Purification and separation method of N-acetyl-D-glucosamine

A technology of glucosamine and glucosamine hydrochloride, which is applied in the field of purification and separation of N-acetyl-D-glucosamine, can solve the problems of chemical residues, complex process, cumbersome operation, etc., achieve low cost, simple process, Easy post-processing effects

Active Publication Date: 2020-01-10
SHANDONG RUNDE BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of N-acetyl-D-glucosamine by microbial fermentation requires the cultivation of microbial strains, followed by fermentation, separation and other processes. The whole process is complicated, the operation is cumbersome, and the yield is very low, which is not conducive to industrial production. Chemical production of N -Acetyl-D-glucosamine, the preparation process requires a lot of toxic and harmful chemical reagents, not only there are chemical residues in the product N-...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 1kg chitin powder, add 2.5L lactic acid glycine hydrochloride and 0.85L hydrochloric acid with a mass concentration of 32%, stir and mix at 43°C, and then use a diaphragm pump to continuously pump into a microporous membrane filter for filtration to obtain Filtrate; the obtained filtrate was heated to 68°C, kept warm and added dropwise with hydrochloric acid with a mass concentration of 25%, stirred for 15 minutes, after cooling, added activated carbon for decolorization, concentrated, washed, and dried to obtain D-glucosamine hydrochloride; to the obtained D-glucosamine The ethanol solution of sodium ethylate was added to the hydrochloride, wherein the mass concentration of sodium ethylate in the ethanol solution of sodium ethylate was 57%, and the molar ratio of D-glucosamine hydrochloride to sodium ethylate was 1:6, and the concentration of the reaction solution was controlled. The pH value is 7-8, and the solid chloride salt precipitated by the reaction is filte...

Embodiment 2

[0030] Take 1kg of chitin powder, add 3.0L lactic acid glycine hydrochloride and 1.0L hydrochloric acid with a mass concentration of 30%, stir and mix at 45°C, and then use a diaphragm pump to continuously pump into a microporous membrane filter for filtration to obtain Filtrate; the obtained filtrate was heated to 70°C, kept warm and added dropwise with hydrochloric acid with a mass concentration of 28%, stirred for 10 minutes, after cooling, added activated carbon for decolorization, concentrated, washed, and dried to obtain D-glucosamine hydrochloride; to the obtained D-glucosamine The ethanol solution of sodium ethylate is added to the hydrochloride, wherein the mass concentration of sodium ethylate in the ethanol solution of sodium ethylate is 55%, and the molar ratio of D-glucosamine hydrochloride to sodium ethylate is 1:7, and the concentration of the reaction solution is controlled. The pH value is 7-8, and the solid chloride salt precipitated by the reaction is filtere...

Embodiment 3

[0032]Take 1kg of chitin powder, add 1.0L of lactic acid glycine hydrochloride and 1L of hydrochloric acid with a mass concentration of 35%, stir and mix at 40°C, and then use a diaphragm pump to continuously pump into a microporous membrane filter for filtration to obtain the filtrate The resulting filtrate was heated to 65°C, kept warm and added dropwise hydrochloric acid with a mass concentration of 23%, stirred for 17 minutes, added activated carbon to decolorize after cooling, concentrated, washed, and dried to obtain D-glucosamine hydrochloride; to the obtained D-glucosamine salt Add the ethanol solution of sodium ethylate to the acid salt, wherein the mass concentration of sodium ethylate in the ethanol solution of sodium ethylate is 60%, the molar ratio of D-glucosamine hydrochloride to sodium ethylate is 1:6, and the pH of the reaction solution is controlled The value is 7-8, and the solid chloride salt precipitated by the reaction is filtered to obtain the free D-gluc...

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Abstract

The invention belongs to the field of pharmaceutical chemicals, and discloses a purification and separation method of N-acetyl-D-glucosamine. The purification and separation method of the N-acetyl-D-glucosamine comprises the following steps: adding lactic acid glycine hydrochloride and hydrochloric acid into chitin powder, performing mixing, and performing filtering to obtain a filtrate; performing heating, adding hydrochloric acid dropwise, performing stirring, performing cooling, and performing decoloring to obtain D-glucosamine hydrochloride; adding an ethanol solution of sodium ethoxide, and performing filtering to obtain a free D-glucosamine solution; adding acetic anhydride to obtain a solution containing the N-acetyl-D-glucosamine; and performing concentration, performing cooling, performing crystallizing, performing filtration to obtain an N-acetyl-D-glucosamine crude product, performing soaking by using absolute ethyl alcohol, performing stirring, performing filtration, and performing drying to obtain the high-purity N-acetyl-D-glucosamine. According to the method, the N-acetyl-D-glucosamine with the purity of 99.95% or above can be obtained, the technological process is simple, the post-treatment is easy to realize, the cost is low, the used alcohol solvent can be recycled, and the method is environmentally friendly, economical and suitable for large-scale promotion and application.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a purification and separation method of N-acetyl-D-glucosamine. Background technique [0002] Amino sugars are generally used as monosaccharide residues in complex oligosaccharides and polysaccharides, glucosamine is an amino derivative of monosaccharide glucose, and N-acetyl-D-glucosamine is an acetylated derivative of glucosamine. It is a special monosaccharide with high sweetness, has reducing properties, and is also an important precursor for the synthesis of bifidus factors. It has many important physiological functions in organisms and is clinically used as a drug for treating rheumatism and rheumatoid arthritis. , It can also be used as food antioxidant and infant food additive or sweetener for diabetic patients. At the same time, it can enhance the function of the human immune system, inhibit the excessive growth of cancer cells or fibroblasts, and inhibit a...

Claims

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Application Information

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IPC IPC(8): C07H1/06C07H5/06
CPCC07H1/06C07H5/06
Inventor 卢健行刘长峰韩宁卢建功马善丽张建华
Owner SHANDONG RUNDE BIOTECH CO LTD
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