Wang Dongli, Jiang Guibin, Cai Zongwei
Department of Chemistry, Hong Kong Baptist University, Kowloon, Hong Kong SAR, China.
Talanta. 2007 Apr 30;72(2):668-74. doi: 10.1016/j.talanta.2006.11.038. Epub 2007 Jan 8.
A column chromatography procedure was developed for the clean-up of solvent-extracted sediment samples for the fractionation of polybrominated diphenyl ethers (PBDEs) and polybrominated dibenzo-p-dioxins and dibenzofurans (PBDD/Fs). The procedure included multiple column chromatography steps for clean-up for the separation of PBDEs from PBDD/Fs. The separation of the two chemical groups overcame the mutual interfering problem during the GC-ion trap MS analysis. The method was validated with the analysis of quality control samples. The method accuracy represented with relative error was less than 16% for all targeted PBDEs and PBDD/Fs congeners. Recoveries of the (13)C-labeled standards ranged from 64% to 117% with relative standard deviation from 7.3% to 15%. Results from the analysis of environmental sediment samples collected in the vicinity of a recycling site for electronic wastes showed high levels of PBDEs (1.5-12ng/g, dry weight), trace levels of PBDFs (0.025-0.92ng/g, dry weight) and non-detectable PBDDs.
开发了一种柱色谱法，用于净化溶剂萃取的沉积物样品，以分离多溴二苯醚（PBDEs）以及多溴二苯并 - 对 - 二恶英和二苯并呋喃（PBDD/Fs）。该方法包括多个柱色谱净化步骤，用于将PBDEs与PBDD/Fs分离。这两种化学物质组的分离克服了气相色谱 - 离子阱质谱分析过程中的相互干扰问题。该方法通过对质量控制样品的分析进行了验证。所有目标PBDEs和PBDD/Fs同系物以相对误差表示的方法准确度小于16%。（13）C标记标准物的回收率在64%至117%之间，相对标准偏差在7.3%至15%之间。对在电子废物回收站点附近采集的环境沉积物样品的分析结果表明，PBDEs含量较高（1.5 - 12ng/g，干重），PBDFs含量痕量（0.025 - 0.92ng/g，干重），未检测到PBDDs。
