摘要
建立了气相色谱-质谱法(GC-MS)分析土壤中的18种多溴联苯(PBBs)和多溴联苯醚类(PBDEs)化合物的方法。利用快速溶剂萃取(ASE)技术和凝胶净化系统(GPC)进行土壤样品的前处理,13C标记物作为进样内标和替代标,采用电子轰击源气相色谱质谱法(GC-EI/MS)分析一溴至七溴代PBBs和PBDEs,负化学源气相色谱质谱法(GC-NCI/MS)分析八溴至十溴代PBBs和PBDEs,BDE-209的分析采用同位素稀释法。结果表明,各化合物的方法检出限为0.15～0.43 ng/g;BDE-209检出限为4.0 ng/g;土壤中各化合物加标回收率为43.8%～97.2%(n=22),RSD为18%～31%,可以满足土壤中PBBs和PBDEs的分析需要。此法适合于土壤调查等大量土壤样品的分析。
A gas chromatography-mass spectrometry（GC-MS） was used for the determination of 18 kinds of polybrominated diphenyl ethers（PBDEs） and polybromominated biphenyls（PBBs） in soils.The sample was extracted by accelerated solvent extraction（ASE） and cleaned up by gel permeation chromatographic technique（GPC）.13C-labeled PCB and PBDE were added as internal standard and surrogate compound for quantitative determination.GC-EI/MS was used to analyze low-brominated PBDEs and PBBs,while GC-NCI/MS was applied for high-brominated PBDEs and PBBs,including BB-209,BB-206,BB-194 and BDE-209.Isotope dilution method was used for the analysis of BDE-209 to obtain accurate data.The average recoveries were 43.8%-97.2%（n=22） and relative standard deviations were 18%-31%.The limit of detection（LOD） of all the compounds were 0.15-0.43 ng/g,and LOD of BDE-209 was 4.0 ng/g.The method is highly sensitive,accurate,and specific for the quantitative determination for PBBs and PBDEs in soil.Furthermore it is practically satisfied for a general survey employing the analytical method.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2011年第6期833-838,共6页
Chinese Journal of Analytical Chemistry
关键词
多溴联苯醚
多溴联苯
气相色谱质谱法
土壤
Polybrominated diphenyl ethers（PBDEs）
Polybromominated biphenyl（PBBs）
Gas chromatography mass spectrometry（GC-MS）
Soil
