Preparation And Application Of Sulfobetaine Hybrid Monolithic Column

The hydrophilic interaction liquid chromatography(HILIC)has attract more and more attention in separation field because of the greater advantage in polar compounds separating than the normal phase chromatography and reverse phase chromatography.Researchers have developed a range of HILIC columns for the separation of polar hydrophilic compound until now,but there are still some limitations in the application areas(such as metabolomics and proteomics).Mainly problem is that,on the one hand,the hydrophilic ability is insufficient forsome hydrophilic chromatographic material,so some complex samples are difficult to be separated;on the other hand,there are fewer types of strongly hydrophilic material and complex preparative monolithic column method,which have limited the available choices to researchers.Organic-inorganic hybrid monolithic column,with a combination of organic and inorganic monolithic respective advantages,containing a high mechanical strength,good stability inorganic matrix section and an easy-modified functional monomer in organic moiety can be prepared of reverse phase,hydrophobic,hydrophilic,ion exchange etc multiple modes of monolithic column,which have a great advantage in the preparation and application of monolithic column.On the basis of this situation,it is necessary and very meaningful to develop new column.We chose the hydrophilic organic-inorganic hybrid monolithic column as the research object,synthesized three strongly hydrophilic monolithic columns through synthesis and selection of more hydrophilic organic monomers,developing simple and reproducible preparation methods.Three main contents are made as follows:1.A novel type of strongly hydrophilic hybrid monolithic column was synthesized through sol-gel one-pot method by using the propylene diamine type gemini sulfobetaine as organic monomer.The optimization of monolithic column preparation condition was carefully carried out,and the chemical properties,topography,mechanical stability,etc.physical and chemical properties were detailed characterized.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 studied.The results show that the monolithic column has a significant hydrophilic ability in separation nucleosides,bases,amides,phenols etc.Finally,the hybrid monolithic column was applied to separation complex proteolytic peptide successfully.2.A POSS functionalized hybrid column was successfully prepared through using dimethylaminoethyl methacrylate methyl acrylate,butyrolactone acid as the monomer,POSS-MA as a crosslinking agent by a "one-pot" method.The betaine sulfonic acid group was introducted in situ in the method,which was free to monomer synthesis,saving large amounts of organic solvent consumption during the synthesis,easy to prepare and environment-friendly.Physical and Chemical Characterization results show that the betaine had successful introducted,and having a uniform structure.Further research shows that the overall performance chromatography column having an excellent hydrophilic properties.That the monolithic column has showed a significant hydrophilic separation ability of nucleosides,bases,amides,phenols and benzoic acids small polar molecules.3.In order to verify the preparation method of the previous chapter was universality and reliability.A kind of strongly hydrophilic hybrid monolithic column based imidazole group was successfully synthesized by using vinylimidazole as monomer(Preparation method is similar to ammonia ethyl column).The physical and chemical properties as well as the overall performance of chromatography performance have been characterized in detail.The results show that the method is stable,reliable,and good hydrophilic properties being achieved.The hybrid monolithic column was successfully applied to separate several types of small polar molecules efficiently.