Study On Preparation And Property Of Novel Organic-inorganic Hybrid Polysaccharide-based Chiral Stationary Phases

Polysaccharide derivatives are widely used for the preparation of chiral stationary phases(CSPs) for high-performance liquid chromatography (HPLC) due to their excellent chiral recognition abilities. Until now, Most of Polysaccharide chiral stationary phases are prepared by coating or immobilizing chiral selectors on the surface of inorganic silica gel. This limits the column capacity because the chiral selector density is only 20%-25%. Thus limiting chiral stationary phases application in the field of preparative chromatography and large scale chromatographic separations.To improve the capacity of CSPs, the Okamoto group first reported the synthesis of Organic-inorganic hybrid particles for enantioseparation.Importangtly the materisls also has excellent mechanical strength. However, this material was not processed, it was easy to trial because of too much Si-OH, which might result in the degress of chiral separation.Meanwhile we could not see any study about amylose in organic-inorganic hybrid particles.Based on this background, This topic of polysaccharide derivatives based preparation methods of organic inorganic hybrid silicon particles to explore, trying to develop a series of new type with a high proportion of cellulose derivatives of organic inorganic hybrid silicon particles and optimize the preparation method.A series of cellulose phenylcarbamate derivatives bearing different groups at 2-, 3- and 6-postions of a glucose unit were synthesized. Firstiy, the cellulose 3,5-dimethylcarbamate containing a small number of 3-(trimethylsilyl)propyl groups was obtained and the chemical structure was then confirmed via FT-IR and 1H NMR. By partical size distribution analysis and TGA for the information ahout proportion of organic and inorganic ingredient.Quantitative determination the proportion of the two kinds of isocyanate of the cellulose and amylose, and priority to choose the structure of cellulose and amylose senior damage small ratio of about 98:2 of derivatives as a subsequent reaction of the reactants.This topic studied two kinds of derivatives associated with TEOS by sol-gel reaction method. We can see chiral stationary phase material particle size, morphology, and the proportion of organic and inorganic determined by SEM and TGA. and evaluation criteria,examines the sol-gel reaction of TEOS, water, trimethyl chlorosilane in stationary phase material particle size, morphology, and the influence of the proportion of organic and inorganic, surface active agent, stirring speed in the process of the gel and its influence on microspheres particle size and uniformity.Results show that when the polysaccharide derivatives of inorganic content was 2%, the organic inorganic hybrid silicon particle is more uniform, and amylose derivatives have more advantages in the high content of inorganic scale,particle uniformity is more stable;In optimizing the preparation technology of two kinds of polysaccharide derivatives performance study found that only in the condition of 2 mL TEOS, 2 mL water, 0.5 mL trimethyl chlorosilane, the dosage of surface active agent is 0.2%, stirring speed is 1100 rpm,which we can get the most complete silicon morphology.