Preparation Of Two Novel Chiral Stationary Phases Based On Silica Microspheres And Their Applications In The Separation Of Chiral Drugs

Separation of chiral compounds is an important topic in the biomedical field.Enantiomers of the same chiral drugs have similar physical and chemical properties,but there may be differences in pharmacodynamics,pharmacodynamics and toxicity.The progress in separation and detection methods enables the analysis of trace chiral compounds in the environmental media.The splitting of chiral drugs is important for the development of safer and more active drugs.In this paper,the preparation method of micron class silica microsphere is optimized,using photodiazride resin(DR)as the coupling agent to connect two newly synthesized chiral recognized molecules to the surface of silica microsphere,thus constructing two different separation systems and exploring the separation properties of different separation systems.The work performed in this paper includes:1.We optimize the preparation method of the medium porous silica microsphere,so that the silica particle size can reach 3.2?m-5?m,and the dispersed uniform silica microspheres of any particle size can be prepared.In addition,by adjusting the reaction parameters,the aperture of the microsphere can change between 12.15 nm-17.12 nm,truly realizing the controllable particle size and the adjustable pore size of the microsphere.At the same time,the prepared silica microspheres have very high mechanical strength and can meet different degrees of application.This experiment is of important significance for the preparation of micron silica microspheres.2.In the first time we connect 3,5-dichlorobenzene isocyanate to?-cyclodextrin.We use diazide as a coupling agent to connect the cyclic dextrin to the silica microspheres.We performed C18 modification of two particle size microspheres,and compared the separation properties of two C18 modified microsphere for benzene and benzene,and showed the highest column effect of silicon dioxide microspheres with small particle size.We present a detailed study of the chiral fixed relative twelve chiral imantiers prepared with silica microspheres of3.2?m.The results revealed a successful separation of three chiral drugs,including antimean diethylene oxide,2-phenylcyclohexone,and isopromazine.Chroographic evaluation shows that the prepared?-CD-DCIPI@Si O₂chromatographic columns have good chiral ability and chemical stability.We effectively solve the problem of large chromatographic column loss,high separation cost,low separation column efficiency and single separable samples.The experiment has broad application prospects for the analysis and preparation of new chiral stationary phase.3.To contrast the differences between the separation of methyl substituents and chloride substituted antagonists,the 3,5-dimethyl phenylisocyanate was connected to the?-cyclodextrin.It is connected to the silica microsphere surface with the diazride resin as a coupling agent.Twelve chiral enantiomers were studied detail using prepared chromatographic columns and showed successful separation of 2-phenyl cyclohexone.Chmatographic evaluation shows that the prepared?-CD-DPIC@Si O₂chromatographic column has chiral separation characteristics compared with the?-CD-DCIPI@Si O₂chromatographic column,and the separable chiral drugs are relatively single.