顶空柱内微萃取-毛细管电泳在线联用新方法的研究与应用
发布时间：2018-08-14 19:08
【摘要】：毛细管电泳(Capillary Electrophoresis,CE)是一种已经发展较为成熟的微分离技术。在CE中,所采用的化学发光(CL)检测器因其背景干扰低、灵敏度高、线性范围宽、仪器要求简单等特点而常被用作CE的后期检测手段。纵观多种分析技术,CE对于很多复杂分析是很有吸引力的。这是因为该技术具有很高的通用性,比其他分析技术便宜,所需样品的量极小,对环境几乎不造成污染,而且相比其他诸如震动光谱这一有利于分化过程的技术,CE拥有更高的灵敏度。因此,CE-CL分析技术被广泛用于测定复杂样品中的多种生物分子,如血清和其他生理液。然而,与传统的CL技术相比,CE-CL法因为只能向分析体系注入很小的一段样品,同时检测光程很短,从而导致毛细管电泳技术的检测灵敏度还不是非常理想。所以,该技术难以检测生物样品基质中的痕量组分。由此可见,提高毛细管电泳技术的检测灵敏度就成为该领域的重要课题。鉴于此,本学位论文进行了如下研究与创新:1.我们自主制作了简易装置用于顶空柱内微萃取(Headspace In-tube Microextration,HS-ITME),并且阐释了其制作方法、特点以及影响因素,我们将HS-ITME与CE进行在线联用并开展了如下五组实验,通过实际的样品测定实验,我们验证了HS-ITME不仅可以有效提高CE的检测灵敏度,还可以简化样品前处理的操作步骤,由此拓宽了毛细管电泳技术在复杂实际组分测定中的应用。2.我们利用HS-ITME和CE进行在线联用来开展对溴酚类化合物的测定实验。在此实验中,我们考察并优化了萃取条件(萃取温度、萃取时间、盐度、样品的量等)和CE分离条件,后期基于优化后的实验条件,我们进一步测定了多种实际水体中的溴酚类物质,并通过一系列方法评估验证了HS-ITME可以使CE的检测灵敏度大大提高。3.基于胶束毛细管电泳(MEKC)的分离机理,结合邻苯二甲酸酯类物质(PAEs)的结构特性,我们采用反向迁移MEKC来分离PAEs,在此之前已开展了HS-ITME对PAEs的在线萃取,此过程考察且优化了萃取条件和CE分离条件,后期基于得到的最佳实验条件,我们进一步测定了多种自然水体和市售饮料中的PAEs,并通过一系列方法评估证明了HS-ITME使CE检测灵敏度大大提高。4.参考3中的实验情况,我们继续利用HS-ITME和反向迁移MEKC进行在线联用,来检测菊酯类农药,同时考察并优化了萃取条件和分离条件,后期我们将实验建立在最佳条件下,测定了多种水果中的菊酯类农残,最后通过一系列方法评估证明了HS-ITME使CE检测灵敏度大大提高。5.基于1中的实验原理和结果以及离子液体(ILs)在CE方面的应用,我们通过向CE运行缓冲液中添加ILs来进一步改善萃取效率,通过检测多种酚类物质,我们考察并优化了萃取条件(在1中条件的基础上增加了ILs种类和浓度的影响)和分离条件,并在此条件下成功测定了实际水体中的多种酚类物质,最后通过方法评估证明了HS-ITME使HS-ITME的检测灵敏度有效提高。
[Abstract]:Capillary Electrophoresis (CE) is a mature micro-separation technology. In CE, the chemiluminescence (CL) detector is often used as a post-detection method for CE because of its low background interference, high sensitivity, wide linear range and simple instrument requirements. Complex analysis is attractive because it is highly versatile, cheaper than other analytical techniques, requires very small amounts of samples, causes little pollution to the environment, and is more sensitive to CE than other techniques such as vibrational spectroscopy, which is conducive to the differentiation process. However, compared with traditional CL technique, CE-CL method can only inject a very small sample into the analytical system, and the detection optical path is very short, so the detection sensitivity of capillary electrophoresis is not very ideal. To improve the detection sensitivity of capillary electrophoresis (CE) has become an important topic in this field. In view of this, the following research and innovations have been made in this dissertation: 1. We have developed a simple headspace in-tube microextration (HS-ITME) device for headspace in-tube microextraction (HS-ITME). The manufacturing method, characteristics and influencing factors of HS-ITME and CE were explained. We combined HS-ITME with CE on-line and carried out the following five groups of experiments. Through the actual sample determination experiments, we verified that HS-ITME can not only effectively improve the detection sensitivity of CE, but also simplify the operation steps of sample pretreatment, thus broadening the capillary electrophoresis. In this experiment, we investigated and optimized the extraction conditions (extraction temperature, extraction time, salinity, sample amount, etc.) and the separation conditions of CE. In the later stage, based on the optimized experimental conditions, we studied and optimized the extraction conditions. HS-ITME can greatly improve the detection sensitivity of CE. 3. Based on the separation mechanism of micellar capillary electrophoresis (MEKC) and the structural characteristics of phthalate esters (PAEs), we used reverse migration MEKC to separate PAEs. The on-line extraction of PAEs by HS-ITME has been carried out before. The extraction conditions and CE separation conditions have been investigated and optimized. Based on the best experimental conditions, PAEs in various natural waters and commercial drinks have been further determined. The sensitivity of CE detection has been greatly improved by HS-ITME through a series of evaluation methods. Referring to the experiment in 3, we continue to use HS-ITME and reverse migration MEKC for on-line detection of pyrethroid pesticides, while investigating and optimizing the extraction conditions and separation conditions. Later we will establish the experiment under the best conditions to determine pyrethroid residues in a variety of fruits, and finally through a series of methods to evaluate and prove HS. Based on the experimental principle and results in 1 and the application of ionic liquids (ILs) in CE, we further improved the extraction efficiency by adding ILs to the running buffer of CE. By detecting a variety of phenolic substances, we investigated and optimized the extraction conditions (adding ILs on the basis of 1 condition). The results show that HS-ITME can effectively improve the detection sensitivity of HS-ITME.
