固相支撑液液萃取-液相色谱-串联质谱法测定尿液中10种单羟基多环芳烃  

Determination of 10 Kinds of Monohydroxylated Polycyclic Aromatic Hydrocarbons in Human Urine by Supported Liquid Extraction Followed by Liquid Chromatography- Tandem Mass Spectrometry

作　　者：商婷 赵灵娟 李佩 曾祥英[1] 于志强[1] SHANG Ting;ZHAO Ling-Juan;LI Pei;ZENG Xiang-Ying;YU Zhi-Qiang(State Key Laboratory of Organic Geochemistry, Guangdong Key Laboratory of Environment and Resources, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China;University of Chinese Academy of Sciences, Beijing 100049, China)

机构地区：[1]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省环境资源利用与保护重点实验室,广州510640 [2]中国科学院大学,北京100049

出　　处：《分析化学》2019年第6期876-882,共7页Chinese Journal of Analytical Chemistry

基　　金：中国科学院战略性先导科技专项(No.XDB14010202);国家重点研发计划(No.2017YFC0212003)资助~~

摘　　要：通过检测人体尿液中多种羟基多环芳烃(OH-PAHs)的浓度可全面评估多环芳烃(PAHs)在人体的负荷水平。本研究建立并优化了一种基于固相支撑液液萃取(SLE)的前处理技术,在此基础上,利用液相色谱-串联质谱法(LC-MS/MS)测定人体尿液中的10种OH-PAHs。尿样采用硅藻土SLE柱进行富集净化,二氯甲烷-正己烷(3∶7,V/V)混合溶液作为目标化合物的洗脱液。前处理优化结果表明,与传统方法相比,本方法具有较好的回收率,同时可有效降低生物基质的干扰。本方法在3个加标浓度水平(10、50和100μg/L)下的回收率为88.5%～120.9%,重复性精密度范围为1.6%～8.1%。检出限与定量限分别在0.06～0.3μg/L和0.2～1.0μg/L之间。本方法成功用于广东省小学生尿液中OH-PAHs的测定,结果表明,2-OHN是最主要的检出化合物,最高浓度达到4.83μg/L。The monitoring of urinary monohydroxylated polycyclic aromatic hydrocarbons(OH-PAHs) can be used for the risk assessment of human exposure to polycyclic aromatic hydrocarbons(PAHs). In this work, we developed and optimized a new pretreatment method based on solid-phase supported liquid-liquid extraction(SLE). After pretreatment, the analytes were then determined by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Urine samples were extracted with a mixed solution of dichloromethane and n-hexane(3∶7, V/V) by a SLE clean-up using a diatomaceous earth mini-cartridge. The results indicated that the developed pretreated procedure had good recoveries and also significantly reduced the interference of biological matrix. At three concentration levels(10, 50 and 100 μg/L), the recoveries of ten OH-PAHs ranged from 88.5% to 120.9%, and the repeatability ranged from 1.6% to 8.1%. The limits of detection ranged from 0.06 μg/L to 0.3 μg/L and the limits of quantitation were between 0.2 μg/L and 1.0 μg/L. This method was finally successfully applied to the determination of OH-PAHs in urines collected from primary school students in Guangdong. The results showed that 2-OHN was the dominant compound, with the highest concentration of 4.83 μg/L.

关 键 词：单羟基多环芳烃 尿液 固相支撑液液萃取 液相色谱-串联质谱 

分 类 号：R446.12[医药卫生—诊断学] R114[医药卫生—临床医学] O657.63[理学—分析化学]