Preparation Of Two Strongly Hydrophilic Monolithic Column And Its Application In The Analysising Small Polar Molecules

The research of hydrophilic interaction liquid chromatography (HILIC) has become increasingly popular in chromatography field because of the superiority in polar compounds separating over reversed-phase chromatography. There have been a large number of researcher engaged in research and development of HILIC material, but there are still some limitations of the study of HILIC. On the one hand, the hydrophilic capacity is insufficient for some complex samples which are difficult to be separated; on the other hand, there is less type of hydrophilic material and limited choices available to researchers. Based on this situation, we chose monolith as the research object, synthesized two strongly hydrophilic monolithic columns through synthesis and selection of more hydrophilic organic monomers. Following three aspects were made:1.The synthetic route of two monolith organic monomer piperazine gimini sulfobetaine and diamine gimini sulfobetaine was explored. We explored two routes acylation process and epoxy method of the sulfobetaine of Gemini Sulfobetaine synthetic in the geminate structure such as piperazine and N,N-dimethyl-1,3-propanediamine.The products were characterized by mass spectrometry. The synthesis method was optimized by choosing the best reaction temperature and material ratio.2.Propylenediamine type gemini sulfobetaine silicone hybrid monolith column was synthesized through sol-gel method by using the propylene diamine type gemini sulfobetaine as organic monomer. The optimization of preparation condition was carried out, uniform structure with porosity and good permeability hybrid monolithic column was developed. Hydrophilic separation performance of propylene diamine type gemini twin sulfobetaine silica hybrid monolithic column was characterized, the results show good results in separating nucleoside compounds. The hydrophilic properties of its type were compared to another sulfobetaine silica hybrid monolithic column. It proves that the hydrophilic separation effect of propylene diamine type gimini sulfobetaine chromatographic is better than other ordinary hydrophilic materials.3.Using polyethylene imine(PEI) as monomer, pentaerythritol ether(PTE) as the crosslinking agent, with binary porogen acetonitrile-Polyethylene glycol600(PEG600), PEI-PTE organic polymer monolithic column was synthesized. The optimization of preparation condition was carried out, uniform structure with porosity and good permeability hybrid monolithic column was developed. Hydrophilic separation performance of PEI-PTE organic polymer monolithic column was characterized, the results show good results in separating nucleosides, nucleotides, phenols, acids and other strong polar hydrophilic small molecules.