旧机电产品中二噁英类多氯联苯的测定

Determination of Dioxin-Likepolychlorinated Biphenyls in Used Electric and Mechanical Products

建立了凝胶渗透色谱-流体自动净化系统净化-高分辨质谱测定电路板中的二噁英类多氯联苯（12种,PCB 77,81,126,169,105,114,118,123,156,157,167,189）残留的分析方法。样品冷冻粉碎后经索氏提取,再用凝胶渗透色谱和流体自动净化系统净化,最后浓缩。以HRGC/HRMS电压选择离子检测模式（VSIR）对样品中的PCBs进行定性分析,同位素稀释技术定量,该方法检测限可达到pg/g水平。12种化合物的标准曲线线性相关系数均大于0.9999,线性范围指标性0.5～800 ng/g;内标回收率64.9%～103.8%;方法检出限0.1pg/g。

A rapid,sensitive and accurate method has been developed for the determination of twelve dioxin-like polychlorinated biphenyls（PCBs） in electric and mechanical products by isotope dilution high resolution gas chromatography/high resolution mass spectrometry（HRGC/HRMS）.Dioxin-like PCBs was extracted from samples by Soxhlet extractor and purified by gel permeation chromatography（GPC）Fluid Management Systems（FMS）.Confirmation and quantitative analysis at pg/g level of PCBs was performed by HRGC/HRMS using voltage selective ion record（VSIR）mode.The recoveries of twelve isotopically labeled compound solution were found to be in the range of 64.9%～103.8%.The quantitative detection limits of the method for dioxin-like PCBs are 0.1 pg/g.