凝胶渗透色谱-硅胶柱-气相色谱-负化学离子源质谱测定生物介质中49种BFRs类化合物

Analysis of 49 BFRs in Biological Medium by Gas Chromatography-mass Spectrometry-negative Chemical Ionization with Gel Permeation Chromatography and Silica-gel Column

建立了生物介质内22种多溴联苯（ PBBs）和27种多溴联苯醚（ PBDEs）的净化和分析方法。通过分析不同时间段凝胶渗透色谱（ GPC）洗脱液中49种化合物含量，得出不同化合物凝胶色谱洗脱曲线。样品经过凝胶渗透色谱-混合硅胶柱净化后，再使用GC-（ NCI）/MS对样品进行检测。实验结果表明，PBBs和PBDEs检出限分别为0.02～0.88 pg/g和0.01～74.00 pg/g。对实验过程进行验证发现，样品不同浓度加标回收率为80％～120％，相对标准偏差小于20％。该方法具有良好的净化效果、准确度和精密度，拥有良好的线性范围及检出限，满足生物介质中溴代阻燃剂的检测分析实际要求。

A method has been developed for the clean-up and determination of 22 polybrominated biphenyls （ PBBs ） and 27 polybrominated diphenyl ethers （ PBDEs） in biological medium. The eluting profiles of 49 compounds were established according to the results of GC quantitation with the eluted liquids in different collecting time. The samples were purified using gel permeation chromatography （ GPC） to eliminate most of the lipids and waxes. Multi-layer silica gel was further used to remove the pigments. The quantitative analysis was performed with GC-（ NCI ）/MS for polybrominated biphenyls and polybrominated biphenyl ethers. The limits of detection of 22 PBBs were in range of 0.02-0.88 ng/L, while 27 PBDEs were in range of 0.01-74.00 ng/L. The average fortified and coefficients of variation of the method were determined. The results showed that recoveries were between 80%-120% and the relative standard deviations were less than 20%. This method is precise, sensitive and highly efficient in extraction. After routine applications, the results indicated that this method is suitable for the determination of BFRs contents in the biological medium.