Method for preparing salvianolic acid A from a plurality of salvia plants

A technology of Salvia genus and salvianolic acid, applied in the separation/purification of carboxylic acid esters, organic chemistry, etc., to achieve the effect of high yield and purity, and simple process

Inactive Publication Date: 2015-11-25
南京虹桥医药技术研究所有限公司
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  • Application Information

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Problems solved by technology

[0011] The technical problem to be solved by the present invention is to provide a preparation method for obtaining salvianolic acid A from a variety of plants of the genus Salvia. This method not only effectively solves the problem of s

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  • Method for preparing salvianolic acid A from a plurality of salvia plants
  • Method for preparing salvianolic acid A from a plurality of salvia plants
  • Method for preparing salvianolic acid A from a plurality of salvia plants

Examples

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Example Embodiment

[0046] Example 1:

[0047] 1. Extraction: Weigh 100g of South Salvia miltiorrhiza medicinal pieces, add 1000ml of water and heat at 70°C for 2 hours under the protection of nitrogen, extract twice, add 800ml of water for the second time, combine and filter to obtain the extract.

[0048] 2. Conversion: Concentrate the extract to 200ml, reflux under normal pressure for 15hr under argon protection, and stop the reaction. The content of salvianolic acid B in the extract was determined to be 1.36%, the content of salvianolic acid A in the conversion solution was 0.53%, and the conversion rate was 56.6%.

[0049] 3. Column chromatography separation: Weigh 200g of DM301 type macroporous resin, pre-process it and pack it into the column. Add the conversion solution to the top of the chromatography column, and eluate 3 column volumes with water after completely entering the column bed, discard this part of the eluate; then eluate 3 column volumes with 70% ethanol, and combine this part of t...

Example Embodiment

[0051] Example 2:

[0052] 1. Extraction: Weigh 100g of the medicinal pieces of Salvia miltiorrhiza, add 1000ml of water and heat at 60°C under argon protection for 2 hours, extract twice, add 800ml of water for the second time, combine and filter to obtain the extract.

[0053] 2. Conversion: Concentrate the extract to 200ml and reflux for 8hr under nitrogen protection to stop the reaction. The content of salvianolic acid B in the extract was determined to be 1.12%, the content of salvianolic acid A in the conversion solution was 0.41%, and the conversion rate was 53.2%.

[0054] 3. Column chromatographic separation: Weigh 200g of 330 type macroporous resin, pre-process it and pack it into the column. Add the conversion solution to the top of the chromatographic column, and eluate 3 column volumes with water after completely entering the column bed, discard this part of the eluate; then elute with 60% methanol for 3 column volumes, and combine this part of the eluate.

[0055] 4. Pu...

Example Embodiment

[0056] Example 3:

[0057] 1. Extraction: Weigh 100g of purple flower Zhejiang Anhui Danshen medicinal pieces, add 1000ml of water and heat for 2 hours at 50°C under nitrogen protection, extract twice, add 800ml of water for the second time, combine and filter to obtain the extract.

[0058] 2. Conversion: Concentrate the extract to 200ml, reflux for 24hr under argon protection, and stop the reaction. The content of salvianolic acid B in the extract was determined to be 1.41%, the content of salvianolic acid A in the conversion solution was 0.53%, and the conversion rate was 54.6%.

[0059] 3. Column chromatography separation: Weigh 200g CAD45 type macroporous resin, pre-process it and pack it into the column. Add the conversion solution to the top of the chromatographic column, and after it has completely entered the column bed, eluate 3 column volumes with water, discard this part of the eluate; then eluate 3 column volumes with 50% ethanol, and combine this part of the eluate.

[...

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Abstract

The present invention relates to a method for preparing salvianolic acid A from a plurality of salvia plants, major steps include: (1) plant roots and rhizomes are sliced, water is poured into a closed container and the decoction pieces are heated for extraction under oxygen free conditions; and (2) the extract is concentrated under reduced pressure to an appropriate volume, refluxed for reaction at 100 DEG C under oxygen free conditions at atmospheric pressure, or placed in an autoclave or a microwave reactor for heating for reaction to obtain a salvianolic acid A conversion solution. The salvianolic acid A conversion solution is further purified by conventional separation techniques such as macroporous resin, reversed phase chromatography on silica gel, Sephadex LH-20, droplet countercurrent chromatography, and the like to obtain a salvianolic acid A product with the content of more than 90%, and the salvianolic acid A product is used for clinical treatment and research. The method is simple in process, higher in salvianolic acid A conversion rate, and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of plant medicines, in particular to a preparation method of salvianolic acid A. Background technique [0002] Salviamiltiorrhiza Bunge, as a commonly used traditional Chinese medicine in my country, has a long history of clinical application and plays an important role in the treatment of cardiovascular and cerebrovascular diseases. Its remarkable curative effect has been widely recognized clinically. At present, Danshen has become the traditional Chinese medicine with the largest consumption, the highest sales and the most preparation manufacturers in my country. The consumption of Danshen medicinal materials exceeds 15,000 tons per year. Clinically used Danshen preparations mainly include: Compound Danshen Dropping Pills, Compound Danshen Injection, Compound Danshen Tablets, Salvianolate Injection, etc. The main active ingredients in these preparations, especially injections, are salvianolic acid compounds, which ...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/48
Inventor 周长新甘礼社朱志彬
Owner 南京虹桥医药技术研究所有限公司
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