毛细管电泳在线双富集方法的研究及应用

发布时间：2018-04-23 22:33

本文选题：毛细管电泳 + 在线双富集方法　；参考：《南方医科大学》2017年硕士论文

【摘要】：目前,由药物残留和药物滥用造成的社会危害越来越明显,因此对微量药物组分残留量的检测引起了广泛重视。而传统方法在药物检测的过程中都会遇到被测组分浓度低、基质复杂、存在大量干扰物等问题,因此为了对微量超微量组分准确分析定量,迫切需要建立简单快速、灵敏的方法。毛细管电泳技术是目前分离学科中最活跃的方法之一,具有操作简单、高效、高速、样品预处理简单、样品需要量小等特点。但因毛细管内径小,检测窗口光程短,而导致的灵敏度小,成为其检测复杂基质中痕量物质最大的限制。可通过改造仪器以提高其灵敏度,例如更换不同的检测器,但价格昂贵,进一步发展的潜力较小。所以,目前灵敏度问题主要通过样品在线富集方法来解决。在线富集是指通过改变体系的条件,使毛细管内样品区带压缩,从而使样品浓度变大,灵敏度增强的一种方法。每种在线富集方法都有一定的适用范围和前提条件,为了进一步降低检测限,针对分析分析物的物理化学性质及基质的复杂性,通常需要几种在线富集方法的联用。因此,毛细管电泳在线富集联用方法的发展成为分析工作者研究的重点。本论文在前人工作的基础上,对毛细管在线富集方法在药物残留中的应用进行了研究,主要开展了如下创新性的工作:1.将有机溶剂胶束堆积和场放大样品堆积富集技术联用,建立了磺胺甲恶唑和甲氧苄啶的分离富集体系。甲氧苄啶和磺胺甲恶唑具有疏水性,在样品基质中加入十二烷基磺酸钠可形成胶束。引入样品后再引入一段有机溶剂,胶束在有机溶剂的诱导下更易于解聚,完成有机溶剂胶束富集。利用磺胺甲恶唑和甲氧苄啶在酸性溶液中的电荷性质使其在有机溶剂低电导率区和缓冲溶液高电导率区带边界完成场强放大样品堆积。建立了生物样品中甲氧苄啶和磺胺甲恶唑的残留检测新方法,并实际应用于6种动物源性食品(纯牛奶、高钙奶、纯羊奶、奶粉、蜂蜜、鸡蛋)。2.建立了 β-CD辅助在线毛细管双富集体系,在毛细管电泳中先后实现了场放大样品堆积和有机溶剂胶束解聚两步富集,并以兴奋剂阿替洛尔和美托洛尔为模型验证了方法的可行性。在样品基质中加入少量的β-CD,可降低十二烷基磺酸钠胶束的表面活性,从而降低胶束的临界胶束浓度(CMC),更有利于胶束解聚。该方法简单、快速、重现性好,并已应用于人尿液中阿替洛尔和美托洛尔的残留检测。
[Abstract]:At present, the social harm caused by drug residue and drug abuse is becoming more and more obvious. Therefore, the detection of trace residues in microdrugs has attracted wide attention. The traditional methods will meet the problems of low concentration, complex matrix and large number of dry disturbances in the process of drug testing. It is urgent to establish a simple, rapid and sensitive method for accurate analysis and quantitative analysis. Capillary electrophoresis (CE) is one of the most active methods in the field of separation. It has the characteristics of simple operation, high efficiency, high speed, simple sample preprocessing and small sample requirement. However, the sensitivity of the detection window is small because of small capillary diameter, and the sensitivity is small. It can detect the greatest limit of trace substance in complex matrix. It can improve its sensitivity by changing the instrument, such as the replacement of different detectors, but the price is expensive and the potential for further development is small. So, the problem of sensitivity is mainly solved by the method of sample on-line enrichment. The sample area in the tube is compressed, which makes the sample concentration larger and the sensitivity enhanced. Each on-line enrichment method has a certain range of application and precondition. In order to further reduce the detection limit, several on-line enrichment methods are usually needed to analyze the physical and chemical properties of the analyte and the complexity of the matrix. On the basis of predecessors' work, this paper studies the application of capillary on-line enrichment in drug residue. The main work is as follows: 1. the accumulation of organic solvent micelles and accumulation of field magnification samples are carried out. The separation and enrichment system of sulfamethoxazole and trimethoprim was established by technology. The hydrophobicity of trimethoprim and sulfamethoxazole was hydrophobic, and the sodium alkyl sulfonate was added to the sample matrix to form micelles. The sample was introduced into an organic solvent and the micelles were more easily depolymerization under the induction of organic solvents and completed the organic solvent micelles. Enrichment. Using the charge properties of sulfamethoxazole and trimethoprim in the acidic solution to complete the accumulation of field strength samples in the low conductivity area of organic solvents and the high conductivity zone of the buffer solution, a new method for the detection of trimethoprim and sulfamethoxazole in biological samples was established and applied to the 6 species of animal origin food. The product (pure milk, high calcium milk, pure goat milk, milk powder, honey, egg).2. has established a beta -CD assisted on-line capillary double rich group. In capillary electrophoresis, the accumulation of field amplification samples and the two steps of organic solvent micelle depolymerization have been realized, and the feasibility of the method is verified by the model of atenolol and metoprolol. The addition of a small amount of beta -CD can reduce the surface activity of the sodium alkyl sulfonate micelle and reduce the critical micelle concentration (CMC) of the micelles, which is more conducive to the depolymerization of the micelles. This method is simple, rapid and reproducible, and has been applied to the determination of atenolol and metoprolol in human urine.

【学位授予单位】：南方医科大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O658.9;R927

【参考文献】