新型分散液液微萃取在水中环境雌激素检测中的应用

发布时间：2018-05-20 06:55

本文选题：环境雌激素 + 盐析辅助液液萃取　；参考：《河北大学》2017年硕士论文

【摘要】：环境雌激素为内分泌干扰物的一类,是指能够模拟或干扰生物体内分泌功能的物质,可通过食物链在生物体内富集,也可通过环境暴露(水)与生物体接触,从而影响生物体的各个系统,破坏机体内环境的稳定,危害生物体的健康。因此,对各类水体中环境雌激素的监测具有十分重要的意义。本文建立了两种新型样品预处理方法对水中的环境雌激素进行监测。全文共分为3章,其基本内容如下:第一章:简要概述了样品预处理的方法。其中重点阐述了分散液液微萃取及环境雌激素的萃取方法,以及本文的选题背景和研究内容。第二章:建立了逆流盐析均匀液液萃取-分散液液微萃取结合高效液相色谱(HPLC-UV)测定水中的环境雌激素。本实验考察了逆流盐析均匀液液萃取方法的萃取剂种类及体积、流速、水样的pH和分散液液微萃取方法的萃取剂种类及体积和离子强度对萃取效率的影响,并对该方法进行了系统评估。最佳萃取条件为:2 mL乙腈;流速0.4 mL/min;50μL四氯化碳;10%离子强度。己烯雌酚和辛基酚的线性关系良好(R20.9991),LOD在0.09-0.203 ng/mL之间,该方法的加标回收率在81.4-105.9%之间,相对标准偏差为1.0-7.6%。所建立的方法已成功应用于河水、井水、瓶装水和校园饮用水的检测,该方法操作简单、成本低、分相速度快,对分析物的测定有较好的重现性和高的回收率。第三章:建立了泡腾辅助分散液液微萃取结合高效液相色谱(HPLC/UV)测定环境水中的雌激素。该方法以碳酸钠与磷酸二氢钠产生的二氧化碳为分散驱动力,使萃取剂快速均匀地分散在水样中,实现整个萃取过程。本实验考察了泡腾剂的组成及总量、加入泡腾剂的方式、萃取剂种类及体积和水样的pH对萃取效率的影响,并对该方法进行了系统评估。最优的萃取条件为:0.35 g的碳酸钠和磷酸二氢钠作为泡腾剂置于试管底部,60μL四氯化碳用作萃取剂,水样的pH对萃取效率无影响。在最佳的萃取条件下,两种物质均呈现良好的线性关系,线性范围为5-200 ng/m L,加标回收率在81.5-102.8%,相对标准偏差为0.90-4.4%。本文所建立的方法已成功应用于海水、井水和饮用水样品的检测,在萃取过程中无需使用有机溶剂作分散剂,整个过程仅需几十秒钟即可达到好的萃取效率。因此,该方法具有操作简单、快速、低成本、绿色环保等特点。
[Abstract]:Environmental estrogens, a class of endocrine disruptors, are substances capable of mimicking or disrupting the endocrine function of organisms, which can be enriched in organisms through the food chain or in contact with organisms through environmental exposure (water), Thus affecting the various systems of the organism, destroying the stability of the environment, endangering the health of the organism. Therefore, the monitoring of environmental estrogens in various water bodies is of great significance. In this paper, two new sample pretreatment methods were established to monitor environmental estrogens in water. The whole paper is divided into three chapters. The basic contents are as follows: chapter 1: the methods of sample pretreatment are summarized briefly. The methods of microextraction and environmental estrogens extraction, as well as the background and research contents of this paper are emphasized. Chapter 2: the determination of environmental estrogens in water by countercurrent salting-out homogeneous liquid-liquid extraction dispersible liquid microextraction and high performance liquid chromatography (HPLC-UV) has been established. The effects of extractant type and volume, flow rate, pH of water sample and extractant type and volume and ionic strength of dispersion liquid microextraction method on extraction efficiency were investigated. The method is systematically evaluated. The optimum extraction conditions were as follows: 1: 2 mL acetonitrile, flow rate 0.4 mL / min ~ (-1) 50 渭 L carbon tetrachloride 10% ionic strength. The linear relationship between diethylstilbestrol and octyl phenol was good. The relative standard deviation was 1.0-7.6% and the recoveries of the method were between 81.4-105.9% and 0.09-0.203 ng/mL. The established method has been successfully applied to the detection of river water, well water, bottled water and campus drinking water. The method is simple in operation, low in cost, fast in phase separation, and has good reproducibility and high recovery rate for the determination of analytes. Chapter 3: a method for the determination of estrogens in environmental water by effervescent assisted dispersible liquid microextraction combined with high performance liquid chromatography (HPLC / UV) was established. In this method, the carbon dioxide produced by sodium carbonate and sodium dihydrogen phosphate is used as the driving force, and the extractant is dispersed in the water sample quickly and uniformly, and the whole extraction process is realized. The effects of the composition and total amount of effervescent agent, the way of adding effervescent agent, the type and volume of extractant and the pH of water sample on the extraction efficiency were investigated, and the method was systematically evaluated. The optimal extraction conditions were as follows: sodium carbonate and sodium dihydrogen phosphate were used as effervescent agents at the bottom of the tube and 60 渭 L carbon tetrachloride was placed at the bottom of the test tube as the extractant. The pH of the water sample had no effect on the extraction efficiency. Under the optimum extraction conditions, the linear range was 5-200 ng/m / L, the recovery rate was 81.5-102.8, and the relative standard deviation was 0.90-4.4%. The method established in this paper has been successfully applied to the detection of seawater, well water and drinking water samples. No organic solvent is used as dispersant in the extraction process, and the extraction efficiency can be achieved in only a few tens of seconds. Therefore, the method has the advantages of simple operation, fast operation, low cost and green environmental protection.
【学位授予单位】：河北大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X832;O658.2

【参考文献】