金属—有机框架核壳色谱材料制备及分离性能研究

发布时间：2018-03-21 14:17

本文选题：高效液相色谱　切入点：金属-有机框架材料　出处：《河北大学》2017年硕士论文　论文类型：学位论文

【摘要】：高效液相色谱(HPLC)作为一种重要的分离分析技术,广泛地应用于化学、药物分析、食品安全检测、环境检测等诸多领域。色谱固定相作为高效液相色谱系统的核心,对色谱的分离性能起着至关重要的作用。金属-有机框架材料(MOFs)是一种新型的有机-无机杂化多孔晶体材料,由于具有独特的结构和杰出的特性,如多孔性、高比表面积及良好的化学和热稳定性,使得其在HPLC中作为固定相具有很大的潜能。全文共分三章:第一章:本章共分为三部分。第一部分简述了金属-有机框架材料及其作为液相色谱固定相的研究现状。第二部分简述了离子液体及其特征。第三部分简述了本论文的创新点和出发点。第二章:本章设计并合成了一种新型的离子液体(ILs)溴化1,3-双(4-羧丁基)咪唑摀(ILI),并以ILI作为有机配体与金属锌离子配位形成MOFs晶体材料ILI-01。进而将ILI-01修饰在氨基硅球表面并通过调节生长周期,制备出一种新型的ILI-01@Si O_2核壳型色谱固定相。分别采用傅里叶变换红外光谱仪、X射线粉末衍射仪、热重量分析仪、扫描电子显微镜、元素分析仪和比表面积及孔隙度分析仪进行了表征,结果证明ILI-01@SiO_2核壳型色谱固定相被成功地制备。第三章:本章将合成的ILI-01@SiO_2核壳型色谱固定相制备成ILI-01@Si O_2色谱柱。由于在MOFs材料中引入了ILI咪唑阳离子,该色谱固定相具有亲水作用色谱(HILIC)的保留机制。分别采用核苷和核酸碱基类化合物、维生素类化合物、酰胺类化合物考察了ILI-01@Si O_2色谱柱的分离性能,并与常用的氨基色谱柱进行比较,结果表明ILI-01@SiO_2色谱柱能够快速分离强极性化合物,并显示出了更高的选择性。ILI-01@SiO_2色谱柱还可用于检测婴幼儿奶粉中非法添加的三聚氰胺,显示了良好的应用潜能。
[Abstract]:High performance liquid chromatography (HPLC), as an important separation and analysis technology, is widely used in many fields such as chemistry, drug analysis, food safety detection, environmental detection and so on. Chromatographic stationary phase is the core of high performance liquid chromatography system. The metal-organic framework material (MOFs) is a novel organic-inorganic hybrid porous crystal material, due to its unique structure and outstanding properties, such as porous. High specific surface area and good chemical and thermal stability, This paper is divided into three chapters: chapter 1: this chapter is divided into three parts. The first part describes the metal-organic framework material and its application as stationary phase in liquid chromatography. The second part briefly describes the ionic liquids and their characteristics. The third part briefly describes the innovation and starting point of this thesis. Chapter 2: this chapter designs and synthesizes a new ionic liquid (ILs) bromide (1k3- bis-cy-4carboxy#china_person0#) imidazole. ILI was used as an organic ligand to coordinate with zinc ion to form MOFs crystal material ILI-01.Then ILI-01 was modified on the surface of aminosilicon spheres and the growth cycle was adjusted. A new type of ILI-01@Si O\ -2 core-shell chromatographic stationary phase was prepared, which was characterized by Fourier transform infrared spectrometer (FTIR), thermogravimetric analyzer (TGA), scanning electron microscope (SEM), X-ray powder diffractometer (XRD), scanning electron microscope (SEM). Element analyzer and specific surface area and porosity analyzer were used to characterize, The results showed that the ILI-01@SiO_2 core-shell chromatographic stationary phase was successfully prepared. Chapter 3: in this chapter, the synthesized ILI-01@SiO_2 core-shell chromatographic stationary phase was prepared into a ILI-01@SiO_2 column. ILI imidazole cations were introduced into the MOFs material. The chromatographic stationary phase has the retention mechanism of hydrophilic interaction chromatography (HILIC). The separation properties of ILI-01@Si O 2 column were investigated by nucleoside, nucleic acid base compounds, vitamin compounds and amides, respectively. Compared with common amino chromatographic column, the results showed that the ILI-01@SiO_2 column could quickly separate the strong polar compounds, and showed a higher selectivity. ILI-01 @ SiO2 column could also be used to detect melamine illegally added in infant milk powder. Shows good application potential.
【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】：O652.63;TB34

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