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色谱-负离子化学源-质谱联用仪测定人体血液中多溴联苯醚
  • 期刊名称:分析化学,2007,35(7):1015-1017
  • 时间:0
  • 分类:O625.322[理学—有机化学;理学—化学]
  • 作者机构:[1]中国科学院广州地球化学研究所有机地球化学国家重点实验室,广东省环境资源与保护重点实验室,广州510640, [2]中国科学院研究生院,北京100039, [3]上海大学环境与化学工程学院,上海200072
  • 相关基金:本文系国家自然科学基金重大项目(No.40590392)和国家自然科学基金委与香港研究资助局联合科研项目(No.40318003)资助
  • 相关项目:低纬度地区电子废物POPs污染的地球化学与环境效应
中文摘要:

建立了血液样品中多溴联苯醚的分析方法。血液样品采用离心和分离,提取血清。血清经过正己烷和甲基叔丁基醚的混合溶液(体积比1:1)萃取,萃取前加入回收率指示物,然后经干燥得到脂肪重量;脂肪再经正己烷溶解、酸洗和酸性硅胶柱(硅胶与浓硫酸的重量比为2:1)净化后,加内标,进气相色谱-负化学离子源.质谱(GC-NCI-MS)联用仪,采用选择离子检测(SIM)法和内标法定性和定量。结果表明加标回收率为76.0%~106.0%;方法检出限0.01—0.1ng;仪器检出限为0.5~2.0Pg。该方法检测血液中8种多溴联苯醚的同系物,灵敏度高、重现性好和回收率良好,可用于人体血液样品的检测。

英文摘要:

A method was developed for the determination of seven congeners of polybrominated diphenyl ethers (PBDEs) in human blood by gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) in the selected ion monitoring mode. Human serum samples were extracted with hexane-methyl tert-butyl ether (MTBE) ( volume ratio is 1 : 1 ). The organic phases were washed with potassium chloride solution, followed by evaporation to dryness for gravimetric determination of extracted lipid content. Lipid was dissolved with n-hexane and washed with H2SO4, and then samples were cleaned up with a silica/sulfuric acid column (2:1 by weight). Internal standard was added prior to GC-MS analysis. The results indicate that the average recovery of the internal standard was from 76.0% to 106.0%. The detection limit of the method was in the range of 0.01 -0.1 ng; The detection limit of instrument was 0.5 -2.0 pg. The method for detection of eight PBDE congeners in human blood was sensitive, high reproducible with satisfied recoveries.

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