人尿中12种多环芳烃代谢物的液相色谱-串联质谱同时测定法  

Simultaneous Determination of Twelve M etabolites of Polycyclic Aromatic Hydrocarbon in Human Urine by Liquid Chromatography-Tandem Mass Spectrometry Method

作　　者：郑磊[1] 丁昌明[1] 胡小键[1] 付慧[1] 金银龙[1] 林少彬[1] 

机构地区：[1]中国疾病预防控制中心环境与健康相关产品安全所,北京100021

出　　处：《环境与健康杂志》2011年第4期348-351,共4页Journal of Environment and Health

基　　金：国家"十一五"科技支撑项目(2006BAI19B01)

摘　　要：目的建立同时测定人体尿中12种羟基多环芳烃的液相色谱串联质谱(liquid chromatography-tandemmass spectrometry,LC-MS-MS)分析法。方法尿液经过酶解、固相萃取法纯化、富集以及浓缩,然后采用液相色谱串联质谱检测尿中12种(2-羟基萘、1-羟基萘、3-羟基芴、2-羟基芴、2-羟基菲、1-羟基菲、1-羟基芘、3-羟基、6-羟基、1-羟基苯并[a]蒽、9-羟基苯并[a]芘和3-羟基苯并[a]芘)多环芳烃代谢物。结果在0.002～177 ng/ml的线性范围内,所得回归方程线性关系良好,均r≥0.99。该方法的检出限为0.002～0.03 ng/ml,平均回收率为77.4%～132.1%,RSD为1.5%～11.8%。结论该方法灵敏度和精密度均较高,回收率和重复性良好,适用于人尿中12种羟基多环芳烃的同时检测。Objective To develop a method for simultaneous determination of twelve metabolites of polycyclic aromatic hydrocarbons（OH-PAHs） in human urine（2-hydroxynaphthalene,1-hydroxynaphthalene,3-hydoxyfluorene,2-hydoxyfluorene,2-hydroxyphenanthrene,1-hydroxyphenanthrene,1-hydroxypyrene,3-hydroxychrysene,6-hydroxychrysene,1-hydoxybenz [a] anthracene,9-hydoxybenz[a]pyrene and 3-hydoxybenz[a]pyrene） by liquid chromatography-tandem mass spectrometry（LC-MS-MS） method.M ethods The samples were hydrolyzed by enzyme first,then were purified and enriched by solid phase extraction,concentrated and determined with LC-MS-MS.Results The regression equations showed a good linearity in the range of 0.002-177 ng/ml and the correlation coefficients were not less than 0.99.The limits of detection of the method were between 0.002-0.03 ng/ml.The recovery rates were 77.4%-132.1% and the relative standard deviations were 1.5%-11.8%.Conclusion The established method is sensitive,reproducible with higher precision and better recoveries,and it is applicable to simultaneous determination of twelve metabolites of polycyclic aromatic hydrocarbons in human urine.

关 键 词：色谱法 液相 固相萃取 串联质谱 多环芳烃代谢物 尿液 

分 类 号：O657.6[理学—分析化学]