Method of fust preparing linkage type polysaccharide chiral fixed phase

Abstract

A method for synthesis of linking polysaccharide chiral stationary phase, includes the following steps: 1) in the reactor with organic solvent, polysaccharide and derivative solvent of polysaccharide react with including functional group which can react with polysaccharide hydrocarbon radical, then though centrifugal separation the solid substance is collected; 2) coat the prepared polysaccharide derivative containing trihydroxyme or on the surface of silica gel matrixof chromatogram filler, then they are mixed with toluene and pyridine in reactor , cooled after reaction, then use tetrahydrofuran and carbinol separately to wash the creature, which are dried in vacuum, acquiring the linking polysaccharide chiral stationary phase. Its advantages are: wide field of use, simple and rapid preparation.

Description

technical field [0001] The invention relates to the preparation of chromatography, in particular to a method for rapidly preparing bonded polysaccharide chiral stationary phase. Background technique [0002] Polysaccharide chiral stationary phases show great advantages in the separation and preparation of chiral enantiomers, and have very broad application prospects. At present, the commercialized polysaccharide derivative stationary phase adopts the method of physical coating to immobilize the polysaccharide derivative on the chromatographic matrix, so there is a problem of chiral selective agent loss, and the components of the mobile phase are affected in practical applications. Larger restrictions. Due to this disadvantage, some enantiomers have very low solubility or even insolubility under suitable mobile phase conditions on such stationary phases, thus limiting their use in chiral separation applications. The preparation of polysaccharide chiral stationary phase by c...

AI Technical Summary

Problems solved by technology

Functional groups with polymerization properties are introduced into polysaccharide molecules under the action of light (document 3. Photochemically cross-linked polysaccharide derivatives as supports for the chromatographic separation of enantiomers; E.Francotte, PCT WO 96 / 27615 (1996).), through photopolymerization The stationary phase is prepared by the action, the process is complicated and the operation is cumbersome

Tatsumi Murakami et al. (Document 4. Separating agent for optical isomers, its preparation method and application; Tatsumi Murakami, Akito Ichida, 94190414 (1994)) through the hydroxyl on the 6-position of polysaccharide derivatives, using two Isocyanate difunctional reagent, cross-linking polysaccharide derivatives to the surface of silica gel, is a selective immobilization method, with many reaction steps and long time

[0003] Therefore, the chemically bonded polysaccharide chiral stationary phase has not yet been commercially produced, and it is urgent to develop a fast and simple chemical bonding method.