加速溶剂萃取/凝胶渗透色谱净化/气相色谱-负化学离子源质谱测定生物样品中的四溴联苯醚  

DEVELOPMENT OF AN ANALYTICAL METHOD FOR MEASURING BDE-47 IN BIOLOGICAL SAMPLES USING ACCELERATED SOLVENT EXTRACTION-GEL PERMEATION CHROMATOGRAPHY PURIFICATION AND GAS CHROMATOGRAPHY/NEGATIVE CHEMICAL IONIZATION-MASS SPECTROMETRY

作　　者：王旭亮[1] 何欢[1] 李文超[1] 杨绍贵[1] 孙成[1] 

机构地区：[1]污染控制与资源化研究国家重点实验室,南京大学环境学院,南京210093

出　　处：《环境化学》2011年第6期1186-1191,共6页Environmental Chemistry

基　　金：国家重点基础研究发展计划(973)项目(2009CB421604)资助

摘　　要：建立了一种分析生物样品中四溴联苯醚(BDE-47)的方法.获得了优化的前处理条件和GC/MS检测条件,采用加速溶剂萃取(ASE)-凝胶渗透色谱(GPC)/多层硅胶-氧化铝复合柱净化,气相色谱-质谱(负化学离子源)(GC/NCI-MS)分析.以猪肝为基质的BDE-47加标回收率结果为77.3%—118.7%,相对标准偏差在1.9%—6.1%之间,方法检出限为0.081 ng·g-1(干重).实验结果证明,该方法不仅灵敏度高、线性范围广、重复性好、回收率高,而且自动化程度高、快速简便,完全满足生物样品中痕量BDE-47的分析要求.所建立的方法已用于4种生物样品中BDE-47的分析,检测结果可靠.An analytical method was developed for the determination of BDE-47 in biological samples.The optimum conditions for the pretreatment and the detection of samples were obtained using accelerated solvent extraction（ASE）,automated gel permeation chromatography（GPC） purification and GC/NCI-MS analysis.The method detection limit is 0.081 ng·g-1（dry weight）.In the swine liver matrix,the spike recovery of the method for BDE-47 was from 77.3% to 118.7% with the relative standard deviation of 1.9% to 6.1%.The results show that the method for detection of BDE-47 is not only of high sensitivity,wide linear range,high recovery and good reproducibility,but also of high automation,simplicity and rapidness.The developed analytical method has been applied successfully to the determination of BDE-47 in four biological samples.

关 键 词：生物样品 BDE-47 加速溶剂萃取 凝胶渗透色谱 气相色谱/负化学离子源质谱 

分 类 号：X830[环境科学与工程—环境工程]