|HE Yun-chen, GAO Li-rong, JIA Tian-qi, DENG Jing-lin, LIU Wen-bin.Determination of Dioxin from ChlorinatedParaffins Industrial Products by High Resolution Gas Chromatography High Resolution Mass Spectrometer with Isotope Dilution Method[J].Environmental Monitoring and Forewarning,2022,14(5):49-53
|氯化石蜡（CPs）作为一种用途广泛、产量大的有机氯化学工业品，具有组成多样、基质复杂等特点，对其中产生的二噁英（PCDD/Fs）检测是当前工作面临的难题。建立了同位素稀释高分辨气相色谱-高分辨质谱法检测CPs工业品中PCDD/Fs的分析方法。对样品净化过程进行了优化，通过提取溶剂筛选，去除固体CPs中部分基质，建立的双活性炭柱法可高效去除CPs基质。方法采用13 C12标记的PCDD/Fs内标物进行定性和定量分析。17种PCDD/Fs同系物的检出限为0.1～3 pg/g，回收率为31.7%～100%。该方法可对高纯度工业品中痕量持久性有机污染物进行高效的定性和定量分析，能够满足国家标准方法对PCDD/Fs检测的要求。
|关键词: 氯化石蜡 二噁英 化学工业品 同位素稀释法
|Determination of Dioxin from ChlorinatedParaffins Industrial Products by High Resolution Gas Chromatography High Resolution Mass Spectrometer with Isotope Dilution Method
HE Yun-chen, GAO Li-rong, JIA Tian-qi, DENG Jing-lin, LIU Wen-bin1,2,3
1.Research Center for EcoEnvironmental Sciences, Chinese Academy of Sciences, Beijing 100085, China;2.2.University of Chinese Academy of Sciences, Beijing 100049, China;3.Hangzhou Institute for Advanced Study, UCAS, Hangzhou, Zhejiang 310024, China
|Chlorinated paraffins, as a kind of industrial organochlorine chemical products with wide use and large yield, have the characteristics of diverse composition and complex matrix. The detection and analysis of dioxins produced unintentionally in chlorinated paraffins is a difficult problem in current work. A method for the determination of dioxins in chlorinated paraffins by isotope dilution high resolution gas chromatography high resolution mass spectrometry (HR-GC-HR-MS) was established. The purification process of samples was optimized, and part of the matrix in solid chlorinated paraffins was removed by solvent screening. The double activated carbon column method was established to efficiently remove the matrix of chlorinated paraffins. The solution to be tested was detected by high resolution gas chromatography high resolution mass spectrometry, and 13 C12 labeled dioxin internal standard was used for qualitative and quantitative analysis. The detection limits of 17 dioxins were 0.1～3 pg/g, and the recoveries of 13 C12 labeled dioxins were 31.7%～100%. This study can be used for the qualitative and quantitative analysis of trace persistent organic pollutants from high purity industrial products, which can meet the requirements of national standard methods for the detection of PCDD/Fs.
|Key words: Chlorinated paraffin Dioxin Chemical industrial products Isotope dilution