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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
引用本文:肖琼娜,霍霞,王远萍,吴库生,郭勇勇,徐锡金. 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[J]. 汕头大学医学院学报, 2011, 24(1): 23-25
作者姓名:肖琼娜  霍霞  王远萍  吴库生  郭勇勇  徐锡金
作者单位:汕头大学医学院分析细胞学实验室,广东 汕头,515041
基金项目: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。

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

Determination of Poly Brominated Diphenyl Ethers in Newborn Umbilical Cord Blood by Solid-phase Extraction and Gas Chromatography-mass Spectrometry
XIAO Qiong-na , HUO Xia , WANG Yuan-ping , WU Ku-sheng , GUO Yong-yong , XU Xi-jin. Determination of Poly Brominated Diphenyl Ethers in Newborn Umbilical Cord Blood by Solid-phase Extraction and Gas Chromatography-mass Spectrometry[J]. Journal of Shantou University Medical College, 2011, 24(1): 23-25
Authors:XIAO Qiong-na    HUO Xia    WANG Yuan-ping    WU Ku-sheng    GUO Yong-yong    XU Xi-jin
Affiliation:XIAO Qiong-na,HUO Xia,WANG Yuan-ping,WU Ku-sheng,GUO Yong-yong,XU Xi-jin(Analytical Cytology Laboratory,Shantou University Medical College,Shantou 515041,China)
Abstract:
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 o...
Keywords:polybrominated diphenyl ethers  umbilical cord blood  solid-phase extraction  gas chromatography-mass spectrometry  negative chemical ionization  
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