高效液相色谱-荧光检测法同时测定健康人群尿液中7种羟基多环芳烃

张磊; 方波; 王宏伟; 杨泽; 李娜; 赵玉琦; 郝玉兰; 王曼曼; 王茜

doi:10.7524/j.issn.0254-6108.2018121301

环境化学

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张磊, 方波, 王宏伟, 杨泽, 李娜, 赵玉琦, 郝玉兰, 王曼曼, 王茜. 高效液相色谱-荧光检测法同时测定健康人群尿液中7种羟基多环芳烃[J]. 环境化学, 2019, (11): 2435-2442. doi: 10.7524/j.issn.0254-6108.2018121301

引用本文:

ZHANG Lei, FANG Bo, WANG Hongwei, YANG Ze, LI Na, ZHAO Yuqi, HAO Yulan, WANG Manman, WANG Qian. Simultaneous determination of seven hydroxyl polycyclic aromatic hydrocarbons in urine of healthy people by high performance liquid chromatography-fluorescence detection[J]. Environmental Chemistry, 2019, (11): 2435-2442. doi: 10.7524/j.issn.0254-6108.2018121301

Citation:

ZHANG Lei, FANG Bo, WANG Hongwei, YANG Ze, LI Na, ZHAO Yuqi, HAO Yulan, WANG Manman, WANG Qian. Simultaneous determination of seven hydroxyl polycyclic aromatic hydrocarbons in urine of healthy people by high performance liquid chromatography-fluorescence detection[J]. Environmental Chemistry, 2019, (11): 2435-2442. doi: 10.7524/j.issn.0254-6108.2018121301

高效液相色谱-荧光检测法同时测定健康人群尿液中7种羟基多环芳烃

华北理工大学公共卫生学院, 唐山, 063210

通讯作者: 王茜, E-mail: wwqq517@aliyun.com

基金项目:
河北省自然科学基金（H2017209232）和河北省卫生计生委项目（20170893）资助.

Simultaneous determination of seven hydroxyl polycyclic aromatic hydrocarbons in urine of healthy people by high performance liquid chromatography-fluorescence detection

School of Public Health, North China University of Science and Technology, Tangshan, 063210, China

Corresponding author: WANG Qian, wwqq517@aliyun.com

Fund Project: Supported by the Natural Science Foundation of Hebei Province, China (H2017209232) and the Research Foundation of Health and Family Planning Commission of Hebei (20170893).

摘要: 基于固相萃取-高效液相色谱-荧光检测法（SPE-HPLC-FLD），建立了同时测定健康人群尿液中7种羟基多环芳烃（OH-PAHs）的分析方法.10 mL酶解后的尿液样品经固相萃取净化富集.实验中考察了淋洗液、洗脱液和洗脱体积对萃取效率的影响.在最优条件下，7种OH-PAHs在各自范围内线性关系良好且相关系数（r）大于0.9970.方法检出限（S/N=3）和定量限（S/N=10）分别为0.04—4.96 ng·mL^-1和0.10—15 ng·mL^-1，日内（n=3）和日间（n=3）相对标准偏差分别为1.4%—8.9%和3.2%—11.5%.用该方法对40份健康人群尿液样品进行测定，OH-PAHs检出率为20.0%—100.0%，平均回收率在88.5%—102.7%之间.该方法操作简单、灵敏、准确，可应用于尿液中羟基多环芳烃的测定.
- 固相萃取 /
- 高效液相色谱 /
- 健康人群 /
- 尿液 /
- 羟基多环芳烃
Abstract: A method based on C₁₈ solid phase extraction (SPE) coupled with high performance liquid chromatography-fluorescence detection (SPE-HPLC-FLD) was developed for the simultaneous determination of seven hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs) in urine of healthy people. The 10 mL enzymatic hydrolyzed urine sample was purified and enriched by SPE process. The parameters influenced on SPE extraction efficiency such as the washing solvent, eluting solvent and eluting volume were investigated in detail. Under the optimized conditions, the method gave good linear ranges with the correlation coefficients (r) higher than 0.9970. The detection limits (S/N=3) and the quantification limits (S/N=10) were in the ranges of 0.04-4.96 ng·mL^-1 and 0.10-15.00 ng·mL^-1, respectively. The relative standard deviations of intra-day (n=3) and inter-day (n=3) were 1.4%-8.9% and 3.2%-11.5%, respectively. The developed method was applied to monitor the OH-PAHs in urine samples of 40 healthy people. The detection rate of seven target OH-PAHs was 20.0%-100.0% and the average recoveries at three spiked levels were 88.5%-102.7%. The method could be applied for the determination of OH-PAHs in urine of healthy people in a simple, sensitive and accurate way.
- solid-phase extraction (SPE) /
- high performance liquid chromatography (HPLC) /
- healthy people /
- urine /
- hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs)

