固相萃取和气相色谱-质谱联用法检测脐带血中的多溴联苯醚  

Determination of Poly Brominated Diphenyl Ethers in Newborn Umbilical Cord Blood by Solid-phase Extraction and Gas Chromatography-mass Spectrometry

作　　者：肖琼娜[1] 霍霞[1] 王远萍[1] 吴库生[1] 郭勇勇[1] 徐锡金[1] 

机构地区：[1]汕头大学医学院分析细胞学实验室,广东汕头515041

出　　处：《汕头大学医学院学报》2011年第1期23-25,共3页Journal of Shantou University Medical College

基　　金：国家自然科学基金资助课题(30972513);教育部博士点基金资助课题(200805600004)

摘　　要：目的:改进新生儿脐带血中多溴联苯醚(PBDEs)的分析方法。方法:取2 mL脐血血清加入2 mL甲酸和100μL乙腈,漩锅、超声;将混合物经过固相萃取柱萃取及酸性硅胶柱净化,再利用带负化学源的气相色谱-质谱(GC-MS)联用仪,采用选择离子监测法和外标法对样品进行分析定量。结果:在0.5～32.0 ng/mL范围内,该方法所得的回归方程线性关系良好,相关系数均>0.997,加标回收率80.0%～110.0%;方法检出限0.01～0.07 ng/g,相对标准偏差5.3%～9.8%。样本回收率86.4%～93.7%。结论:用固相萃取和GC-MS法检测新生儿脐带血中PBDEs的同系物,更省时、灵敏、精确,且重复性和回收率较好。Objective：To improve the analytical method of the poly brominated diphenyl ethers（PBDEs）in newborn umbilical cord blood.Method：The formic acid and acetonitrile were added in 2 mL serum,vortexed and ultrasonic processed.The mixture was extracted by solid-phase extraction and cleaned-up with a silica/sulfuric acid column.Samples were analyzed by gas chromatograph-mass spectrometry（GC-MS）with negative chemical ionization,operated in selected ion monitoring mode and external standard method for quantification of PBDEs.Results： The concentration had a good linear range（0.5～32.0 ng/mL）,the correlation coefficient was above 0.997.The average recovery of the internal standard was from 80.0% to 110.0%.The detection limit of the method was within range of 0.01 to 0.07 ng/g.The average recovery of the samples and the relative standard deviation of the method were 86.4%～93.7% and 5.3%～9.8% respectively.Conclusion： Determination of PBDEs in newborn umbilical cord blood by solid-phase extraction and GC-MS.This method is fast、sensitive,high reproducible with satisfied recoveries.

关 键 词：多溴联苯醚 脐带血 固相萃取 气相色谱-质谱 负离子化学源 

分 类 号：R446.1[医药卫生—诊断学]