GC/MS法测定生物样品中多溴联苯醚类化合物

本研究建立了多溴联苯醚（PBDEs）生物样品分析方法,获得了优化的前处理条件、气相色谱和质谱检测条件.对定性定量方法及实验条件必须满足的要求进行了评价.通过质量控制（quality control, QC）对整个方法进行了验证.结果证明,本研究所建立的分析方法满足生物样品PBDEs测定的要求,回收率在50.5%～112.3%之间,回收率相对标准偏差在5.3%～9.9%之间,方法检测限在7.1～161.8 pg/g之间.在建立的方法基础上,测定了部分养殖和野生鱼类样品,测得的野生鳜鱼和鲫鱼以及2个养殖鲈鱼样品的结果分别为1.53、1.11、5.31和6.15 ng/g(干重),其中主要的同族体为BDE47.

Determination of Polybrominated Diphenyl Ethers (PBDEs) in Biota Using GC/MS Method

The aim of this study is to build a method of determining PBDEs in biota, and to gain the optimum condition of preparation of samples, and the best condition of Gas Chromatography (GC) and Mass Spectrometer (MS). Also, the requirements of quality, quantity and experimental condition were assessed. According to the validation of the quality control (QC), the results proved that the analytical method satisfied the requirements of the determination of PBDEs in biota. The recoveries were between 50.5% and 112.3%, of which the relative standard deviations were between 5.3% and 9.9%, and the limits of detection were between 7.1 and 161.8 pg/g. Based on the determination method, several bred and wild fishes were analyzed. The concentration of PBDEs in the wild Chinese perch and crucian carp and 2 bred weevers were 1.53, 1.11, 5.31, 6.15 ng/g(dry weight), respectively, and the most congener was BDE47.