厦门近海沉积物中PBDEs与PBBs残留的GC-NCI/MS和GC-ECD分析

Abstract

将气相色谱-负离子化学源-质谱法(gC-nCI/MS)和气相色谱-电子捕获检测法(gC-ECd)应用于分析沉积物中6种多溴联苯醚(PbdES)和5种多溴联苯(PbbS)残留。沉积物样品以V(正己烷)∶V(丙酮)=1∶1作为提取剂,采用索式提取法,提取液经酸性硅胶和中性硅胶层析柱净化和正己烷洗脱后,以PCb-103为内标物和gC-nCI-MS的选择离子监测方式(SIM)进行定性与定量分析,PbdE-209则采用gC-ECd法分析。平均加标回收率为93.3%--110.8%,相对标准偏差为1.2%--8.6%,方法检测限均小于0.20μg/kg(PbdE-209的方法检测限是7.74μg/kg),相关系数都大于0.9990。所分析沉积物样品中均含有微量的PbdE-99、Pbb-49和PbdE-209。

Soxhlet extraction was developed for the determination of six polybrominated diphenyl ethers and five polybrominated biphenyls in sediment.Hexane/actone(1∶1, V/V) was used as the extraction solvent and hexane as elution solvent,after the extraction was cleaned by the cartridge filling with acidic and neutral silica gel,the analysis of samples was accomplished by using gas chromatography with negative chemical ionization mass spectrometric detection(GC-NCI/MS) in the selected ion monitoring mode(SIM) and gas chromatography-electron capture detector,and with PCB-103 as internal standard(IS).The average recoveries of the spiked-samples ranged from 93.3% to 110.8% with relative standard deviations between 1.2% and 8.6%,the detection limit(MDL) was smaller than 0.20 μg/kg (the MDL was 7.74 μg/kg for PBDE-209),and the correlation coefficients were larger than 0.9990.PBDE-99、 PBB-49 and PBDE-209 were detected in all sediments.