A kind of preparation method of chitosan hydroxybutyl derivative

A chitosan hydroxybutyl and polysaccharide hydroxybutyl technology, which is applied in the biological field, can solve the problems of no hydroxybutyl chitosan commodity sales, limited research and application development, long preparation process cycle, etc., so as to shorten the preparation process. cycle, improved preparation efficiency, and the effect of wide pH dissolution range

Active Publication Date: 2011-12-14
惠众国际医疗器械(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, although there are international research reports on hydroxybutyl chitosan as a biological material, and there are also patented technology disclosures on preparation methods, the preparation process cycle is long,

Method used

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  • A kind of preparation method of chitosan hydroxybutyl derivative
  • A kind of preparation method of chitosan hydroxybutyl derivative
  • A kind of preparation method of chitosan hydroxybutyl derivative

Examples

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Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 20g of chitosan, dissolve it in 1000ml of 1% HCl aqueous solution, filter, add dropwise 1mol / l NaOH solution to the filtrate to obtain a precipitate, wash with distilled water several times until neutral, desalt with 70% ethanol, and desalt with 95% ethanol Dehydrate and dry at 50°C to obtain a purified chitosan sample. Weigh 1g of purified chitosan and disperse it in 10ml of 50% NaOH aqueous solution, N 2 Protected, stirred under the power of 600W microwave for 24 hours, filtered, squeezed out the excess lye to obtain solids. Add the obtained solid to 20ml of isopropanol aqueous solution (isopropanol: water (V:V) = 19:1) and stir for 24h, add 25ml of 1,2-epoxybutane dropwise, react for 1h, and then turn on the power of 1200W Under microwave, the temperature was raised to 60°C for 48 hours. After cooling to room temperature, 10% HCl aqueous solution was added dropwise to the reaction solution to adjust the pH of the system to neutral. Filter out the insoluble m...

Embodiment 2

[0018] Weigh 20g chitosan, dissolve in 1000ml 1% HCl aqueous solution, filter, add dropwise 1mol / l NaOH solution to the filtrate to obtain a precipitate, wash with distilled water until neutral, desalt with 70% ethanol, dehydrate with 95% ethanol, Dry at 50°C to obtain purified chitosan samples. Get 1g of purified chitosan and disperse it in 10ml of 50% NaOH aqueous solution, N 2 Protected, stirred under the power of 1200W microwave for 24h, filtered, squeezed out the excess lye to obtain solids. Add the obtained solid to 20ml of isopropanol aqueous solution (isopropanol:water (V:V)=10:10) and stir for 24h, add dropwise 20ml of 1,2-epoxybutane, react for 1h, power 1000W microwave, The temperature was raised to 25°C for 72h. After cooling to room temperature, 10% HCl aqueous solution was added dropwise to the reaction solution to adjust the pH of the system to neutral. Filter out the insoluble matter, precipitate with 3 times the volume of ethanol, centrifuge (12000 rpm, 10 ...

Embodiment 3

[0020] Weigh 20g chitosan, dissolve in 1000ml 1% HCl aqueous solution, filter, add dropwise 1mol / l NaOH solution to the filtrate to obtain a precipitate, wash with distilled water until neutral, desalt with 70% ethanol, dehydrate with 95% ethanol, Dry at 50°C to obtain purified chitosan samples. Get 1g of purified chitosan and disperse it in 10ml of 50% NaOH aqueous solution, N 2 Protected, stirred under the power of 1000W microwave for 24h, filtered, squeezed out the excess lye to obtain solids. Add the obtained solid to 20ml of isopropanol aqueous solution (isopropanol: water (V:V) = 1:19) and stir for 24h, add 5ml of 1,2-epoxybutane dropwise, react for 1h, and use a microwave with a power of 600W , the temperature was raised to 80°C for 24h. After cooling to room temperature, 10% HCl aqueous solution was added dropwise to the reaction solution to adjust the pH of the system to neutral. Filter out the insoluble matter, precipitate with 3 times volume of ethanol, centrifug...

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Abstract

The invention relates to a preparation method of a chitosan hydroxybutyl derivative. Chitosan is used as a raw material; 1,2-epoxybutane is used as an etherifying agent; the hydroxybutyl modification of the chitosan is performed in an isopropanol aqueous solution dispersion system under microwave action with controlled reaction temperature and time; a chitosan derivative, hydroxybutyl chitosan, is successfully prepared; the preparation period is greatly shortened, and the preparation efficiency is increased. During the reaction, the hydroxybutyl modification of the chitosan is performed orderly under the microwave action and with controlled reaction temperature and time, which shortens the preparation period. The product has a wider pH dissolution range, and has a soluble property in weakacid, neutral, and weak alkaline aqueous solutions, that is to say, the limitation that chitosan is only soluble in acids or acid solutions is improved; the aqueous solution of the product has temperature sensitivity, can be transformed between an aqueous solution and hydrogel by adjusting the temperature; and the product is widely applicable to fields of biomedicine, tissue engineering, pharmaceutical carriers, chemical engineering, food, cosmetics, etc.

Description

technical field [0001] The invention relates to a preparation method of chitosan hydroxybutyl derivatives. In particular, it relates to a preparation method of a chitosan derivative-hydroxybutyl chitosan with good water solubility, temperature and pH sensitivity. Belongs to the field of biotechnology. Background technique [0002] Chitosan (chitosan) is an amino polysaccharide widely present in nature, which is the product of chitin after deacetylation. It has excellent properties such as biocompatibility, non-toxicity, biodegradability and antibacterial properties, and is widely used as a drug release carrier, tissue engineering scaffold, wound dressing, etc. in the biomedical field. However, due to the distribution of many amino groups and hydroxyl groups on the macromolecular chain, which can form intramolecular and intermolecular hydrogen bonds, chitosan has high crystallinity and poor solubility, which greatly limits its development and application. Preparation of wa...

Claims

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Application Information

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IPC IPC(8): C08B37/08
Inventor 陈西广李晶晶程晓杰王倩倩
Owner 惠众国际医疗器械(北京)有限公司
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