离子液体功能化杂化整体柱制备及其性能研究

发布时间：2018-07-05 00:40

本文选题：多面体寡聚倍半硅烷化试剂 + 咪唑离子液体　；参考：《河北大学》2016年硕士论文

【摘要】：毛细管液相色谱作为一种重要的微尺度分离分析技术,具有快速、高效、经济、环保等特点,在毛细管液相色谱中,固定相是其核心部分,决定着物质分离过程中的柱效、选择性和分离度。其中,杂化整体柱作为最有前途色谱材料之一,具有机械强度高、pH值适用范围广等特点,可弥补有机聚合物整体柱和无机硅胶整体柱的不足,因此,开发新型高效的杂化整体柱具有重要意义。本论文全文共分三章:第一章:分为三部分,第一部分综述了杂化整体柱的提出、发展和应用;第二部分综述了新型纳米材料在整体柱中的应用及研究现状;第三部分综述了离子液体修饰整体柱的研究现状。第二章:以甲基丙烯酸酯取代的多面体寡聚倍半硅烷化试剂(POSS-MA)为交联剂,以溴化1-乙烯基-3-辛烷基咪唑(VOI)为功能单体,通过“一锅法”制备了咪唑嵌合C8杂化毛细管整体柱(POSS-VOI),并分别采用扫描电子显微镜、红外光谱、元素分析等技术对合成的整体柱进行了表征;以烷基苯为样品考察了POSS-VOI杂化整体柱的保留特性,显示了典型的反相色谱保留机制,理论塔板数可达到124,000 N/m,与已报道的全氟咪唑修饰POSS的杂化毛细管整体柱相比,POSS-VOI呈现了较高的理论塔板数和较好的分离效果。第三章:以POSS-MA和溴化1-烯丙基-3-乙烯基咪唑(AVI)为前体物,通过“一锅法”制备了咪唑桥连POSS-MA的微孔杂化整体柱(POSS-AVI),红外光谱和元素分析结果表明AVI成功的被引入到整体材料上;同时,对整体柱的形态、孔径分布、热稳定性进行了考察;该固定相具有反相色谱的保留机制,可实现酸性、碱性和中性物质的高效分离分析,与常规的咪唑修饰POSS-MA的杂化整体柱(POSS-AEI)相比,POSS-AVI杂化整体柱呈现了不同的保留特性和略高的柱效;此外,POSS-AVI杂化整体柱可在纯水模式下实现亲水性核苷和核酸碱基的高效分离分析,同时对多肽的分离也显示了良好的潜能。
[Abstract]:As an important micro scale separation and analysis technique, capillary liquid chromatography has the characteristics of rapid, efficient, economical and environmental protection. In capillary liquid chromatography, fixed phase is its core part, which determines the column efficiency, selectivity and separation degree in the process of material separation. The hybrid monolithic column is one of the most promising chromatographic materials and has a machine. This paper is divided into three chapters: the first chapter is divided into three chapters: the first chapter is divided into three parts. The first part describes the proposed, development and application of hybrid monolithic columns, and second parts. The application and research status of new nanomaterials in the whole column were reviewed. The third part reviewed the status of the research on the ionic liquid modified monolithic column. The second chapter: the polyhedron oligomeric polysiliylated reagent (POSS-MA) substituted by methacrylate as the crosslinker, and the 1- vinyl -3- octanidazole (VOI) as the functional monomer, The imidazole chimeric C8 hybrid capillary monolithic column (POSS-VOI) was prepared by one pot method, and the synthesized monolithic column was characterized by scanning electron microscopy, infrared spectroscopy and elemental analysis. The retention characteristics of POSS-VOI hybrid monolithic columns were investigated with alkyl benzene as samples, and the typical retention mechanism of reversed phase chromatography was shown. The number of pylon can reach 124000 N/m. Compared with the reported perfluorimidazole modified POSS hybrid capillary monolithic column, POSS-VOI presents a higher theoretical tray number and better separation effect. The third chapter: using POSS-MA and brominated 1- allyl -3- vinyl imidazole (AVI) as precursors, the imidazole bridge continuous POSS-MA is prepared by "one pot method". Hole hybrid monolithic column (POSS-AVI), infrared spectrum and elemental analysis showed that AVI was successfully introduced into the whole material. Meanwhile, the morphology, pore size distribution and thermal stability of the whole column were investigated. The fixed phase has the retention mechanism of the reversed phase chromatography, which can realize the efficient separation and analysis of acid, alkaline and neutral substances. Compared with the hybrid monolithic column (POSS-AEI) modified with POSS-MA, the POSS-AVI hybrid monolithic column has different retention characteristics and slightly higher column efficiency. In addition, the POSS-AVI hybrid monolithic column can efficiently separate the hydrophilic nucleosides and nucleic acid bases in the pure water model, and also show good potential for the separation of the peptides.
【学位授予单位】：河北大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O645.1;O657.72

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