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Preparation method for salvianolic acid A

A technology of salvianolic acid and salvianolic acid salt, which is applied in the field of preparation of salvianolic acid A, can solve the problems of inability to meet the needs of industrialization, low yield of salvianolic acid A, difficult product separation, etc., and achieve convenient control of the degradation process , The effect of small product changes between batches and stable process

Active Publication Date: 2012-07-04
SUZHOU LEINA PHARMA RES DEV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Patents or applications in recent years (CN1830947A, CN101230003, CN100999470A, etc.) involve pyrolysis under high temperature and high pressure, followed by conventional separation and purification techniques to prepare salvianolic acid A. The composition is complex, and the reaction solution obtained by the thermal degradation method is more complex, resulting in extremely difficult separation of subsequent products, making the yield of salvianolic acid A extremely low, which cannot meet the needs of industrialization

Method used

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  • Preparation method for salvianolic acid A
  • Preparation method for salvianolic acid A
  • Preparation method for salvianolic acid A

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1. prepares salvianolic acid A conversion liquid

[0022] Take 12g of salvianolic acid salt (the content is greater than 80% based on the magnesium acetate of salvia miltiorrhiza), add 1L of water, adjust the pH value to 6.0 with trisodium citrate, put it in an autoclave, heat at 125°C and 0.15MPa for 4 hours , after solution cooling, add hydrochloric acid and adjust pH value to 2~3, obtain salvianolic acid A conversion liquid; The HPLC analysis of conversion liquid shows, the molar conversion rate of salvianolic acid A 45% ( figure 1 ).

Embodiment 2

[0023] Embodiment 2. prepare salvianolic acid A

[0024] Take the conversion solution of the salvianolic acid A conversion solution of Example 1 and pass through the HPD100 resin column, and then eluted with water for 10 column volumes, 25% ethanol solution for 8 column volumes, discarded, and then 40% ethanol solution for 10 column volumes. column volume, collect the eluent 1, concentrate the eluate 1 under reduced pressure to a salvianolic acid A concentration of 25 mg / ml, pass the concentrated solution through a CG161 resin column, elute with 20% ethanol solution for 10 column volumes, and discard it. Then eluted with 35% ethanol solution for 12 column volumes, collected the eluate 2, concentrated under reduced pressure to a salvianolic acid A concentration of 50 mg / ml; adjusted the pH to 2-3 with hydrochloric acid, extracted three times with an equal volume of ethyl acetate, and combined Concentrate the extract under reduced pressure, add 2.5 times the amount of 80-120 mes...

Embodiment 3

[0025] Embodiment 3. prepare salvianolic acid A conversion liquid

[0026] Take 10g of salvia miltiorrhiza magnesium acetate, add 1L of water, add 10ml of ethyl acetate, adjust the pH value of the solution to 6, put it in an autoclave at 125°C, 0.15MPa, heat for 4 hours, after the solution is cooled, add hydrochloric acid to adjust the pH value From 2 to 3, the conversion solution of salvianolic acid A is obtained, and the HPLC analysis of the conversion solution shows that the molar conversion rate of salvianolic acid A is 72%.

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Abstract

The invention provides a preparation method for a salvianolic acid A conversion solution, more specifically, a preparation method for obtaining salvianolic acid A by means of macroporous resin column chromatography, extraction and a silicagel column. The salvianolic acid A obtained by the method can be industrially produced, and moreover, the purity of the salvianolic acid A is high, so that the medication safety is guaranteed. The invention provides a simple, convenient and high-efficiency method for the preparation of the salvianolic acid A. When the method provided by the invention is used for preparing the salvianolic acid A, the process is stable, the quality can be controlled, the conversion rate is high, the total yield of the salvianolic acid A as main product is high, and the cost is low; and in combination with the separation and purification technique, the method can industrially prepare the high-purity salvianolic acid A in large batches.

Description

technical field [0001] The invention relates to the fields of medicine and health food, in particular to a preparation method of salvianolic acid A. Background technique [0002] [Research Progress on Water-soluble Active Components of Salvia Miltiorrhiza-Salvianolic Acid, Basic Medicine and Clinic, Du Guanhua 2000, 20(5): 10-14.] It is reported that salvianolic acid is the most important active ingredient in the water-soluble components of Salvia miltiorrhiza, salvianolic acid A is a phenolic acid compound, see ([Salvianolic acid A resists carbon tetrachloride poisoning-induced liver injury and liver fibrosis in rats, Acta Pharmacological Journal of Chinese Materia Medica, Hu Yiyang 1997, 18(5): 478-480. ]), but its content in Salvia miltiorrhiza is low (about five parts per million, or even none, [Modern Research on Chinese Herbal Medicine (Volume II) Institute of Materia Medica, Chinese Academy of Medical Sciences, 2005, P479-496.]), even through A series of methods are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/48
Inventor 刘珂韩飞刘军锋许卉邵萌邹晓丽
Owner SUZHOU LEINA PHARMA RES DEV
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