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Preparation method of chitin oligose with single degree of polymerization

A technology of chitosan oligosaccharide and degree of polymerization, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc. , The effect of reducing production costs and stabilizing the production process

Inactive Publication Date: 2019-03-26
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a preparation method of chito-oligosaccharides with a single degree of polymerization, to solve the problems in the prior art that the mass production of chito-oligosaccharides with a single degree of polymerization cannot be realized.

Method used

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  • Preparation method of chitin oligose with single degree of polymerization
  • Preparation method of chitin oligose with single degree of polymerization
  • Preparation method of chitin oligose with single degree of polymerization

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preparation example Construction

[0034] In the specific implementation process, the preparation method of chitosan oligosaccharide with a single degree of polymerization of the present invention comprises the following steps:

[0035] (1) Use a pulverizer to pulverize the flake chitin to an appropriate particle size, generally about (80-200 mesh).

[0036] (2) Chitin particles are dispersed in a solvent with 5 times to 50 times the mass, and under strong stirring, chitin dissolves or fully swells in the solvent.

[0037] (3) The reactants are kept at 0°C to 100°C for 1 to 10 hours, the chitin begins to degrade, and the molecular weight gradually decreases. By controlling the reaction temperature and reaction time, chitooligosaccharide solutions with different polymerization degree distributions are obtained.

[0038] (4) methods such as vacuum decompression evaporation solvent, alcohol precipitation, etc. are used to remove the reaction liquid solvent.

[0039](5) After dissolving and filtering chitosan olig...

Embodiment 1

[0044] In the present embodiment, the preparation method of single degree of polymerization chitosan oligosaccharide is as follows:

[0045] At 10°C, 10 g of chitin was slowly added into 200 mL of concentrated hydrochloric acid (36 wt%). After stirring for 6 hours, the chitin was completely dissolved. Raise the reaction temperature to 30° C., stir for 1.5 hours, and then slowly add NaOH solid powder to the reaction solution to neutralize the reaction solution. 1000 mL of ethanol was added to the reaction solution for alcohol precipitation, and the precipitated solid precipitate was filtered, washed with ethanol, and air-dried to obtain 6 g of chitooligosaccharide mixture.

[0046] Take 107mg of chitosan-oligosaccharide mixture, add 4mL of water, dissolve and then add 6mL of acetonitrile, shake well and pass through the membrane, the injection volume is 10mL. Use amide column (XAmide, 50*250mm, 275g) for separation and purification at a flow rate of 70mL / min. In the mobile...

Embodiment 2

[0054] The difference from Example 1 is that in this example, the preparation method of chitosan oligosaccharide with a single degree of polymerization is as follows:

[0055] At 30 °C, 10 g of chitin was slowly added to 500 mL of hexafluoroisopropanol. After stirring for 6 hours, 25 mL of concentrated hydrochloric acid was added after the chitin was completely dissolved. Raise the reaction temperature to 50° C., stir for 1.2 hours, and then spin-evaporate in vacuum at 50° C. to evaporate and recover most of the reaction solvent. The reaction product was washed with ethanol, filtered, and air-dried to obtain 7 grams of chitooligosaccharide mixture.

[0056] Take 500mg of chitosan oligosaccharides, add 20mL of water, dissolve and then add 30mL of acetonitrile, shake well and pass through the membrane, the injection volume is 50mL. Use amide column (XAmide, 100*250mm, ) for separation and purification at a flow rate of 280mL / min. In the mobile phase, phase A is acetonitrile...

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Abstract

The invention relates to the technical field of fine chemical engineering and particularly relates to a preparation method of chitin oligose with a single degree of polymerization. The preparation method comprises the following steps: dissolving or adequately swelling chitin into a certain solvent, carrying out uniform-phase degradation under an acid catalysis condition so as to obtain chitin oligose mixtures with different degrees of polymerization; dissolving the chitin oligose mixtures, filtering insoluble parts, and carrying out separation and purification by virtue of an efficient preparative chromatography; and collecting eluant at different time periods, removing the solvent in the eluant, and drying, so as to obtain the chitin oligose with the single degree of polymerization. According to the preparation method, high-purity chitin oligose products with degrees of polymerization of 2-10 can be prepared, the yield in the preparation process is high, byproducts are few, the production cost is greatly lowered, meanwhile, the production process is stable, the repeatability is good, the operation is simple, convenient and controllable, and the preparation method is suitable for batch production of high-performance chitin oligose products.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of chito-oligosaccharides with a single degree of polymerization. Background technique [0002] Chitin, also known as chitin, is a polymer composed of varying numbers of N-acetylglucosamine (GlcNAc) linked by β-1,4-glucosidic bonds. It has a structure similar to that of cellulose and is widely used. Existing in the shells of marine crustaceans, the inner skeletons of molluscs, insect wings, fungi and algae cell walls, it is the natural polysaccharide and the second largest renewable resource on earth after cellulose reserves. It is estimated that natural organisms can produce 100 billion tons of chitin per year, of which 2 million tons are used by modern industries. With the depletion of fossil resources and the continuous increase in costs, chitin and other biomass resources are used as raw materials for development. Fine chemicals have important res...

Claims

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Application Information

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IPC IPC(8): C07H13/06C07H1/00C07H1/06C08B37/08
CPCC07H1/00C07H1/06C07H13/06C08B37/003
Inventor 赵岩郭志谋张文昌金高娃张劲松梁鑫淼
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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