| High performance liquid chromatography(HPLC)as a kind of high efficient,novel,the rapid separation and analysis technology,is one of the widely used means of analysis.Now the HPLC is a method of separation which is the most commonly used in many fields such as chemical,food,health,drug testing,environmental monitoring.Chromatographic column is the "heart" of high performance liquid chromatography(HPLC),and the chromatographic packing is the basis of the establishment and development of all kinds of HPLC separation mode,so the high performance chromatographic column packing is the most abundant,dynamic and creative part in the chromatographic study.At present,silica microspheres have become the most commonly used inorganic matrix chromatographic filler,mainly because of its advantages of high mechanical strength and easy surface modification.In addition,styrene-divinylbenzene polymer microspheres have been widely used in organic matrix chromatography packing.This paper combines of advantages of inorganic and organic matrix substrate stationary phase,studied the synthesis and functionalization of modified silica microspheres as well as the preparation of porous cross-linked polystyrene microspheres and functional modification respectively,and further researches the prepared new type of chromatographic stationary phase used for chromatographic separation field,the main work is as follows:1.Using the improved Stober method to prepare monodisperse silica microspheres,the particle size of Si O2 microspheres can be controlled between 2-5 ?m by changing the temperature and the amount of ammonia.With a particle size of 2.4 ?m silicon spheres as a fixed phase matrix,a water-soluble non-toxic light-sensitive polymer heavy nitrogen resin(DR)was used to replace the more toxic silica microsphere surface for functional modification.Using diazo resin itself unique optical properties,through UV exposure,induction of diazo resin in situ cross-linking reaction,thus in the introduction of covalent bond and the surface of the silica microspheres,hydrophilic and hydrophobic group of benzene ring secondary amino group.Finally,using the modified silica microspheres as the stationary phase of chromatographic column,the separation and application of mixed mode in liquid chromatography were realized.2.The improved Stober prepared particle size is about 2 ?m(includingmonodisperse silica microspheres,photosensitive polymer diazo resin as a bridge,in situ by using light cross-linking reaction and the layers of the principle of self-assembly,the macrocyclic sugar peptide vancomycin modifications in the surface of silica,formed a new type of vancomycin chiral stationary phase.In addition,the chiral separation of chiral drugs in different liquid chromatographic separation modes can be achieved by the novel chiral stationary phase of vancomycin.Using chlorpheniramine maleate and benzoin chiral drugs as samples,explores the new chiral stationary phase in the chromatographic pattern and reverse phase chromatography separation performance of the mode,and further explores the stability and repeatability of the chromatographic stationary phase.3.Monodisperse porous cross-linked polystyrene microspheres were successfully prepared with the improved two-step seed swelling methord.Furthermore taking the sulfonated porous cross-linked polystyrene microspheres as a chromatographic column packing,not only keep a low column pressure in the high velocity,and successfully realized the separation of organic acids.This paper studies the use of the optical properties of diazo resin to the functional modification of silica microspheres as well as the simple sulfonation modification to porous cross-linked polystyrene microspheres,both are effective,stable,simple,the modification methods of green environmental protection.The preparation technology of these new column packing is of great significance for the future development of high performance liquid chromatography column packing. |
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