本文選題：高效液相色譜　切入點(diǎn)：金屬-有機(jī)框架材料　出處：《河北大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：高效液相色譜(HPLC)作為一種重要的分離分析技術(shù),廣泛地應(yīng)用于化學(xué)、藥物分析、食品安全檢測、環(huán)境檢測等諸多領(lǐng)域。色譜固定相作為高效液相色譜系統(tǒng)的核心,對色譜的分離性能起著至關(guān)重要的作用。金屬-有機(jī)框架材料(MOFs)是一種新型的有機(jī)-無機(jī)雜化多孔晶體材料,由于具有獨(dú)特的結(jié)構(gòu)和杰出的特性,如多孔性、高比表面積及良好的化學(xué)和熱穩(wěn)定性,使得其在HPLC中作為固定相具有很大的潛能。全文共分三章:第一章:本章共分為三部分。第一部分簡述了金屬-有機(jī)框架材料及其作為液相色譜固定相的研究現(xiàn)狀。第二部分簡述了離子液體及其特征。第三部分簡述了本論文的創(chuàng)新點(diǎn)和出發(fā)點(diǎn)。第二章:本章設(shè)計并合成了一種新型的離子液體(ILs)溴化1,3-雙(4-羧丁基)咪唑摀(ILI),并以ILI作為有機(jī)配體與金屬鋅離子配位形成MOFs晶體材料ILI-01。進(jìn)而將ILI-01修飾在氨基硅球表面并通過調(diào)節(jié)生長周期,制備出一種新型的ILI-01@Si O_2核殼型色譜固定相。分別采用傅里葉變換紅外光譜儀、X射線粉末衍射儀、熱重量分析儀、掃描電子顯微鏡、元素分析儀和比表面積及孔隙度分析儀進(jìn)行了表征,結(jié)果證明ILI-01@SiO_2核殼型色譜固定相被成功地制備。第三章:本章將合成的ILI-01@SiO_2核殼型色譜固定相制備成ILI-01@Si O_2色譜柱。由于在MOFs材料中引入了ILI咪唑陽離子,該色譜固定相具有親水作用色譜(HILIC)的保留機(jī)制。分別采用核苷和核酸堿基類化合物、維生素類化合物、酰胺類化合物考察了ILI-01@Si O_2色譜柱的分離性能,并與常用的氨基色譜柱進(jìn)行比較,結(jié)果表明ILI-01@SiO_2色譜柱能夠快速分離強(qiáng)極性化合物,并顯示出了更高的選擇性。ILI-01@SiO_2色譜柱還可用于檢測嬰幼兒奶粉中非法添加的三聚氰胺,顯示了良好的應(yīng)用潛能。
[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.
【學(xué)位授予單位】：河北大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O652.63;TB34

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