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Method for preparing przewalskinic acid A by hydrolysis conversion of salvianolic acid B

A technology of sage salvia and salvianolic acid, applied in the field of preparing salvianolic acid A, can solve the problems of unsuitable mass production, slow speed and the like, and achieve a good separation effect, short time consumption, and easy quality control. Effect

Active Publication Date: 2017-05-17
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above-mentioned prior art adopts the method of enzyme-catalyzed conversion to prepare ganxi carnosic acid A, but the speed of preparing ganxi carnosic acid A through enzymatic hydrolysis conversion of salvianolic acid B is slow, generally takes a week, and is not suitable for industrialized large-scale Production

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  • Method for preparing przewalskinic acid A by hydrolysis conversion of salvianolic acid B
  • Method for preparing przewalskinic acid A by hydrolysis conversion of salvianolic acid B

Examples

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Embodiment 1

[0030] A method for hydrolyzing and transforming salvianolic acid B to prepare Gansey carnosic acid A, characterized in that it comprises the following process steps:

[0031] A. Base-catalyzed hydrolysis

[0032] Take 500g of salvianolic acid B solid, slowly add a 3% aqueous alkali solution to adjust the pH to 12, heat in a water bath at 55°C for 30 minutes, wait for the salvianolic acid B to be hydrolyzed into ganxicarnosic acid A, and then add 5% of the volume fraction The hydrochloric acid aqueous solution adjusts the pH of the hydrolyzed solution to weak acidity; slowly adding the alkaline aqueous solution can make the alkaline solution evenly distributed, and the alkali-catalyzed hydrolysis of the system is more sufficient.

[0033] The hydrolysis of salvianolic acid B into carnosic acid can be judged by HPLC detection. The reaction rate is very slow when the pH value of the lye is below 12, and the reaction rate is too fast when the pH value of the lye is above 13, whi...

Embodiment 2

[0044] A method for hydrolyzing and transforming salvianolic acid B to prepare Gansey carnosic acid A, characterized in that it comprises the following process steps:

[0045] A. Base-catalyzed hydrolysis

[0046] Take 1000g of salvianolic acid B solid, slowly add 5% alkali aqueous solution to adjust the pH to 13, heat in a water bath at 55°C for 50 minutes, wait for the salvianolic acid B to be hydrolyzed into ganxicarnosic acid A, and then add 5% of the volume fraction Aqueous hydrochloric acid adjusts the pH of the hydrolyzate to weak acidity.

[0047] B. Extraction and concentration

[0048] The hydrolyzate collected in step A was extracted with ethyl acetate until the product was complete, concentrated and pulled to dryness at 50°C.

[0049] C. Purification of hydrolyzate

[0050] First dissolve the extract concentrate with 28% acetonitrile, then filter it with a thin layer of silica gel, and finally filter it with a microporous membrane with a pore size of 0.45 μm, an...

Embodiment 3

[0055]A method for hydrolyzing and transforming salvianolic acid B to prepare Gansey carnosic acid A, characterized in that it comprises the following process steps:

[0056] A. Base-catalyzed hydrolysis

[0057] Take 10,000g of salvianolic acid B solid, slowly add 5% alkali aqueous solution to adjust the pH to 13, heat in a water bath at 55°C for 50 minutes, wait for salvianolic acid B to be hydrolyzed into gansey carnosic acid A, and then use 0% volume fraction of Aqueous hydrochloric acid adjusts the pH of the hydrolyzate to weak acidity.

[0058] B. Extraction and concentration

[0059] The hydrolyzate collected in step A was extracted with ethyl acetate until the product was complete, concentrated and pulled to dryness at 55°C.

[0060] C. Purification of hydrolyzate

[0061] First dissolve the extract concentrate with 25% acetonitrile, then filter it with a thin layer of silica gel, and finally filter it with a microporous membrane with a pore size of 0.45 μm, and sep...

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Abstract

The invention discloses a method for preparing przewalskinic acid A by hydrolysis conversion of salvianolic acid B. The method comprises alkali catalyzed hydrolysis, extraction and concentration, purification of hydrolysate and recovery of przewalskinic acid A. The invention solves the problems that the content of przewalskinic acid A in primary przewalskinic acid A is low, the preparation speed of przewalskinic acid A by enzymatic hydrolysis is slow and the purity is low. The method provided by the invention has the advantages of simple operation, high conversion rate, short production cycle, stable process and easy control of cost, and can realize the high purity separation and preparation of a large amount of przewalskinic acid A.

Description

technical field [0001] The present invention relates to a method for large-scale preparation of gansey carnosic acid A, and in particular provides a method for preparing high-purity dansey carnosic acid A from a conversion liquid obtained by hydrolyzing salvianolic acid B to prepare gansey carnosic acid A , belongs to the technical field of separation and purification of traditional Chinese medicine. Background technique [0002] Gancy carnosic acid A is a rare water-soluble and highly biologically active substance. At present, it only exists in Gansey sage. The study of oxalic acid A caused difficulties. Preparation of przewalskinic acid A from salvianolic acid B using a crudeenzyme from an Aspergillus oryzae strain In the article, salvianolic acid B is enzymatically hydrolyzed to obtain gansey carnosic acid A, and the hydrolysis process is as follows: [0003] [0004] The hydrolysis process is: salvianolic acid B Danshensu + Ganxi carnosic acid A. [0005] The abo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/84
CPCC07D307/84
Inventor 何文彬吴明春文焕松江洪兵刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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