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Preparation method of high-purity N-acetyl-D-glucosamine

A glucosamine, high-purity technology, applied in the field of preparation of high-purity N-acetyl-D-glucosamine, can solve the problem that it is difficult to ensure the yield and purity of the final product, the recrystallization conditions of multi-impurity crude products, and the high price of chitinase. problem, to achieve the effect of high product purity, simple preparation process and high cost

Active Publication Date: 2016-07-13
厦门蓝湾科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One is through the method of chemical synthesis, using (GAH) as raw material, acetic anhydride as acylating reagent, adding silver acetate, anhydrous methanol or pyridine to react at a certain temperature, the reaction process of this method is relatively complicated, and it is easy to produce more impurities Moreover, the recrystallization conditions of the crude product are harsh, and it is difficult to ensure the yield and purity of the final product. At the same time, the use of glucosamine hydrochloride as a raw material is costly
The second is to use enzymatic hydrolysis, using chitin as raw material, and adding specific chitinase can obtain GlcNAc with higher purity, but the high price of chitinase will greatly increase the preparation cost

Method used

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  • Preparation method of high-purity N-acetyl-D-glucosamine
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  • Preparation method of high-purity N-acetyl-D-glucosamine

Examples

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Effect test

Embodiment 1

[0033] Weigh 20 g of chitin, add 80 mL of sulfuric acid with a mass concentration of 60%, and keep the temperature in a water bath at 60°C. After the degradation reaction at this temperature for 14 hours, unreacted chitin is removed by filtration. Sulfuric acid is removed by diffusion dialysis until the mass concentration of sulfuric acid is below 5%, and calcium hydroxide solid is added to adjust the pH of the solution to 5.5-7.0. Remove the precipitate by filtration, decolorize the filtrate with activated carbon, add absolute ethanol and stir, and collect the precipitate by filtration after the precipitation is complete. Slowly add purified water, while stirring, until the precipitate is just completely dissolved. Anhydrous ethanol was added again for recrystallization, and the precipitate was collected by filtration after the precipitation was complete. The obtained solid is dried under normal pressure to obtain the product N-acetyl-D-glucosamine, and the sample is assayed...

Embodiment 2

[0035] Weigh 20 g of chitin, add 40 mL of sulfuric acid with a mass concentration of 70%, and keep the temperature in a water bath at 40°C. After the degradation reaction at this temperature for 10 h, unreacted chitin is removed by filtration. Sulfuric acid is removed by diffusion dialysis until the mass concentration of sulfuric acid is below 5%, and calcium hydroxide solid is added to adjust the pH of the solution to 5.5-7.0. Remove the precipitate by filtration, at this time, the product in the filtrate is as figure 1 As shown, the filtrate was decolorized by activated carbon, then added absolute ethanol and stirred, and the precipitate was collected by filtration after the precipitation was complete. Slowly add purified water, while stirring, until the precipitate is just completely dissolved. Anhydrous ethanol was added again for recrystallization, and the precipitate was collected by filtration after the precipitation was complete. Gained solid obtains product N-acetyl...

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Abstract

The invention provides a preparation method of high-purity N-acetyl-D-glucosamine, and relates to monosaccharide. The invention provides the preparation method of the high-purity N-acetyl-D-glucosamine with the advantages that the operation is simple, the production cost is low, and economy and environment-friendly effects are achieved. The method comprises the following steps of (1) chitin is used as a raw material, and a degradation agent of sulphuric acid is used for performing degradation reaction on the chitin; (2) filtering is performed to remove unreacted chitin, and unreacted sulphuric acid is removed by a membrane method; (3) calcium hydroxide solid is added into a solution subjected to unreacted sulphuric acid removal by the membrane method, and the pH value is regulated to be 5.5 to 7.0; (4) separated precipitates are removed through filtering, and the filtered solution is decolored by activated carbon; (5) absolute ethyl alcohol is added into the decolored solution until no precipitates separate out; (6) the precipitates are filtered and collected; the precipitates are dissolved by water; then, the absolute ethyl alcohol is added for separating out solid; next, the solid is collected and dried, and the product of N-acetyl-D-glucosamine powder is obtained. The product purity can be greater than 98 percent.

Description

technical field [0001] The invention relates to monosaccharides, in particular to a method for preparing high-purity N-acetyl-D-glucosamine. Background technique [0002] N-Acetyl-D-glucosamine (N-Acetyl-D-(+)-glucosamine, GlcNAc) is an endogenous monosaccharide, and current studies have shown that it can treat osteoarthritis, rheumatoid arthritis and anti-inflammatory Oxidation, antibacterial, antitumor and other effects. In addition, it also has a wide range of functions such as stabilizing cardiomyocytes and anti-oxidative stress. In terms of practical applications, GlcNAc has important applications in the fields of medicine, food and fine chemicals, and can be used as sweeteners for diabetics, food antioxidants and food additives for infants and young children. [0003] At present, there are two main methods for the preparation of GlcNAc. One is through the method of chemical synthesis, using (GAH) as raw material, acetic anhydride as acylating reagent, adding silver ...

Claims

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Application Information

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IPC IPC(8): C07H5/06C07H1/00C07H1/06
CPCC07H1/00C07H1/06C07H13/06
Inventor 石国宗王锌源吴招斌邓美健张慧兰孙丽
Owner 厦门蓝湾科技有限公司
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