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Method for purifying salvianolic acid A

A purification method and technology of salvianolic acid, applied in chemical instruments and methods, separation/purification of carboxylic acid esters, organic chemistry, etc., can solve problems such as high cost, many conversion by-products, serious organic solvent residues, etc., and achieve production The effect of low cost and high conversion rate

Active Publication Date: 2013-03-27
JIANGZI QINGFENG PHARMACEUTICALS INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But above-mentioned prior art transformation process can't be controlled, and transformation by-product is many, and the productive rate of main product salvianolic acid A is lower
Moreover, the damage to salvianolic acid A is very large, the cost is extremely high, and the obtained extract has serious organic solvent residues, which is extremely difficult to store and use
[0006] In summary, there are insurmountable defects in the actual production process in the above-mentioned prior art

Method used

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  • Method for purifying salvianolic acid A
  • Method for purifying salvianolic acid A
  • Method for purifying salvianolic acid A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Adjust the pH value of the eluate or extract containing salvianolic acid A to 2.5 with 20% phosphoric acid, centrifuge, concentrate the supernatant under reduced pressure to contain 3 mg of salvianolic acid A per 1 ml, and perform HPD-100 macroporous resin column chromatography For separation, the ratio of the loading amount of salvianolic acid A to the macroporous adsorption resin is 1:50, and the diameter-to-height ratio of the resin column is 1:10, and eluted with 3 times column volume of water and 5 times column volume of 25% ethanol to remove impurities , then eluted with 4 times the column volume of 40% ethanol, detected by HPLC, collected the 40% ethanol eluted part containing salvianolic acid A, recovered the ethanol under reduced pressure and concentrated to no alcohol smell; the aqueous solution was concentrated to contain 5 mg salvianol per ml The solution of acid A is separated by polyamide chromatography column, the ratio of salvianolic acid A loading to pol...

Embodiment 2

[0031]Adjust the pH value of the eluate or extract containing salvianolic acid A to 2.5 with 15% hydrochloric acid, centrifuge, concentrate the supernatant under reduced pressure to contain 5 mg of salvianolic acid A per 1 ml, and perform HPD-100 macroporous resin column chromatography For separation, the ratio of the loading amount of salvianolic acid A to the macroporous adsorption resin was 1:45, and the diameter-to-height ratio of the resin column was 1:8, and eluted with 3.5 times column volume of water and 4 times column volume of 25% ethanol to remove impurities , then eluted with 5 times column volume of 45% ethanol, detected by HPLC, collected the 45% ethanol eluted part containing salvianolic acid A, recovered the ethanol under reduced pressure and concentrated to no alcohol smell; the aqueous solution was concentrated to contain 5 mg salvianol per ml The solution of acid A is separated by polyamide chromatography column, the ratio of salvianolic acid A loading to pol...

Embodiment 3

[0033] Adjust the pH value of the eluate or extract containing salvianolic acid A to 2.8 with 15% nitric acid, centrifuge, concentrate the supernatant under reduced pressure to contain 6 mg of salvianolic acid A per 1 ml, and perform HPD-100B macroporous resin column chromatography For separation, the ratio of the loading amount of salvianolic acid A to the macroporous adsorption resin was 1:40, and the ratio of diameter to height of the resin column was 1:7, and eluted with 4 times column volume of water and 4 times column volume of 25% ethanol respectively to remove impurities , then eluted with 5 times column volume of 40% ethanol, detected by HPLC, collected the 40% ethanol eluted part containing salvianolic acid A, recovered the ethanol under reduced pressure and concentrated to no alcohol smell; the aqueous solution was concentrated to contain 6 mg salvianol per ml The solution of acid A is separated by polyamide chromatography column, the ratio of salvianolic acid A load...

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Abstract

The invention relates to a method for purifying salvianolic acid A, which comprises the steps of: adjusting the pH of eluate or extract liquid containing salvianolic acid A to 2.5-4.5, and centrifuging; separating supernatant by non-polar or weak-polar macroporous resin column chromatography; eluting with water and then eluting with eluent; carrying out high-efficiency liquid phase detection of salvianolic acid A, and collecting eluate containing salvianolic acid A; separating the obtained eluate with a dextrane gel LH-20 or ODS-C18 or polyamide chromatographic column; eluting with eluent; carrying out high-efficiency liquid phase detection of salvianolic acid A, and collecting eluate containing salvianolic acid A; adjusting the pH of the eluate to 2.0-4.0, extracting the eluate with an organic solvent and separating the organic solvent phase; separating the obtained solution by using a silica gel chromatographic column, eluting with the eluent, carrying out high-efficiency liquid phase detection of salvianolic acid A, and collecting eluate containing salvianolic acid A; recovering the eluent at reduced pressure; and dissolving the eluate with water, and carrying out microwave vacuum drying to further purify salvianolic acid A.

Description

technical field [0001] The invention relates to a method for purifying salvianolic acid A. technical background [0002] Salvia miltiorrhiza preparation is the basic treatment drug for cardiovascular and cerebrovascular diseases in my country. Because of its definite curative effect, Danshen has become one of the traditional Chinese medicines with the largest consumption, the highest sales, the most preparation factories and the most complete clinical dosage forms in China. There are two main types of effective chemical components in Danshen: fat-soluble tanshinone compounds and water-soluble phenolic compounds. Studies have shown that salvianolic acids have significant activities in anti-liver damage, anti-atherosclerosis and apoptosis, and improvement of memory dysfunction. Among them, the antioxidant activity of salvianolic acid A (Saivianolic acid A) is the strongest. [0003] The structure of salvianolic acid A is as follows: [0004] [0005] However, the natural...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/48C07C67/56C07C67/58
Inventor 刘地发张功俊王振汤新乾刘尧奇廖祝元
Owner JIANGZI QINGFENG PHARMACEUTICALS INC
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