Liu Hanxia, Zhang Qinghua, Song Maoyong, Jiang Guibin, Cai Zongwei
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, PR China; Dioxin Analysis Laboratory, Hong Kong Baptist University, Kowloon, Hong Kong, China.
Talanta. 2006 Aug 15;70(1):20-5. doi: 10.1016/j.talanta.2005.11.051. Epub 2006 Jan 6.
A comprehensive method was developed for quantitative analysis of polybrominated diphenyl ethers (PBDEs), polychlorinated biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins and dibenzo-furans (PCDD/Fs) in one single extract of environmental samples. The sample preparation procedure included two fractionation steps using silver nitrate silica chromatography to separate PBDEs from PCBs and PCDD/Fs and florisil column to separate PCBs from PCDD/Fs. Acidic silica, acidic alumina and gel permeation chromatography (GPC, for PCBs) or activated carbon column (for PCDD/Fs) were used for further clean-up. The sample extracts were analyzed by using high-resolution gas chromatography/high-resolution mass spectrometry. The entire method was validated from the analysis of mixed standards of PBDEs, PCBs and PCDD/Fs (n=3); the analysis of certified reference biota (WMF-01). The method was applied for the analysis of 10 sediment samples collected from Haihe River and Dagu Drainage River in Tianjin City. No significant PBDEs pollution was found in the areas.
开发了一种综合方法，用于对环境样品的单一提取物中的多溴二苯醚（PBDEs）、多氯联苯（PCBs）以及多氯二苯并对二恶英和二苯并呋喃（PCDD/Fs）进行定量分析。样品制备程序包括两个分馏步骤，使用硝酸银硅胶色谱法将PBDEs与PCBs和PCDD/Fs分离，以及使用弗罗里硅土柱将PCBs与PCDD/Fs分离。酸性硅胶、酸性氧化铝和凝胶渗透色谱法（用于PCBs）或活性炭柱（用于PCDD/Fs）用于进一步净化。样品提取物通过高分辨率气相色谱/高分辨率质谱法进行分析。整个方法通过对PBDEs、PCBs和PCDD/Fs混合标准品（n = 3）的分析以及对认证参考生物群（WMF - 01）的分析进行了验证。该方法应用于对从天津市海河和大沽排污河采集的10个沉积物样品的分析。在这些区域未发现明显的PBDEs污染。
