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