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。
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.