Preparation Of Novel High Performance Liquid Chromatography Stationary Phase And Its Chromatographic Properties

High performance liquid chromatography(HPLC), known as an important analytical separation method, has been widely used in many fields such as petrochemical engineering, food, chemistry, pharmaceutical and life science. The stationary phase is the core of chromatographic separation, its performance is directly related to the efficiency of separation and accuracy of test results. Therefore, the research and development of new column packing materials has always been a hot topic in the field of chromatography.The stationary phase can be generally divided into three categories based on the different matrix: inorganic, organic and organic-inorganic packing materials. Silica(SiO2)spheres have become the most commonly used inorganic stationary phase matrix of HPLC due to its high mechanical strength, good biocompatibility, rich surface groups, etc.And styrene-divinylbenzene copolymer(PS-DVB) is most widely used as organic matrix materials. On the combination of advantages of inorganic and organic materials, a new modified method of silica and preparation of porous cross-linked polystyrene microspheres were respectively studied. The new stationary phases were detected on HPLC and achieved good results, the main work is as follows:1. Monodisperse silica spheres with an average particle size of about 2.5 μm were successfully prepared using a modified sol-gel method(St?ber method). The functional modification of silica spheres has been achieved by replacing toxic silane reagent with the water-soluble photosensitive polymer DR basing on the reaction principle of photo-crosslinking. Under the effect of ultraviolet irradiation, in situ crosslinking reaction was induced by photosensitive polymer, thereby introducing covalently bonded functional groups on the surface of silica spheres. Depending on the chemical structure of DR and mobile phase composition, the modified silica spheres can perform two different kinds of separation mechanisms and have achieved good results.2. Monodisperse poly(styrene-co-divinylbenzene)(PS-DVB) microspheres with binary porous structures were synthesized using a modified seeded polymerization method. Using the binary porous PS-DVB(BPPSD) microspheres as packing materials for HPLC, several benzene analogs as same as C60 and C70 were effectively separated.And the back pressure of BPPSD column could be maintained at especially low level even at high flow rates due to the excellent permeability of the fillers.This study gives a new modified method of silica spheres for chromatography which combines the advantages of physical adsorption and chemical bonding method. The easyand quick modification of silica spheres can be achieved only by UV irradiation cross-linking and the results have proved it is an efficient, stable and green method. And the prepared porous polystyrene spheres can effectively reduce the column pressure and improve the efficiency of separation. These new preparation techniques have certain significance to help optimize the preparation process of stationary phase for HPLC.