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高效液相色谱-荧光检测法同时测定健康人群尿液中7种羟基多环芳烃

通讯作者: 王茜, E-mail: wwqq517@aliyun.com

华北理工大学公共卫生学院, 唐山, 063210

收稿日期: 2018-12-13

基金项目:

河北省自然科学基金（H2017209232）和河北省卫生计生委项目（20170893）资助.

关键词:

摘要: 基于固相萃取-高效液相色谱-荧光检测法（SPE-HPLC-FLD），建立了同时测定健康人群尿液中7种羟基多环芳烃（OH-PAHs）的分析方法.10 mL酶解后的尿液样品经固相萃取净化富集.实验中考察了淋洗液、洗脱液和洗脱体积对萃取效率的影响.在最优条件下，7种OH-PAHs在各自范围内线性关系良好且相关系数（r）大于0.9970.方法检出限（S/N=3）和定量限（S/N=10）分别为0.04—4.96 ng·mL^-1和0.10—15 ng·mL^-1，日内（n=3）和日间（n=3）相对标准偏差分别为1.4%—8.9%和3.2%—11.5%.用该方法对40份健康人群尿液样品进行测定，OH-PAHs检出率为20.0%—100.0%，平均回收率在88.5%—102.7%之间.该方法操作简单、灵敏、准确，可应用于尿液中羟基多环芳烃的测定.

English Abstract

Simultaneous determination of seven hydroxyl polycyclic aromatic hydrocarbons in urine of healthy people by high performance liquid chromatography-fluorescence detection

Corresponding author: WANG Qian, wwqq517@aliyun.com

School of Public Health, North China University of Science and Technology, Tangshan, 063210, China

Received Date: 2018-12-13

Fund Project: Supported by the Natural Science Foundation of Hebei Province, China (H2017209232) and the Research Foundation of Health and Family Planning Commission of Hebei (20170893).

Keywords:

solid-phase extraction (SPE) /
high performance liquid chromatography (HPLC) /
healthy people /
urine /
hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs)

Abstract: A method based on C₁₈ solid phase extraction (SPE) coupled with high performance liquid chromatography-fluorescence detection (SPE-HPLC-FLD) was developed for the simultaneous determination of seven hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs) in urine of healthy people. The 10 mL enzymatic hydrolyzed urine sample was purified and enriched by SPE process. The parameters influenced on SPE extraction efficiency such as the washing solvent, eluting solvent and eluting volume were investigated in detail. Under the optimized conditions, the method gave good linear ranges with the correlation coefficients (r) higher than 0.9970. The detection limits (S/N=3) and the quantification limits (S/N=10) were in the ranges of 0.04-4.96 ng·mL^-1 and 0.10-15.00 ng·mL^-1, respectively. The relative standard deviations of intra-day (n=3) and inter-day (n=3) were 1.4%-8.9% and 3.2%-11.5%, respectively. The developed method was applied to monitor the OH-PAHs in urine samples of 40 healthy people. The detection rate of seven target OH-PAHs was 20.0%-100.0% and the average recoveries at three spiked levels were 88.5%-102.7%. The method could be applied for the determination of OH-PAHs in urine of healthy people in a simple, sensitive and accurate way.