尿中多环芳烃单羟基代谢产物的液相色谱-质谱测定方法研究  

Using HPLC-MS /MS method to analyze monohydroxy metabolites of PAHs in urine

作　　者：黄传峰[1] 闫慧芳[1] 潘祖飞[1] 戴宇飞[1] 牛勇[1] 王玉江[2] 郑玉新[1] 

机构地区：[1]中国疾病预防控制中心职业卫生与中毒控制所,北京100050 [2]北京市丰台区疾病预防控制中心

出　　处：《卫生研究》2010年第3期355-357,360,共4页Journal of Hygiene Research

基　　金：国家杰出青年基金项目(No.30625031);卫生公益行业科研专项(No.200802020)

摘　　要：目的建立同时测定尿液中萘、菲和芘的单羟基代谢产物1-羟基萘、2-羟基萘、3-羟基菲和1-羟基芘等的液相色谱-质谱检测方法。方法尿液样品经酶水解后,利用液液萃取进行净化提取,吹氮定容后进液相色谱质谱仪进行分析,利用内标标准曲线法对目标化合物进行定量。结果利用内标法进行定量分析,提高了方法的重现性和精密度,4种目标化合物的回收率在89.7%～103.0%范围内,批内和批间精密度分别在1.0%～4.2%和1.8%～5.8%范围内;1-羟基萘、2-羟基萘和1-羟基芘的检出限为0.2μg/L,3-羟基菲的检出限为0.1μg/L。结论液相色谱-质谱法灵敏度高,重现性和回收率好,适用于正常人群和多环芳烃暴露人群尿中1-羟基萘、2-羟基萘、3-羟基菲和1-羟基芘等多环芳烃代谢产物的检测。Objective To establish a HPLC-MS /MS method for the simultaneous determination of 4 monohydroxy metabolites of polycyclic aromatic hydrocarbons（PAHs） in urine,including 1-naphthol,2-naphthol,3-phenanthrol and 1-pyrenol）.Methods After being treated by enzymatic hydrolysis,urine samples were purified by liquid-liquid extraction,evaporated under nitrogen to constant volume and examined by HPLC-MS /MS.Target compounds were quantified by internal standard calibration curve.Results The reproducibility and precision were improved by internal standard calibration.The recovery of four target compounds were in the range of 89.7% 103.0%.The precision of intra-and inter-batch was 1.0%-4.2% and 1.8%-5.8% respectively.The limits of quantification was 0.2μg /L for 1-naphthol,2-naphthol and 1-pyrenol and the limits of quantification was 0.1μg /L for 3-phenanthrol.Conclusion The sensitivity,reproducibility and recovery of HPLC-MS /MS method were good for the analysis of 1-naphthol,2-naphthol,3-phenanthrol and 1-pyrenol in the urine of people on occupational and nonoccupational exposure to PAHs.

关 键 词：多环芳烃 尿液 基质效应 羟基萘 羟基菲 液相色谱质谱 

分 类 号：R972.6[医药卫生—药品]