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Preparation method of sodium trimetaphosphate cross-linked hyaluronic acid powder as well as obtained product and application

A technology for cross-linking hyaluronic acid and sodium trimetaphosphate, which is used in cosmetic preparations, cosmetic preparations, preparations for skin care, etc. problems, to achieve excellent resistance to hyaluronidase degradation, efficient utilization, and a wide range of applications.

Active Publication Date: 2020-04-17
BLOOMAGE BIOTECHNOLOGY CORP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method prepares a particle-free hydrogel. The amount of cross-linking agent used in the preparation process is large, and because the concentration of hyaluronic acid itself is too high, the entire reaction must be carried out in a semi-solid state. During the cross-linking reaction and swelling stage The requirements for equipment are very high, not suitable for mass production

Method used

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  • Preparation method of sodium trimetaphosphate cross-linked hyaluronic acid powder as well as obtained product and application
  • Preparation method of sodium trimetaphosphate cross-linked hyaluronic acid powder as well as obtained product and application
  • Preparation method of sodium trimetaphosphate cross-linked hyaluronic acid powder as well as obtained product and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Dissolve 2g of sodium hydroxide in 200mL of water, add 0.26g of sodium trimetaphosphate, stir to dissolve, add 20g of hyaluronic acid (molecular weight: 1360kDa) in a water bath at 30°C, stir to dissolve, then stir and react at 300rpm for 0.5h in the solution state. Adjust the rotation speed to 600rpm, add 320mL of 95% ethanol to the reaction solution, hyaluronic acid and cross-linked products precipitate in the state of microspheres, stop stirring after feeding, let stand, suspend the microspheres in the ethanol solution, and continue the cross-linking reaction for 6h . Start stirring, adjust the pH of the reaction solution to 7.2 with 2mol / L hydrochloric acid solution, continue to add 60mL of 95% ethanol at 600rpm, the microspheres precipitate at the bottom of the ethanol solution, collect the precipitate by filtration, and wash with 75% ethanol and 95% ethanol in turn Three times, the wet powder was obtained by filtration, and vacuum-dried at 50° C. for 12 hours to o...

Embodiment 2

[0040] Dissolve 2g of sodium hydroxide in 200mL of water, add 0.16g of sodium trimetaphosphate, stir to dissolve, add 20g of hyaluronic acid (molecular weight: 1360kDa) in a water bath at 20°C, stir to dissolve, then stir and react at 300rpm for 1h in the solution state. Adjust the rotation speed to 600rpm, add 400mL 95% ethanol to the reaction solution, hyaluronic acid and cross-linked products precipitate in the state of microspheres, stop stirring after feeding, let stand, microspheres are suspended in the ethanol solution, and cross-linked for 8 hours. Start stirring, adjust the pH of the reaction solution to 7.0 with 2mol / L hydrochloric acid solution, continue to add 100mL of 95% ethanol at 600rpm, the microspheres precipitate at the bottom of the ethanol solution, collect the precipitate by filtration, and wash with 75% ethanol and 95% ethanol in turn Three times, the wet powder was obtained by filtration, and vacuum-dried at 50° C. for 12 hours to obtain 16.8 g of cross-...

Embodiment 3

[0042] Dissolve 3g of sodium hydroxide in 200mL of water, add 0.072g of sodium trimetaphosphate, stir to dissolve, add 18g of hyaluronic acid (molecular weight: 1700kDa) in a water bath at 25°C, stir to dissolve, then stir and react at 400rpm for 0.5h in the solution state. Adjust the rotational speed to 600rpm, add 270mL isopropanol to the reaction solution, hyaluronic acid and cross-linked products precipitate in the state of microspheres, stop stirring after feeding, let stand, the microspheres are suspended in the isopropanol solution, and the crosslinking reaction 5h. Start stirring, adjust the pH of the reaction solution to 7.2 with 2mol / L hydrochloric acid solution, continue to add 60mL of isopropanol at 600rpm, the microspheres precipitate at the bottom of the isopropanol solution, collect the precipitate by filtration, and use 75% isopropanol, isopropanol and Each was washed three times with propanol, filtered to obtain wet powder, and vacuum-dried at 40° C. for 18 ho...

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Abstract

The invention provides a preparation method of sodium trimetaphosphate cross-linked hyaluronic acid powder, an obtained product and application. The method comprises the following steps: firstly, carrying out first-step cross-linking reaction on hyaluronic acid or a salt of hyaluronic acid in an alkaline solution containing sodium trimetaphosphate, then adding an organic solvent under rapid stirring to separate out hyaluronic acid in the form of microspheres, and then carrying out second-step cross-linking reaction in the microspheres; and after the reaction is finished, regulating the pH value of an obtained reaction solution to be 7, continuously adding the organic solvent, filtering, collecting precipitates, washing and drying to obtain a product. According to the preparation method, the efficient utilization rate of a cross-linking agent is guaranteed, the effective cross-linking efficiency of the cross-linking reaction is also guaranteed, and a gel obtained through water swellingof the obtained product has excellent hyaluronidase degradation resistance and is wide in application prospect.

Description

technical field [0001] The present invention relates to a preparation method of a hyaluronic acid cross-linked product, in particular to a method for preparing cross-linked hyaluronic acid powder with sodium trimetaphosphate as a cross-linking agent, and also to the product obtained according to the method and the product The application belongs to the technical field of hyaluronic acid. Background technique [0002] Hyaluronic acid is a straight-chain polymeric acidic mucopolysaccharide. It is an inherent component in the human body. It has no species specificity and is widely distributed in the articular cartilage, lens, skin and other tissues of the human body. Moisturizing effect is one of the important functions of hyaluronic acid. Compared with other humectants, the relative humidity of the surrounding environment has little effect on its moisturizing type. Hyaluronic acid has good biocompatibility and biodegradability. It can be used as a biomedical material and is w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/24C08J3/14C08L5/08C08K3/32A61K8/73A61K8/24A61K8/02A61Q19/10A61Q11/00
CPCC08J3/24C08J3/14A61K8/735A61K8/24A61K8/022A61Q19/10A61Q11/00C08J2305/08C08K3/32
Inventor 魏健郭学平石艳丽王成山王冠凤栾贻宏耿凤邵萌
Owner BLOOMAGE BIOTECHNOLOGY CORP LTD
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