对标准偏差为0.9%~14.0%(n=3);方法检出限为1.01~2.92 pg·L-1,可满足实际样品分析检测的需求,为进一步分析积雪中污染物分布特征提供了依据。此外,通过对我国东北典型地区积雪中PCBs的分析发现,积雪中PCBs以五、六氯联苯为主要组成,含量较高的PCB单体为PCB81、128、126及169,结合已有研究初步推断积雪中PCBs的污染除与PCB历史生产、残留有关外,还与燃烧与热工业过程等有关。

关键词: GC-QTOF/MS, 积雪, 多氯联苯

Abstract:

Polychlorinated biphenyls (PCBs) are typical components of persistent organic pollutants (POPs) with long-term retention, bioaccumulation, semi-volatility and high toxicity. PCBs can exist in the environment for a long time and migrate over long distances through a variety of environmental media, which result in serious threaten to environmental safety and human health. Snow is considered an almost ideal depositing medium for assessing atmospheric deposition. Previous studies have shown that PCBs exist widely in the atmosphere, but the concentration of PCBs in snow is extremely low, and the collection of a large number of snow samples brings difficulties to analysis and research. In order to explore the content and distribution characteristics of PCBs in snow, this study first established a method for the determination of 28 PCB congeners in snow based on gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF/MS). The quantitative analysis of PCBs in snow was achieved with a small sample volume (1~2 L) by optimizing the parameters of high-resolution GC-MS. By comparing the qualitative and quantitative parameters of PCBs under different ion sources, it was finally found that the electron bombardment ion source was optimal, and the emission current was further optimized to improve the sensitivity of the instrument. The results showed that the PCBs standard samples had a good linear relationship within the concentration of 0.05~10 μg·L-1, and the correlation coefficient was in the range of 0.993~0.999. At three spiked levels, the recoveries of PCBs were 60.2%~103.2%, the relative standard deviations were 0.9%~14.0% (n=3), and the detection limit of the method was 1.01~2.92 pg·L-1. This method can be applied to the analysis of snow samples, which provides a basis for further analysis of the distribution characteristics of pollutants in snow. In addition, through the analysis of PCBs in snow in typical areas of Northeast China, it was found that PCBs in snow were mainly composed of pentachlorobiphenyl and hexachlorobiphenyl, and the PCB monomers with higher content were PCB81, 128, 126 and 169. The study preliminarily concluded that the pollution of PCBs in snow is not only related to the historical production and residues of PCBs, but also related to combustion and thermal industrial processes.

Key words: GC-QTOF/MS, snow cover, polychlorinated biphenyls

中图分类号: 

  • P426.63+5