Preparation method of water-soluble chitosan-oligosaccharide

A technology of chitooligosaccharide and water-solubility, applied in the field of preparation of chitooligosaccharide, can solve the problems of low molecular weight, influence product quality, poor physiological activity of the product, etc., and achieve the purpose of reducing production requirements and production costs, and facilitating purification and separation. Effect

Inactive Publication Date: 2012-11-21
ZHEJIANG OCEAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as the patent No. ZL200510009669.8 Chinese invention patent "preparation method of water-soluble chitosan oligosaccharides" (authorization announcement number is CN1283668C), this patent is hydrolyzed with hydrogen peroxide after 80~100min, because the hydrolysis reaction is not terminated, directly through Freeze-drying prepared chitosan oligosaccharides, resulting in too low molecular weight of the reaction product, 609 Daltons, resulting in poor physiological activity of the product, and the introduction of Na+ in the reaction, the difficulty of separation seriously affects the quality of the product; then refer to the patent of ZL02135410.3 Chinese invention patent "A Preparation Method of Low Molecular Weight Chitosan" (authorized announcement number is CN1202136C), using H 2 o 2 with FeSO 4 The mixture degrades chitosan and introduces Fe 2+ Difficult to remove, seriously affecting the application value of the product in food and pharmaceuticals
[0007] At present, the research on the degradation of chitosan by hydrogen peroxide is mostly concentrated in the laboratory, and the research on the relevant process parameters in the degradation process, the controllability of the degradation process of hydrogen peroxide and the separation and purification of products in actual production are rarely studied. to report

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: Accurately weigh 10.0 g of chitosan with a degree of deacetylation of 70%, and dissolve it in 0.5% acetic acid solution to prepare a 2% (w / v) chitosan acetic acid solution. The temperature was raised to 55°C, and the molar ratio of chitosan to hydrogen peroxide was 1:1.5, and 2% H was added. 2 o 2 Solution, pH 5.5, after continuous stirring for 70min and hydrolysis, 3ml of hydrolyzate was added to 2ml of 4mol / L NaOH solution without flocculent precipitation. Manganese terminates the reaction until no bubbles are generated, and the reaction solution is filtered to remove MnO 2 (MnO 2 collected and recycled), and the filtrate was spray-dried to obtain a weight-average molecular weight of 80,000 completely water-soluble chitooligosaccharides.

[0024] where, 2% H 2 o 2 The solution is H per 100 ml of water 2 o 2 The mass is 2g.

Embodiment 2

[0025] Embodiment 2: Accurately weigh 10.0 g of chitosan with a degree of deacetylation of 85%, and dissolve it with a 1.0% acetic acid solution to prepare a 3% (w / v) chitosan acetic acid solution. The temperature was raised to 60°C, and the molar ratio of chitosan to hydrogen peroxide was 1:2.0, and 2% H was added. 2 o 2 solution, pH 6.0, after continuous stirring for 1 hour for hydrolysis, the hydrolyzate was added to 4mol / L NaOH solution without flocculent precipitation. Pure manganese dioxide terminates the reaction until no bubbles are generated, and the reaction solution is filtered to remove MnO 2 (MnO 2 collected and recycled), the filtrate was collected and spray-dried to obtain a fully water-soluble chitooligosaccharide with a weight average molecular weight of 10,000.

Embodiment 3

[0026] Embodiment 3: Accurately weigh 10.0 g of chitosan with a degree of deacetylation of 95%, and dissolve it with a 1.5% acetic acid solution to prepare a 4% (w / v) chitosan acetic acid solution. The temperature was raised to 65°C, and the molar ratio of chitosan to hydrogen peroxide was 1:2.5, and 2% H was added. 2 o 2 solution, the pH was adjusted to 6.5, and after continuous stirring for 1 hour for hydrolysis, the hydrolyzate was added to 4mol / L NaOH solution without flocculent precipitation. High-purity manganese dioxide terminates the reaction until no bubbles are generated, and the reaction solution is filtered to remove MnO 2 (MnO 2 collected and recycled), and the filtrate was collected to obtain completely water-soluble chitooligosaccharides with a weight-average molecular weight of 986 through a spray-drying method.

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Abstract

A preparation method of water-soluble chitosan-oligosaccharide comprises the following steps: (1) dissolving chitosan in an acetic acid solution to prepare a chitosan acetic acid solution with a concentration of 2.0-4.0 g/ml; (2) heating to 55-65 DEG C, adding a 1-5% H2O2 solution according to a molar ratio of the chitosan to hydrogen peroxide of 1:1.5-1:2.5, adjusting the pH to be 5.5-6.5, continuously stirring for hydrolyzation to obtain a hydrolysate; (3) sampling, adding strong alkali liquor till no flocculent precipitate is generated so as to determine the hydrolysate; (4) continuously performing hydrolyzation for not more than 2 hours; (5) adding a degradation reaction terminator to obtain a preliminary product; (6) processing the preliminary product by a spray-drying process to obtain the water-soluble chitosan-oligosaccharide. Compared with the prior art, the invention has the advantages that: the degradation reaction terminator is used for controlling the degree of the degradation reaction so as to control the weight average molecular weight of the obtained chitosan-oligosaccharide; real production requirements are met; and large scale production requirements are met.

Description

technical field [0001] The invention relates to a preparation method of chitooligosaccharides. Background technique [0002] Chitin widely exists in the shells of lower plants, fungi, crustaceans and cell walls of higher plants, and is the only positively charged polysaccharide found in nature so far. Chitosan is the product of deacetylation of chitin, which is formed by condensation of 2-amino-2-deoxy-D-glucose with β-1,4 glycosidic bonds. Due to the presence of free amino groups and hydroxyl groups in chitosan molecules, it has special physiological activities, and has excellent performance in antibacterial, hypoglycemic, hypolipidemic, antitumor and immune regulation. However, its large molecular weight and poor water solubility are limited in practical applications. After chitosan is degraded into chitooligosaccharides, its water solubility is greatly improved, and it has many more superior and unique physiological activities than chitosan. Therefore, the preparation o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
Inventor 陈小娥方旭波余辉李振达
Owner ZHEJIANG OCEAN UNIV
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