本文選題：多面體寡聚倍半硅烷化試劑 + 咪唑離子液體　； 參考：《河北大學》2016年碩士論文

【摘要】：毛細管液相色譜作為一種重要的微尺度分離分析技術(shù),具有快速、高效、經(jīng)濟、環(huán)保等特點,在毛細管液相色譜中,固定相是其核心部分,決定著物質(zhì)分離過程中的柱效、選擇性和分離度。其中,雜化整體柱作為最有前途色譜材料之一,具有機械強度高、pH值適用范圍廣等特點,可彌補有機聚合物整體柱和無機硅膠整體柱的不足,因此,開發(fā)新型高效的雜化整體柱具有重要意義。本論文全文共分三章:第一章:分為三部分,第一部分綜述了雜化整體柱的提出、發(fā)展和應用;第二部分綜述了新型納米材料在整體柱中的應用及研究現(xiàn)狀;第三部分綜述了離子液體修飾整體柱的研究現(xiàn)狀。第二章:以甲基丙烯酸酯取代的多面體寡聚倍半硅烷化試劑(POSS-MA)為交聯(lián)劑,以溴化1-乙烯基-3-辛烷基咪唑(VOI)為功能單體,通過“一鍋法”制備了咪唑嵌合C8雜化毛細管整體柱(POSS-VOI),并分別采用掃描電子顯微鏡、紅外光譜、元素分析等技術(shù)對合成的整體柱進行了表征;以烷基苯為樣品考察了POSS-VOI雜化整體柱的保留特性,顯示了典型的反相色譜保留機制,理論塔板數(shù)可達到124,000 N/m,與已報道的全氟咪唑修飾POSS的雜化毛細管整體柱相比,POSS-VOI呈現(xiàn)了較高的理論塔板數(shù)和較好的分離效果。第三章:以POSS-MA和溴化1-烯丙基-3-乙烯基咪唑(AVI)為前體物,通過“一鍋法”制備了咪唑橋連POSS-MA的微孔雜化整體柱(POSS-AVI),紅外光譜和元素分析結(jié)果表明AVI成功的被引入到整體材料上;同時,對整體柱的形態(tài)、孔徑分布、熱穩(wěn)定性進行了考察;該固定相具有反相色譜的保留機制,可實現(xiàn)酸性、堿性和中性物質(zhì)的高效分離分析,與常規(guī)的咪唑修飾POSS-MA的雜化整體柱(POSS-AEI)相比,POSS-AVI雜化整體柱呈現(xiàn)了不同的保留特性和略高的柱效;此外,POSS-AVI雜化整體柱可在純水模式下實現(xiàn)親水性核苷和核酸堿基的高效分離分析,同時對多肽的分離也顯示了良好的潛能。
[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.
【學位授予單位】：河北大學
【學位級別】：碩士
【學位授予年份】：2016
【分類號】：O645.1;O657.72

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