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尿中多种多环芳烃代谢物同时测定的高效液相色谱-荧光检测法

Simultaneous Determination of Several Polycyclic Aromatic Hydrocarbon Metabolites in Human Urine by High-Performance Liquid Chromatography With Fluorescence Detection

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【作者】 王宇董玉莲范瑞芳盛国英傅家谟

【Author】 WANG Yu, DONG Yu-lian, FAN Rui-fang, et al. Guangdong Key Laboratory of Environment Protection and Resources Utilization, State Key Laboratory of Organic Geochemistry, Guangzhuo Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou, Guangdong 510640, China

【机构】 中国科学院广州地球化学研究所有机地球化学国家重点实验室中国科学院广州地球化学研究所有机地球化学国家重点实验室 广东广州510640广东广州510640

【摘要】 目的建立同时测定人尿中多种多环芳烃代谢物(PAHm)的高效液相色谱分析法。方法尿样经过酶解、固相萃取(SPE)法纯化、富集以及氮吹浓缩,然后采用高效液相色谱-荧光检测器检测尿中5种多环芳烃代谢物(PAHm):2-羟基萘、2-羟基芴、9-羟基菲、1-羟基芘以及3-羟基苯并(a)芘。结果2-羟基萘、2-羟基芴、9-羟基菲、1-羟基芘、3-羟基苯并穴a雪芘的检测限分别为1.65×10-3、0.550、0.084、0.032、0.132μg/L,线性范围分别为0.099~74.000、0.900~680.000、0.63~470.00、1.3~940.0、1.7~1200.0μg/L。回收率为29.41%~132.11%。日内RSD为1.01%~6.27%,日间RSD为2.23%~11.90%。结论该方法可同时检测尿中2-羟基萘、2-羟基芴、9-羟基菲、1-羟基芘、3-羟基苯并(a)芘,灵敏度、精密度高,重复性、回收率良好,可用于PAHs在人体内暴露的生物监测。

【Abstract】 Objective To develop a method for simultaneous determination of several metabolites of polycyclic aromatic hydrocarbons(PAH) in urine, i.e. 2-hydroxynaphthalene, 2-hydoxyfluorene, 9-hydroxyphenanthrene, 1-hydroxypyrene and 3-hydoxybenz[a]pyrene, by high-performance liquid chromatography (HPLC) with fluorescence detection (FLD). Methods The samples were hydrolyzed by enzyme first, then were purified and enriched by solid phase extraction (SPE), nitrogen dry, and then were determined with HPLC/FLD. Results Three samples were detected by this method. The detection limit were 1.65×10-3, 0.550, 0.084, 0.032 and 0.132 μg/L, and the linear ranges were 0.099-74.000, 0.900-680.000, 0.63-470.00, 1.3-940.0, 1.7-1200.0 μg/L for 2-hydroxynaphthalene, 2-hydoxyfluorene, 9-hydroxyphenanthrene, 1-hydroxypyrene, and 3-hydoxybenz[a]pyrene respectively. The recovery rates was 29.41%-132.11%. RSD within the day was 1.01%-6.27%. RSD between days was 2.23%-11.90%. Conclusion The established method for simultaneous detection of 2-hydroxynaphthalene, 2-hydoxyfluorene, 9-hydroxyphenanthrene, 1-hydroxypyrene, and 3-hydoxybenz[a]pyrene in human urine is sensitive, reproducible with high precision and good recoveries and suitable for the biomonitoring of PAH exposure.

【基金】 国家自然科学基金委员会与香港研究资助局联合科研资助基金项目(40318003);中国科学院广州地球化学研究所知识创新工程领域前沿项目(GIGCX-0311106)
  • 【文献出处】 环境与健康杂志 ,Journal of Environment and Health , 编辑部邮箱 ,2006年01期
  • 【分类号】X838
  • 【被引频次】37
  • 【下载频次】668
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