气相色谱-质谱联用法测定人体血清中的全氟辛酸  

Detection of perfluorooctanoic acid in serum by gas chromatogrphy-negative chemical ionization-mass spectrometry

作　　者：吴库生[1] 徐锡金[1] 刘俊晓[1] 郭勇勇[1] 李燕[1] 黄晋荣[1] 郑桂娜[1] 霍霞[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：《华南预防医学》2010年第5期5-10,共6页South China Journal of Preventive Medicine

基　　金：广东省科技计划项目(2009B030801308)

摘　　要：目的建立血清中全氟辛酸（PFOA）的气相色谱-负离子化学源-质谱联用分析方法。方法采用固相萃取法萃取人体血清中的PFOA,以全氟癸酸（PFDA）为内标物,萃取液及内标物与乙酰化试剂酯化反应后,采用气相色谱-负化学离子源-质谱法测定血清中全氟辛酸的含量,用内标法进行定量。应用建立的方法对来自电子垃圾拆解区汕头贵屿镇84例及作为对照的汕头潮南区57例的产妇血清样品进行了实际检测。结果方法的线性范围为1.0~1.0×105μg/L,线性相关系数r=0.998 267。平均回收率为91.9%~98.1%,相对标准偏差（RSD）为1.57%~5.17%,血清中全氟辛酸的检出限为0.2μg/L。应用此方法对来自电子垃圾拆解区的母体血清进行了PFOA检测,结果显示其中位浓度为1.70μg/L,高于对照组（0.87μg/L）（P〈0.01）。结论用气相色谱-质谱联用内标法结合衍生化技术定量分析血清中PFOA的浓度灵敏度高,分析速度快,适于血清PFOA含量的测定。Objective To establish a method of gas chromatography-negative chemical ionization-mass spectrometry（GC-NCI-MS） for measuring perfluorooctanoic acid（PFOA） in human serum.Methods Serum PFOA was extracted by a solid-phase method,and after reacting with an acetyl reagent,was quantified by GC-NCI-MS,with perflurodecanoic acid methyl ester as an internal standard.The procedure was applied to a study,where serum samples were collected from 84 postpartum mothers from an e-waste recycling area and from 57 postpartum mothers from a control area.Results The created calibration curve was linear over a concentration range from 1.0 μg/L to 1.0×105 μg/L with a correlation coefficient of 0.998 267.The average recovery rate of PFOA was 91.9%-98.1% and its coefficient of variation was 1.57 %-5.17 %.The limit of detectionwas 0.2 μg/L.The median of PFOA level in postpartum maternal sera from the e-waste recycling area was 1.70 μg/L,significantly higher than 0.87 μg/L from the control area（P0.01）.Conclusion The method of GC-NCI-MS,using internal standards and derivation techniques,is sensitive and fast in measuring PFOA in human serum.

关 键 词：碎片质谱法 全氟辛酸 血清 

分 类 号：O657.63[理学—分析化学]