Preparing linkage type polysaccharide chiral fixed phase by free radical copoly merization method

A chiral stationary phase and polysaccharide technology, applied in the field of chromatography preparation, can solve the problems of unrealized commercial production, numerous reaction steps, cumbersome operation, etc., achieve wide solvent selectivity, wide application range, and simple production process Effect

Inactive Publication Date: 2005-06-08
萍乡分水科技有限公司
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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)), prepared by photopolymerization Obtain a stationary phase, the process is complicated, and the operation is cumbersome
Tatsumi Murakami (Document 4. Separating agent for optical isomers, its preparation method and application; Tatsushi Murakami, Akito Ichida, 94190414 (1994)) utilizes diisocyanate through the hydroxyl group at the 6-position of polysaccharide derivatives Bifunctional reagents, 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.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Preparation of methacrylate polysaccharide derivatives

[0020] Take 3g of cellulose and place it in a reactor filled with 100mL of pyridine, add 10mL of phenyl isocyanate and 1mL of methacryloyl chloride under stirring conditions, heat up the reaction system to 80°C, and react for 10 hours under the protection of nitrogen; cool to After room temperature, a large amount of methanol was added, centrifuged, and the solid was collected and dried for future use.

[0021] 2) Preparation of Acrylate Silica Gel Derivatives

[0022] The silylating reagent γ-methacrylateoxypropyltrimethoxysilane (12mL) containing methacrylate was placed in a reactor filled with toluene solvent, and reacted with chromatographic silica gel (6g) carrier (5 μ, 200 Å) , to obtain methacrylate silica gel derivatives;

[0023] 3) By-radical copolymerization

[0024] The methacrylate polysaccharide derivatives prepared above are coated on the surface of the obtained methacrylate silica gel derivat...

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Abstract

The invention relates to preparation of chromatogram, which concretely is using free radical polymerization method to prepare linking polysaccharide chiral stationary phase ,including the following steps of reaction: 1) prepare derivative of polysaccharide containing methacrylate; 2)prepare derivative of silica gel 3) free radical polymerization reaction . Its advantages are high efficiency of chiral stationary phase prepared, wide field of use, suitable for each kind of mibile phase, sample and rapid preparation.

Description

technical field [0001] The invention relates to the preparation of chromatography, in particular to the free radical copolymerization method for 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 chir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
Inventor 邹汉法陈小明秦峰刘月启
Owner 萍乡分水科技有限公司
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