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Preparation method of salvinaolic acid A

A technology for salvianolic acid and salvia miltiorrhiza, which is applied in the field of separation and purification of active components of traditional Chinese medicine, can solve the problems of increasing the production cost of salvianolic acid A, and the inability to recycle proteins.

Active Publication Date: 2015-07-08
ZHEJIANG YONGNING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this process uses protein to adsorb salvianolic acid A, and its protein cannot be recycled, which will undoubtedly greatly increase the production cost of salvianolic acid A, and will also bring greater environmental problems

Method used

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  • Preparation method of salvinaolic acid A
  • Preparation method of salvinaolic acid A
  • Preparation method of salvinaolic acid A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Step 1: Take 100 g of Danshen medicinal material, add 1.2 L of 70% ethanol, heat and extract at 100° C. for 1 hour, and filter the extract. Add 1.2L of 70% ethanol to the filter residue, heat and extract at 100°C for 2 hours, and filter the extract.

[0037] Step 2: Combine the two extracts and concentrate under reduced pressure to 300 mL. Adjust the pH to 5 with hydrochloric acid and sodium hydroxide, and heat to reflux at 90°C for 36 hours to obtain a crude salvianolic acid A solution.

[0038] Step 3: 100mL macroporous adsorption resin XAD-2 is filled in a glass chromatographic column with an aspect ratio of 5:1. Salvianolic acid A crude product solution, adjusted to pH8, flows through the chromatographic column at a flow rate of 200mL / hour. The resin column was eluted with 1L deionized water at a flow rate of 200mL / hour. Then adopt 30% ethanol to elute the resin column, collect step by step, 50mL / bottle, and detect by HPLC until no salvianolic acid A flows out. ...

Embodiment 2

[0041] The solvent for extracting the salvia miltiorrhiza in Example 1 was replaced with water, and the rest was the same as that in Example 1 to finally obtain 0.82 g of 97.1% salvianolic acid A.

Embodiment 3

[0043] The solvent for extracting the salvia miltiorrhiza medicinal material in Example 1 was replaced with 10% ethanol, and the rest was the same as in Example 1 to finally obtain 0.88 g of 97% salvianolic acid A.

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Abstract

The invention discloses a method for preparing salvinaolic acid A. The method comprises the steps of adding an extractant into crude salvia miltiorrhiza medicines, heating and extracting, and then filtering and concentrating extracting solution, to obtain salvia miltiorrhiza extracting solution; regulating the pH of the salvia miltiorrhiza extracting solution to be 4-8, performing vacuum concentration to obtain the concentrated salvia miltiorrhiza extracting solution, heating and reacting the concentrated salvia miltiorrhiza extracting solution at 70-100 DEG C for 5-40h, to obtain crude salvinaolic acid A solution; regulating the pH of the crude salvinaolic acid A solution to be 6-8, performing antiphase resin adsorption, then firstly eluting with water and then eluting with methanol aqueous solution or ethanol aqueous solution, collecting eluant by steps, performing HPLC (High Performance Liquid Chromatography) detection, and combining sample solution containing salvinaolic acid A with the purity of more than 97%; concentrating and drying the sample solution containing salvinaolic acid A with the purity of more than 97%, to obtain salvinaolic acid A powder. The purity of the salvinaolic acid A can achieve more than 97%, and the yield can exceed 0.8% (according to crude medicines). The method is applicable to large-scale preparation for high-purity salvinaolic acid A products.

Description

technical field [0001] The invention relates to a method for separating and purifying active components of traditional Chinese medicines, in particular to a method for preparing salvianolic acid A from salvia miltiorrhiza. Background technique [0002] Salvia miltiorrhiza is a commonly used clinical traditional Chinese medicine, which is widely used in the prevention and treatment of cardiovascular and cerebrovascular diseases, liver diseases, kidney diseases, nervous system diseases and tumors. Since the traditional method of using traditional Chinese medicine is mainly decoction, the water-soluble active components in Salvia miltiorrhiza have attracted widespread attention. Salvianolic acid B has the highest content of water-soluble active components in Salvia miltiorrhiza, and it also contains shikonian acid, rosmarinic acid, and danshensu (attached figure 1 ). [0003] Salvianolic acid B can undergo a series of reactions such as ester hydrolysis, decarboxylation, and r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/732C07C67/48C07C67/62
CPCC07C67/48C07C67/62C07C69/732
Inventor 阚士东
Owner ZHEJIANG YONGNING PHARMA