熔喷布固相萃取结合高效液相色谱-荧光检测法测定尿液中的1-羟基芘  

Determination of 1-Hydroxypyrene in Urine by Meltblown Nonwoven Fabrics Based Solid-Phase Extraction Combined with HPLC-FLD

作　　者：乐诗文 程冰薇 周漪涟 赵琴 YUE Shiwen;CHENG Bingwei;ZHOU Yilian;ZHAO Qin(School of Public Health,Wuhan University of Science and Technology,Hubei Province Key Laboratory of Occupational Hazard Identification and Control,Wuhan,430070)

机构地区：[1]武汉科技大学公共卫生学院,职业危害识别与控制湖北省重点实验室,湖北武汉430070

出　　处：《分析科学学报》2022年第4期455-461,共7页Journal of Analytical Science

基　　金：国家自然科学基金(No.81903366)。

摘　　要：建立了一种基于熔喷布固相萃取,结合高效液相色谱-荧光检测法(HPLC-FLD)测定尿液中1-羟基芘的新方法。优化了一系列影响萃取效率的参数,包括萃取材料熔喷布的用量、熔喷布裁剪的大小、上样液的体积和含盐量、解吸液的种类和体积等。在优化的条件下,1-羟基芘在0.01~200μg/L范围内线性关系良好(R^(2)>0.9999),检出限(LOD)0.003μg/L,日内、日间相对标准偏差(RSD)分别小于5.2%和4.2%。该方法具有有机试剂消耗少,分析成本低廉,简便快速,绿色环保等优点,成功应用于实际尿样的分析检测。In this study,a new method for the determination of 1-hydroxypyrene(1-OHP)in urine sample was developed based on meltblown nonwoven fabrics solid-phase extraction(SPE)combining with high performance liquid chromatography-fluorimetric detection(HPLC-FLD).As the core material of medical mask,meltblown nonwoven fabric is made of polypropylene superfine fibers which are randomly distributed and bonded together with a relatively large specific surface area and good permeability.Polypropylene as a high molecular hydrocarbon-based polymer,has the characteristics of good hydrophobicity and lipophilicity which can be applied for separation and enrichment of hydrophobic substances in food,environment and biology samples.The meltblown nonwoven fabric is soft and can fill the SPE cartridge tightly.This characteristics also makes it suitable to be used as an ideal SPE sorbent.In this study,key parameters influencing the extraction efficiency were investigated,including the amount of meltblown nonwoven fabrics,the volume and ionic strength of sampling solution,the type and volume of eluting solvent,etc..Under the optimized conditions,1-OHP had good linear relationship in the range of 0.01-200μg/L with R^(2)more than 0.9999.The recoveries in urine samples at three spiked concentrations were in the range of 91.7%-98.6%with the RSDs less than 5.2%(intra-day)and 4.2%(inter-day).The limit of detection(LOD)for 1-OHP was 0.003μg/L.Finally,this method was successfully applied in the analysis of 1-OHP in urine samples.

关 键 词：熔喷布 1-羟基芘 固相萃取 尿液 高效液相色谱-荧光检测 

分 类 号：O657.72[理学—分析化学]