Preparation method of high quality and high molecular weight carboxymethyl chitosan

A carboxymethyl chitosan and high molecular weight technology is applied in the field of preparation of carboxymethyl chitosan, can solve the problems of difficult isoelectric point control of carboxymethyl chitosan, etc., and achieves long action time and high quality. Good, heat-free effect

Active Publication Date: 2020-04-14
CHANGZHOU INST OF MATERIA MEDICA
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Problems solved by technology

"In this method, it is difficult to control the isoelectric point of carboxymethyl chitosan; in addition, the method of using ethanol to precipitate carboxymethyl chitosan will completely remove all high and low molecular weight carboxymethyl chitosan. Precipitation, that is, the coexistence of high and low molecular weight carboxymethyl chitosan in the obtained product

Method used

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  • Preparation method of high quality and high molecular weight carboxymethyl chitosan
  • Preparation method of high quality and high molecular weight carboxymethyl chitosan
  • Preparation method of high quality and high molecular weight carboxymethyl chitosan

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Embodiment 1）

[0026] The preparation method of the high-quality high molecular weight carboxymethyl chitosan of the present embodiment comprises the following steps:

[0027] ① Preparation of crude carboxymethyl chitosan.

[0028] Add sodium hydroxide in isopropanol solution in the reaction flask, the concentration of sodium hydroxide is 40%.

[0029] Add chitosan with a deacetylation degree of 15% to 45% into the reaction flask, and the mass ratio of chitosan to sodium hydroxide after adding is 1:4.8.

[0030] Slowly add the pre-dissolved isopropanone solution of chloroacetic acid dropwise into the reaction flask under stirring, and continue to stir and react for 3 hours after the addition. The mass ratio of chitosan to chloroacetic acid is 5:1.

[0031] After the reaction is completed, add concentrated hydrochloric acid to the reacted material, adjust the pH value of the material to 6-7, filter with suction, wash the filter cake 3 times with absolute ethanol, and dry the washed filter c...

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Abstract

The invention discloses a preparation method of high-quality high-molecular-weight carboxymethyl chitosan. The preparation method comprises the following steps: 1, preparing crude carboxymethyl chitosan; 2, dissolving the crude carboxymethyl chitosan prepared in step 1 in distilled water, adding an aqueous solution of hexadecylpyridinium chloride to obtain a precipitate, and carrying out suction filtration to obtain a CPC complex salt of carboxymethyl chitosan; 3, carrying out salting-out to obtain a carboxymethyl chitosan solution; 4, adding anhydrous ethanol to the solution to precipitate carboxymethyl chitosan, and carrying out suction filtration; 5, washing the carboxymethyl chitosan obtained in step 4 through the suction filtration with dimethyl sulfoxide; and 6, carrying out graded alcohol precipitation by using anhydrous ethanol. The carboxymethyl chitosan with the molecular weight being 70-80 W is prepared through the preparation method, and an osteoarticular cavity injection prepared from the prepared carboxymethyl chitosan allows the carboxymethyl chitosan to have a long residence time and a long action time in vivo due to its large molecular weight, and achieves few sidereactions after being injected to the osteoarticular cavity due to its high purity.

Description

technical field [0001] The invention relates to a preparation method of carboxymethyl chitosan with high quality and high molecular weight. Background technique [0002] The recurrent attacks of osteoarthritis and the progressive decline in the function of the affected joints make it an important disease that seriously endangers the quality of life of middle-aged and elderly people. The most essential pathological change of osteoarthritis is the progressive degeneration of articular cartilage, so it can be delayed or even reversed. Cartilage degeneration is the focus of research on the prevention and treatment of osteoarthritis. [0003] Carboxymethyl chitosan can provide a large amount of glucosamine monomer, which is not only the basic nitrogen source of proteoglycan, an important component of cartilage matrix, but also the material basis for cartilage to have good viscoelastic properties. In recent years, studies have shown that such biological agents can improve cartila...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/08
CPCC08B37/0003C08B37/003
Inventor 黄金钱何浩明杨子中朱莲邱鑫鑫夏青
Owner CHANGZHOU INST OF MATERIA MEDICA
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