Preparation method of acetylated hyaluronate

A technology of hyaluronic acid salt and hyaluronic acid, applied in the field of hyaluronic acid salt, can solve the problems of not being very environmentally friendly, large water volume, etc., and achieve the effect of saving material cost, low cost and little environmental pollution

Active Publication Date: 2020-04-10
JIANGSU CHENGXIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mixed acids are used in the reaction process, and the amount of water used in the po...

Method used

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Embodiment 1

[0032] This embodiment provides a preparation method of acetylated hyaluronate, the preparation method comprising the following steps:

[0033] (1) Mix sodium hyaluronate and acetic anhydride in a mass ratio of 1:12, and carry out acylation reaction at 5° C. for 48 hours under the catalysis of concentrated sulfuric acid; wherein, the molecular weight of the sodium hyaluronate is 3000 kDa; the concentrated sulfuric acid The added amount is 35% of the mass of sodium hyaluronate;

[0034] (2) The reaction solution obtained after the reaction is finished is diluted with 4 times of water, and solid is obtained through solid-liquid separation;

[0035] (3) Beat the solid obtained in step (2) with water 5 times the mass of the sodium hyaluronate to obtain an acetylated hyaluronic acid solution, then adjust the pH to 5.5, then filter and dry in sequence to obtain acetylated hyaluronate Sodium hyaluronate.

[0036] The relevant indicators of the obtained acetylated sodium hyaluronate...

Embodiment 2

[0038] This embodiment provides a preparation method of acetylated hyaluronate, the preparation method comprising the following steps:

[0039] (1) Potassium hyaluronate and acetic anhydride are mixed at a mass ratio of 1:13.5, and the acylation reaction is carried out at 25° C. for 38 hours under the catalysis of concentrated sulfuric acid; wherein, the molecular weight of the potassium hyaluronate is 500 kDa; the concentrated sulfuric acid The added amount is 33% of the mass of potassium hyaluronate;

[0040] (2) The reaction solution obtained after the reaction is finished is diluted with 9 times of water, and solid is obtained through solid-liquid separation;

[0041](3) Beat the solid obtained in step (2) with water twice the mass of the potassium hyaluronate to obtain an acetylated hyaluronic acid solution, adjust the pH to 6.4, and then filter and dry in sequence to obtain acetylated hyaluronate Potassium hyaluronate.

[0042] The relevant indicators of the obtained a...

Embodiment 3

[0044] This embodiment provides a preparation method of acetylated hyaluronate, the preparation method comprising the following steps:

[0045] (1) Mix the mixed solution of hyaluronic acid and sodium hyaluronate and acetic anhydride at a mass ratio of 1:5.5, and carry out acylation reaction at 35°C for 28 hours under the catalysis of concentrated sulfuric acid; wherein, the hyaluronic acid and hyaluronic acid The molecular weight of sodium hyaluronate is 1800kDa; The added amount of the concentrated sulfuric acid is 50% of the total mass of hyaluronic acid and sodium hyaluronate in the mixed solution;

[0046] (2) The reaction solution obtained after the reaction is finished is diluted with 20 times of water, and solid is obtained through solid-liquid separation;

[0047] (3) The solid obtained in step (2) is beaten with water that is 7 times the total mass of the hyaluronic acid and sodium hyaluronate, and the pH is adjusted to 4.2 after obtaining the acetylated hyaluronic a...

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Abstract

The invention relates to a preparation method of acetylated hyaluronate, which comprises the following steps: (1) mixing hyaluronic acid or a hyaluronate with an acetic anhydride, and carrying out acylation reaction under the catalysis of a catalyst; (2) after the reaction is finished, diluting an obtained reaction solution with water, and carrying out solid-liquid separation to obtain a solid; and (3) pulping the solid obtained in the step (2) to obtain an acetylated hyaluronic acid solution, and purifying to obtain the acetylated hyaluronate. According to the method provided by the invention, the preparation of the hyaluronate can be realized by only using acetic anhydride without using acetic acid in the raw materials, and meanwhile, the production cost is remarkably reduced due to thefact that acetic acid is not used, and furthermore, the preparation process is greener and more environment-friendly.

Description

technical field [0001] The invention relates to the field of hyaluronate, in particular to a preparation method of acetylated hyaluronate. Background technique [0002] Hyaluronic acid, also known as hyaluronic acid, is a disaccharide repeat of (1-3)-2-N-acetylamino-2-deoxy-D-glucose-(1-4)-O-β-D-glucuronic acid An acidic straight-chain polymucopolysaccharide formed by arrangement, has strong hydrophilicity and very good moisturizing properties, widely exists in the cytoplasm of animal tissue cells and the interlayer of some bacteria, and is used in medicine, cosmetics and food Among them, it is also recognized as the most ideal natural moisturizing factor by the international cosmetics industry. Sodium acetylated hyaluronate has more efficient moisturizing, repairing skin barrier and increasing skin elasticity than traditional sodium hyaluronate. [0003] There are few reports about acetylated sodium hyaluronate. US005679657A discloses a preparation method of acetylated sod...

Claims

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Application Information

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IPC IPC(8): C08B37/08
CPCC08B37/0072
Inventor 李斌李二军魏云亮王鑫祝俊刘根
Owner JIANGSU CHENGXIN PHARMA
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