Preparation Of Core-shell Silica Gel Materials And Its Application In Glycopeptides Enrichment

The development of chromatographic packing materials has always been the core of the development of chromatographic technology.Non-porous silica packing materials can be used for rapid analysis of biological macromolecules.This kind of stationary phase has no pores on the surface,which eliminates the residual flow of solute on the stationary phase,so the separation rate is obviously accelerated.However,its disadvantage is that the column capacity is small.The biggest bottleneck in the development of totally porous silica microspheres is the wide particle size distribution,and the use of screening technology does not result in fully porous silica microspheres with a narrow particle size distribution.Core-shell silica packing has the advantages of narrow particle size distribution,solid sphere and shallow pore structure,which is not only shortens the diffusion distance inside the particle,reduces the resistance of mass transfer and accelerates the separation speed,but also avoids the problem of excessive column pressure of small particle size packing.It has been widely used in ultra performance liquid chromatography(UPLC).In order to address the problems encountered in preparation and chromatographic application of core-shell microspheres,in this thesis we use a hard template method to synthesize nano core-shell silica microspheres materials.The prepared particle diameter is 160-340 nm and the thickness of the shell is 25-83 nm.The shell of preparation process only requires one step reaction.The prepared core-shell silica microspheres have a pore structure that diverges from the center to the outside,and have been successfully applied in the glycopeptide enrichment.In order to solve the problem of poor specificity and low sensitivity of commonly used hydrophilic chromatographic materials during glycopeptide enrichment,we prepared glutathione functionalized core-shell silica gel microspheres by light-induced thiol-ene click polymerization.The hydrophilic core-shell silica microspheres have a detection limit of 700 fmol IgG digests,and the adsorption capacity is 35 ?g IgG digests.Furthermore,the hydrophilic chromatographic stationaryphase was applied to enrich glycopeptides in complex peptide mixtures,and the results showed that it had high selectivity for glycopeptides enrichment.Furthermore,this study focused on exploring an effective method of preparing micron core-shell silica microspheres to meet the growing demand for separation and analysis of biomedical macromolecules by high performance liquid chromatography.In this paper,the phenolic resin and silica source are coated on the surface of non-porous silica by hard template method,and the final micron-sized core-shell silica particles are obtained after subsequent sintering and pore expansion.At present,the experiment is in process of preparation optimization,which is expected to be applied in biological analysis and catalysis and other fields.