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高分辨气相色谱/高分辨质谱联用测定大气降尘中的二噁英
Determination of Dioxins in Atmospheric Deposition by High Resolution Gas Chromatography/High Resolution Mass Spectrometry

作  者: ; ; ; ; ; ; ;

机构地区: 中国科学院广州地球化学研究所有机地球化学国家重点实验室

出  处: 《分析化学》 2006年第1期16-20,共5页

摘  要: 样品采取索氏抽提,抽提液依次经多段混合硅胶柱、氧化铝柱和硅胶柱净化后,采用同位紊稀释法和高分辨气相色谱/高分辨质谱联用仪(HRGC/HRMS)对其中的17个2,3,7,8-氯取代二噁英(PCDD/Fs)同系物进行了测定。研究结果表明,用本法4次分析二噁英标准溶液,其结果的RSD〈7.1%;回收率可达62%~103%;标准参考样品的分析结果与标准值基本吻合,3次实验结果的RSD≤15%;仪器检出限为2,3,7,8-TCDF0.1pg,2,3,7,8-TCDD 0.2pg,OCDD 0.8Pg;测定某降尘样品中二噁英,计算得降尘通量为14.02pg TEQm^-1day^-1。 A method was evaluated for the determination of seventeen 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in atmospheric deposition with isotope dilution-high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). Sample extracts were cleaned up successively through multi-layer silica gel, alumina and silica gel columns. Precise and recoveries of the entire procedure were evaluated by replicate analysis (n =4) of PCDD/Fs standard solutions, with RSD below 7.1% and the recoveries in the range of 62% - 103%. The method was also validated by replicate analysis ( n = 3) of certified reference material. The values determined were in agreement with those certified, and the RSD below 15%. The detection limits were o. 1 pg for 2,3,7,8-tetrachlorodibenzofuran, 0. 2 pg for 2,3,7,8- tetrachlorodibenzo-p-dioxin and 0. 8 pg for octachlorodibenzo-p-dioxin. PCDD/Fs were analyzed in an atmospheric deposition sample, with the deposition flux of 14.02 pg m-2 day-l toxicity equivalent.

关 键 词: 二噁英 高分辨气相色谱 高分辨质谱 大气降尘

领  域: [理学] [理学] [环境科学与工程]

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