新型样品前处理结合毛细管电泳对环境污染物的分离与测定

发布时间：2018-07-11 12:56

  本文选题：毛细管电泳 + 分散液液微萃取　； 参考：《烟台大学》2016年硕士论文

【摘要】：环境水体中污染物含量较低,且基质复杂、干扰物质较多,因而,在检测污染物之前需要对实际样品进行预处理,以达到对待测物浓缩净化的目的。液液萃取和固相萃取是两种较为经典的传统样品前处理技术,然而,这种传统的样品前处理技术需要消耗大量的有机试剂,过程复杂,耗时较长,对环境和人体造成危害。分散液液微萃取(DLLME)和分散固相萃取(dSPE)是在传统的液液萃取和固相萃取的基础上发展而来的新型样品前处理技术,以其简单、快速、高效等优势得到了快速的发展,广泛应用于各种样品的检测,受到广大分析工作者的关注。毛细管电泳(CE)是一种相对成熟的分离检测技术,具有分析速度快、样品用量少、自动化程度高的优点,在环境、医药、食品等各个领域有着广泛的应用。在本文中,采用新型的样品前处理技术与毛细管电泳结合检测环境水样中的污染物,并探究了毛细管电泳的在线富集技术用于检测酚类雌激素。本文主要包括以下内容:第1章,绪论,着重介绍了分散液液微萃取和分散固相萃取两种新型的样品前处理技术。介绍了毛细管电泳技术的原理、分离模式、在线富集技术等。阐述了论文研究的依据及主要内容。第2章,采用分散固相萃取的前处理技术结合毛细管电泳检测环境水样中的有机汞。首次采用自主合成的巯基功能化材料作为分散固相萃取的吸附剂,并使用含有盐酸的L-半胱氨酸溶液作为洗脱剂进行洗脱。对合成的材料进行扫描电镜表征,对影响萃取效果的前处理条件进行了优化,包括溶液pH,吸附剂的用量,洗脱剂的体积以及洗脱溶液中盐酸的浓度。在最优的条件下,我们得到甲基汞和苯基汞的线性范围是2-200μg/L,乙基汞的线性范围是4-200μg/L,分析物的检出限和定量限为0.24-1.07μg/L和0.79-3.57μg/L,富集倍数为109-184。此方法成功应用于自来水和湖水中有机汞的分析,回收率为62.3%-107.2%,RSDs为3.5 10.1%,结果满意。第3章,采用分散液液微萃取的样品前处理技术结合胶束电动色谱(MEKC)检测环境水样中的己烷雌酚、双酚A、己烯雌酚和双烯雌酚四种雌激素。实验考察了毛细管电泳条件和分散液液微萃取的前处理条件。在最优的条件下,我们得到四种分析物的富集因子为241-467,检出限分别为0.3-0.6μg/L。将方法DLLME-MEKC成功应用于海水、湖水、自来水三种的真实水样中雌激素的检测,回收率在70.4 108.1%之间,RSDs为2.1 9.7%,结果令人满意。第4章,在胶束电动色谱的模式下,采用压力辅助电动进样的进样方式在线富集四种酚类雌激素,对影响富集效果的进样电压、进样时间等进行考察,并与传统的压力进样进行比较。在最优的条件下,四种分析物在压力辅助电动进样时得到的检出限为0.0071-0.017 mg/L,富集倍数为11-15。
[Abstract]:The content of pollutants in environmental water is relatively low, the matrix is complex, and there are many interfering substances. Therefore, it is necessary to pretreat the actual samples before detecting the pollutants in order to achieve the purpose of concentrating and purifying the test materials. Liquid-liquid extraction and solid-phase extraction are two classical traditional sample pretreatment techniques. However, this traditional sample pretreatment technology needs a large number of organic reagents, the process is complex and time-consuming, which is harmful to the environment and human body. Dispersible liquid microextraction (DLLME) and dispersed solid phase extraction (dSPE) are new sample pretreatment techniques developed on the basis of traditional liquid-liquid extraction and solid-phase extraction. Widely used in the detection of various samples, the majority of analysts pay attention to. Capillary electrophoresis (CE) is a relatively mature separation and detection technology with the advantages of fast analysis, less sample consumption and high automation. CE has been widely used in many fields, such as environment, medicine, food and so on. In this paper, a new sample pretreatment technique combined with capillary electrophoresis was used to detect pollutants in environmental water samples, and the on-line enrichment technique of capillary electrophoresis was explored for the detection of phenolic estrogens. The main contents of this paper are as follows: chapter 1, introduction, focusing on two new sample pretreatment techniques: dispersible liquid microextraction and dispersible solid phase extraction. The principle, separation mode and on-line enrichment of capillary electrophoresis were introduced. The basis and main contents of this paper are expounded. In chapter 2, organic mercury in environmental water samples was determined by dispersive solid phase extraction (DSPE) combined with capillary electrophoresis (CE). For the first time, the self-synthesized thiol functionalized material was used as the adsorbent for dispersive solid-phase extraction, and the L-cysteine solution containing hydrochloric acid was used as the eluent for elution. Scanning electron microscope (SEM) was used to characterize the synthesized materials. The pretreatment conditions affecting the extraction effect were optimized, including the pH of the solution, the amount of adsorbent, the volume of eluent and the concentration of hydrochloric acid in the elution solution. Under the optimal conditions, the linear range of methylmercury and phenyl mercury is 2-200 渭 g / L, the linear range of ethyl mercury is 4-200 渭 g / L, the detection and quantification limits of the analyte are 0.24-1.07 渭 g / L and 0.79-3.57 渭 g / L, and the enrichment multiple is 109-184. The method has been successfully applied to the analysis of organic mercury in tap water and lake water. The recovery rate is 62.3- 107.2 and the RSDs is 3.5 ~ 10.1.The results are satisfactory. In chapter 3, the sample pretreatment technique of dispersive liquid microextraction and micellar electrokinetic chromatography (MEKC) were used to detect four kinds of estrogens in environmental water samples, such as hexanoestrin, bisphenol A, diethylstilbestrol and dienoestriol. The conditions of capillary electrophoresis and the pretreatment of dispersive liquid microextraction were investigated. Under the optimal conditions, the enrichment factors of the four analytes were 241-467, and the detection limits were 0.3-0.6 渭 g / L. DLLME-MEKC was successfully applied to the determination of estrogen in seawater, lake water and tap water. The recovery rate was between 70.4 and 108.1% and the RSDs was 2.1%. The results were satisfactory. In chapter 4, in the mode of micellar electrokinetic chromatography, four phenolic estrogens were enriched online by pressure-assisted electrokinetic sampling, and the sampling voltage and injection time which affected the enrichment effect were investigated. And compared with the traditional pressure injection. Under the optimum conditions, the detection limit of the four analytes was 0.0071-0.017 mg / L and the enrichment factor was 11-15 when the pressure assisted electric injection was carried out.
【学位授予单位】：烟台大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：X832;O658.9
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本文编号：2115269