A Study On The Preparation And Separation Of Cellulose Tribenzoate As Chiral Stationary Phase

With the development on the research of chiral chemical compound, application of chiral split technology on pharmacy and pharmic intermediate was taken into account progressively. Chiral stationary phase split technology has the advantages of high split efficient, low running cost and non-pollution, which makes it widely used among many chiral split technologies.The prospective were studied on this thesis. The preparation and evaluation of cellulose tribenzoate were committed from the synthesis, steep of stationary phase and characterization of stationary phase by high performance liquid chromatography.Through changing synthetical catalyzer and improving the reaction condition, the damage of burn in reaction was alleviated. Also, the crystal craft was optimized to improve the product quality and overall reaction yield,and got high qualified and pure cellulose tribenzoate. The prepared cellulose tribenzoate was evaluated by elemental analysis and IR spectrum analysis. It showed better results than those reported from literature and proved that the optimization of crystal craft contributed improving the purity of cellulose tribenzoate。By comparison of cellulose tribenzoate coated alkylating silica gels via multiple method of steep, isometric steep method was ultimately chosen to get uniform-coated and high quality chiral stationary phase without particle agglomeration. φ5μm andφ40μm carrier were used to prepare the chiral stationary phase for high performance liquid chromatography and preparative chromatography under the necessity of application. Comparing the isometric steep and no-isometric steep,the distribution of particle diameter and distribution of pore diameter data during the steep of different particle diameter were measured and discussed in detail. The result showed that the method of isometric steep was better than the method no-isometric steep.The cellulose tribenzoate coated chiral stationary phase was evaluated by system of high performance liquid chromatography. For the analysis of actual situation, appropriate mobile phase, flow rate and detector were chosen by impulse input method to get a series of chromatographic peaks in this thesis. By argumentation, the prepared cellulose tribenzoate have high chiral split ability. Origin 7.0 and Peak Fitting Module 7.0 software were used to fit the experimental data for math model based on the Gauss formula and these results were compared. From the discussion, it could be seen that the math model based on the Gauss formula can fit the chromatographic peaks well under the lower input volume and the fitted correlation coefficient was higher than 99%. Under higher input volume,however, the math model based on the Gauss formula had more fitting deviation, because thechromatographic column was overloaded and chromatographic peak was severely asymmetry .A advanced cellulose tribenzoate preparative method by advanced synthetic method, optimization of crystal craft and the method of isometric steep was reported in this thesis, which supported the base of chromatographic analysis, chromatographic separation, simulated moving bed to split chiral compound by cellulose tribenzoate as chiral stationary phase in lab and industry.