色谱2011，Vol.29Issue(8)：743-749,7.DOI:10.3724/SP.J.1123.2011.00743
固相萃取-气相色谱-负化学源质谱法测定人血清中的多溴联苯醚
Determination of polybrominated diphenyl ethers in human serum using solid-phase extraction and gas chromatography coupled with negative chemical ionization mass spectrometry
摘要
Abstract
A simplified analytical method comprised of solid-phase extraction ( SPE) and gas chromatography coupled with negative chemical ionization mass spectrometry (GC-NCI/MS) has been developed for the determination of 10 polybrominated diphenyl ethers ( PBDEs) congeners in human serum. After the extraction by Oasis, HLB custom-made SPE cartridges, the lipids in serum were decomposed by concentrated sulfuric acid directly added on the SPE column. The solvent for protein cleanup and the SPE conditions, such as elution solvent and its volume were optimized. The recoveries of the PBDEs spiked in fetal bovine serum relative to internal standards were in the range of 78. 5% - 109.1% at five spiked levels (three spiked levels for BDE-209). The intra-day relative standard deviations (RSDs) were between 0. 3% and 7. 4%, while the inter-day ESDs were between 1. 42% and 14.1%. The limits of detection (LOD, S/N = 3) and the limits of quantification (LOQ, S/N = 10) were in the range of 0. 10 -0.27 ng/L and 0. 35 -0. 91 ng/L respectively for all PBDEs, except BDE-209. The LOQ (blank concentration value x 3) for BDE-209 was 7. 91 ng/L. The method was verified by accurate analysis of organic contaminant standard reference materials (SEM) 1957 and 1958. The results indicated that the proposed method is sensitive, accurate, fast, simple, low solvent consump-tion and suitable for the determination of tri- to deca-BDE in human serum.关键词
固相萃取/气相色谱-负化学源质谱/多溴联苯醚/血清Key words
solid-phase extraction (SPE)/ gas chromatography coupled with negative chemical ionization mass spectrometry (GC-NCI/MS)/ polybrominated diphenyl ethers ( PBDEs)/ serum分类
化学化工引用本文复制引用
黄飞飞,赵云峰,李敬光,吴永宁..固相萃取-气相色谱-负化学源质谱法测定人血清中的多溴联苯醚[J].色谱,2011,29(8):743-749,7.基金项目
国家“十一五”科技支撑计划项目(2007BAC27B02)、卫生公益性行业科研专项基金项目(200902009)和中国博士后科学基金项目(20090450459) （2007BAC27B02）