【学位授予单位】：青岛科技大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O658
本文编号：2183836
[Abstract]:Capillary Electrophoresis (CE) is a mature micro-separation technology. In CE, the chemiluminescence (CL) detector is often used as a post-detection method for CE because of its low background interference, high sensitivity, wide linear range and simple instrument requirements. Complex analysis is attractive because it is highly versatile, cheaper than other analytical techniques, requires very small amounts of samples, causes little pollution to the environment, and is more sensitive to CE than other techniques such as vibrational spectroscopy, which is conducive to the differentiation process. However, compared with traditional CL technique, CE-CL method can only inject a very small sample into the analytical system, and the detection optical path is very short, so the detection sensitivity of capillary electrophoresis is not very ideal. To improve the detection sensitivity of capillary electrophoresis (CE) has become an important topic in this field. In view of this, the following research and innovations have been made in this dissertation: 1. We have developed a simple headspace in-tube microextration (HS-ITME) device for headspace in-tube microextraction (HS-ITME). The manufacturing method, characteristics and influencing factors of HS-ITME and CE were explained. We combined HS-ITME with CE on-line and carried out the following five groups of experiments. Through the actual sample determination experiments, we verified that HS-ITME can not only effectively improve the detection sensitivity of CE, but also simplify the operation steps of sample pretreatment, thus broadening the capillary electrophoresis. In this experiment, we investigated and optimized the extraction conditions (extraction temperature, extraction time, salinity, sample amount, etc.) and the separation conditions of CE. In the later stage, based on the optimized experimental conditions, we studied and optimized the extraction conditions. HS-ITME can greatly improve the detection sensitivity of CE. 3. Based on the separation mechanism of micellar capillary electrophoresis (MEKC) and the structural characteristics of phthalate esters (PAEs), we used reverse migration MEKC to separate PAEs. The on-line extraction of PAEs by HS-ITME has been carried out before. The extraction conditions and CE separation conditions have been investigated and optimized. Based on the best experimental conditions, PAEs in various natural waters and commercial drinks have been further determined. The sensitivity of CE detection has been greatly improved by HS-ITME through a series of evaluation methods. Referring to the experiment in 3, we continue to use HS-ITME and reverse migration MEKC for on-line detection of pyrethroid pesticides, while investigating and optimizing the extraction conditions and separation conditions. Later we will establish the experiment under the best conditions to determine pyrethroid residues in a variety of fruits, and finally through a series of methods to evaluate and prove HS. Based on the experimental principle and results in 1 and the application of ionic liquids (ILs) in CE, we further improved the extraction efficiency by adding ILs to the running buffer of CE. By detecting a variety of phenolic substances, we investigated and optimized the extraction conditions (adding ILs on the basis of 1 condition). The results show that HS-ITME can effectively improve the detection sensitivity of HS-ITME.
【学位授予单位】：青岛科技大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O658
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