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Preparation method of high-molecular-weight zinc hyaluronate

A technology of zinc hyaluronate and high molecular weight, applied in the field of biomedicine, can solve the problems such as the decrease of the molecular weight of HA-Zn

Active Publication Date: 2020-09-11
BLOOMAGE BIOTECHNOLOGY CORP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because hyaluronic acid is prone to degradation under acidic conditions, and in the drying process, it will also cause the molecular weight of HA-Zn to decrease.
As we all know, the higher the molecular weight of HA, the better the moisturizing performance, the better the film-forming and barrier effects. Zinc hyaluronate is a polymer compound, and the molecular weight will decrease to varying degrees during storage. Therefore, the currently prepared HA-ZnM r Mostly below 500,000 Da, the preparation of HA-Zn greater than 1,000,000 Da has become a major technical problem. In addition, the light transmittance of the samples prepared by the prior art (light transmittance is an index to characterize the clarity of the sample, light transmittance The higher the rate, the better the clarity) is often lower than 95%, and the opalescence can be seen with the naked eye in severe cases

Method used

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  • Preparation method of high-molecular-weight zinc hyaluronate
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[0026] The invention provides a preparation method of high-molecular-weight zinc hyaluronate, which comprises the following steps: adding powdery sodium hyaluronate into a replacement solution for replacement to obtain powdery zinc hyaluronate;

[0027] washing the precipitate with a washing solution;

[0028] The washed precipitate is dehydrated with a dehydrating solution and dried in vacuum to obtain high molecular weight zinc hyaluronate powder.

[0029] In a specific embodiment, the molecular weight of the sodium hyaluronate is greater than or equal to 2 million Da, such as 2 million Da, 2.5 million Da, 3 million Da, 4 million Da, etc.

[0030] In a specific embodiment, the concentration of ethanol in the replacement solution is 70%-85% (v / v), for example, 70%, 72%, 75%, 78%, 80%, 82%, 85% . The zinc ion concentration is 0.15%-1.0% (w / v), for example, 0.15%, 0.24%, 0.30%, 0.40%, 0.50%, 0.60%, 0.72%, 1.0%. Zinc ions can be prepared by adding zinc salts to the replacemen...

Embodiment 1

[0061] (1) Prepare replacement fluid, washing fluid and dehydration fluid. Wherein, the ethanol concentration in the replacement solution was 70% (v / v), the zinc ion concentration was controlled to be 0.48% (w / v), and the pH of the replacement solution was adjusted to 6.0 with glacial acetic acid. The concentration of ethanol in the washing solution was 85% (v / v), and the pH of the washing solution was adjusted to 5.5 with glacial acetic acid. The ethanol concentration in the dehydration solution was 90% (v / v), and the pH of the dehydration solution was adjusted to 5.8 with glacial acetic acid.

[0062] (2) Add sodium hyaluronate with a molecular weight of 2 million Da to the above-mentioned ethanol replacement solution while stirring, continue to stir (replace) for more than 2 hours, stand to separate the supernatant, and replace twice to obtain hyaluronic acid Zinc precipitation.

[0063] (3) Wash the precipitate with the above washing solution for 6 times.

[0064] (4) T...

Embodiment 2-5

[0067] The difference between Examples 2-5 and Example 1 is that the zinc ion concentration, ethanol concentration and corresponding pH in the prepared replacement solution, washing solution and dehydration solution are different, and the corresponding replacement, washing and dehydration times are different, and other The operation steps are the same. The conditions adopted in the specific preparation method are shown in Table 1.

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Abstract

The invention provides a preparation method of high-molecular-weight zinc hyaluronate, comprising the following steps of: adding sodium hyaluronate into a replacement solution, and replacing to obtainzinc hyaluronate precipitate; washing the precipitate with a washing liquid; and dehydrating the washed precipitate with a dehydration solution, and carrying out vacuum drying to obtain the high-molecular-weight zinc hyaluronate powder. According to the preparation method, the optimal preparation conditions are obtained by exploring the preparation conditions such as the replacement liquid pH, the replacement frequency, the washing pH, the washing frequency, the dehydration liquid pH and the dehydration frequency. The molecular weight of the zinc hyaluronate prepared by the preparation methoddisclosed by the invention can reach 1,000,000 Da or above, the light transmittance is greater than 99.5 percent, the zinc content is greater than 7.0 percent, and the problems of low molecular weight and low clarity are successfully solved.

Description

technical field [0001] The invention belongs to the field of biomedicine and relates to a method for preparing high molecular weight zinc hyaluronate, in particular to a method for preparing high molecular weight zinc hyaluronate. Background technique [0002] Hyaluronic acid (hyaluronic acid) is also known as hyaluronic acid, referred to as HA. It is called hyaluronic acid in the field of cosmetics and food. It is called hyaluronic acid or hyaluronic acid in the field of medicine. The commonly used form is sodium hyaluronate, and its carboxyl binding ion is sodium Ion, also known as sodium hyaluronate or sodium hyaluronate, when its carboxyl-binding ion is zinc ion, it is called zinc hyaluronate, zinc hyaluronate (abbreviated as HA-Zn) HA-Zn has the lubricating properties of HA-Na, In addition to moisturizing and viscoelasticity, it also has the functions of resisting digestive tract ulcers, treating bacterial and fungal infections and inhibiting Helicobacter pylori. There...

Claims

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Application Information

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IPC IPC(8): C08B37/08
CPCC08B37/0072C08B37/0003
Inventor 郭学平杨桂兰肖慧栾贻宏刘爱华石艳丽耿凤阚洪玲
Owner BLOOMAGE BIOTECHNOLOGY CORP LTD
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