Preparation method of coating-type polysaccharide chiral stationary phase

A technology of chiral stationary phase and polysaccharides, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of inability to coat polysaccharide derivatives, inability to prepare chiral immobilization, etc., and achieve good stability

Inactive Publication Date: 2012-04-25
WUHAN INSTITUTE OF TECHNOLOGY
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  • Abstract
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Problems solved by technology

But some polysaccharide derivatives can not be dissolved in general organic solvents, such as cellulose three (3,5-dimethylbenzoate) etc. (Y.Okamoto, R.Aburatani, K.Hatada, Chromatographic chiral resolution XIV. Cellulose tribenzoate derivatives as chiral stationary phases for high-performance liquid chromatography, Journal of chromatography, 389 (1987) 95.), with the above method, these polysaccharide derivatives cannot be coated on the surface of the carrier, and cannot be prepared as chiral immobilized Mutually

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  • Preparation method of coating-type polysaccharide chiral stationary phase
  • Preparation method of coating-type polysaccharide chiral stationary phase
  • Preparation method of coating-type polysaccharide chiral stationary phase

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Embodiment 1

[0043] A method for preparing a coated polysaccharide chiral stationary phase (or called: cellulose-tris(3,5-dimethylbenzoate)-silica gel composite chiral stationary phase), specific steps as follows:

[0044] 1) Preparation of cellulose solution,

[0045] First put the dry cellulose (0.70g) in a three-necked flask, add dimethylacetamide (25mL), protect it under nitrogen, stir and activate at 160°C for 1h, cool, filter, and wash with acetone several times, and then the fiber The element was dried under normal pressure at 60°C. Take dry LiCl (6.50g) (dried at 200°C for 4h before use) and dimethylacetamide (65mL) in a three-necked flask, heat to 100°C, after LiCl is completely dissolved in dimethylacetamide, add dry For good cellulose, cool down to 80°C, stir to dissolve for 3 hours, and cool to room temperature. Then the cooled solution was heated to 80°C, stirred for 2h, and cooled to room temperature. The cooled solution was centrifuged to obtain a clear cellulose solutio...

Embodiment 2

[0055] Embodiment 2: Preparation of starch-three (3,5-dimethylphenylcarbamate)-silica gel composite chiral stationary phase,

[0056] 1) preparation of starch solution,

[0057] Amylose (4.02g) was added into cold distilled water (396mL), then heated to boil, stirred to dissolve, and cooled to obtain a 1wt% clear starch solution.

[0058] 2) coating of starch (preparation of starch-silica gel composite),

[0059] The obtained starch solution (380.47g) was divided into 7 equal parts, and the first part was mixed with dry blank silica gel (13.49g), and then distilled under reduced pressure at 70°C with a rotary evaporator. After evaporating to dryness, repeat the above-mentioned coating operation 6 times with the remaining starch solution, and use the same amount of starch solution each time to obtain a white powdery product (starch-silica gel composite 17.21g) after drying, and the coating amount is 28.2%. .

[0060] 3) Preparation of starch-tris(3,5-dimethylphenylcarbamate)...

Embodiment 3

[0067] Preparation of chiral stationary phase of chitosan-tris(4-methylphenylcarbamate)-silica gel composite

[0068] 1) preparation of chitosan solution,

[0069] Weigh 2.52g of chitosan and add it into 1wt% hydrochloric acid (198mL), stir and dissolve to obtain a 1wt% clear chitosan solution.

[0070] 2) coating of chitosan (preparation of chitosan-silica gel composite),

[0071]Get the prepared chitosan solution (180.41g) and dry blank silica gel (10.42g) and mix evenly, under the condition of stirring, dropwise add precipitating agent sodium hydroxide solution (1wt%) until the solution becomes neutral, filter and wash with distilled water 3 times until chloride ions are no longer detected with an aqueous solution of silver nitrate. After drying, a white powdery product (12.04 g of chitosan-silica gel composite) was obtained, and the coating amount was 14.8%.

[0072] 3) Preparation of chitosan-tris(4-methylphenylcarbamate)-silica gel complex (derivatization of chitosan-...

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Abstract

The invention relates to a preparation method of a chiral stationary phase. A preparation method of a coating-type polysaccharide chiral stationary phase is characterized in that the method comprises the following steps: 1) coating polysaccharides on a silica gel surface to obtain a polysaccharide-silica gel compound; 2) performing derivatization of the polysaccharide-silica gel compound by isocyanate or acyl chloride to obtain a derivatized polysaccharide-silica gel compound; 3) performing end blocking of the surface silanol groups of the derivatized polysaccharide-silica gel compound by silane to obtain the coating-type polysaccharide chiral stationary phase. The method can overcome the problem that some polysaccharide derivatives are difficult to be dissolved in common organic solventsand thus can not be coated, and the prepared stationary phase has very good chiral separation capability.

Description

technical field [0001] The invention relates to a preparation method of a chiral stationary phase. Background technique [0002] Many drugs are chiral compounds, and the enantiomers of these compounds often have different physiological and pharmacological activities. For a pair of enantiomers, one enantiomer is effective in treating diseases, while the other enantiomer may not be effective in treating diseases, or even have toxic side effects, so the separation and detection of enantiomers of chiral drugs is of great importance to the pharmaceutical industry. is crucial. At present, a relatively mature method for analyzing and detecting the content of enantiomers is high-performance liquid chromatography. This technology requires the use of chiral stationary phases, and hundreds of chiral stationary phases have been commercialized. So far, some scholars are still studying new chiral stationary phases, or preparation methods of chiral stationary phases. [0003] Natural po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/29B01J20/30
Inventor 陈伟段蓉柏正武尹传奇
Owner WUHAN INSTITUTE OF TECHNOLOGY
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