Method of preparing high purity Danshensu

A Danshensu, high-purity technology, applied in the field of preparation of high-purity Danshensu, can solve the problems of poor controllability, low yield, complicated post-processing operation process, etc., and achieves low cost, high product yield, and short production cycle. Effect

Inactive Publication Date: 2007-08-08
上海朗萨医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of these two methods is that the yield is too low. In addition, due to the use of extraction and normal phase chromatography, the post-treatment process is more complicated and the controllability is poor.

Method used

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  • Method of preparing high purity Danshensu
  • Method of preparing high purity Danshensu
  • Method of preparing high purity Danshensu

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1. Extraction and transformation: Weigh 200g of Salvia miltiorrhiza, heat and extract with 10 times the amount of 3mol / L hydrochloric acid aqueous solution at 75°C for 2 hours, extract twice, combine and filter to obtain the extract.

[0040] 2. Column chromatography separation: Weigh 200g of DM301 macroporous resin, pretreat and pack into a column. Add the extract to the top of the chromatography column, and elute with water after completely entering the column bed, until the effluent is neutral by pH test paper, elute with 30% ethanol for 3 column volumes, and combine this part of the eluate.

[0041] 3. Recrystallization: The eluent was concentrated under reduced pressure to remove the solvent, heated and dissolved with methanol: acetone 1:1, and left at room temperature to precipitate Danshensu crystals with a yield of 1.8%, and a purity of 92.2% as measured by HPLC.

Embodiment 2

[0043] 1. Extraction and transformation: Weigh 200g of Salvia miltiorrhiza medicinal material, use 8 times the amount of 2mol / L hydrochloric acid 50% ethanol solution, reflux extraction for 2 hours, extract twice, combine and filter to obtain the extract.

[0044] 2. Column chromatography separation: Weigh 200g of 330 type macroporous resin, pretreat and pack into column. Appropriately concentrate the extract to remove ethanol, add it to the top of the chromatography column, and elute with water after completely entering the column bed, until the effluent is neutral by pH test paper, elute with 50% ethanol for 4 column volumes, and combine this part eluent.

[0045]3. Recrystallization: The eluent was concentrated under reduced pressure to remove the solvent, heated and dissolved with water: ethanol 4:1, and left at 2°C to precipitate Danshensu crystals with a yield of 2.0% and a purity of 91.6% as measured by HPLC.

Embodiment 3

[0047] 1. Extraction and transformation: Weigh 500 g of Danshen medicinal material, reflux extraction with 8 times the amount of 0.1 mol / L sulfuric acid 50% methanol solution for 2 hours, extract twice, combine and filter to obtain the extract.

[0048] 2. Column chromatography separation: Weigh 500g of NKA-II type macroporous resin, pretreat and pack into column. Properly concentrate the extract to remove methanol, add it to the top of the chromatography column, and elute with water after completely entering the column bed, until the effluent is neutral by pH test paper, elute with 50% acetonitrile for 5 column volumes, and combine the parts eluent.

[0049] 3. Recrystallization: The eluate was concentrated under reduced pressure to remove the solvent, heated and dissolved with acetonitrile: acetone 1:4, and placed at -10°C to precipitate Danshensu crystals with a yield of 2.1%, and a purity of 90.9% as measured by HPLC.

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Abstract

The invention discloses a making method of high-purity tanshinone, which comprises the following steps: (1) heating and refluxing to extract salvia miltiorrhizae root and stalk through 0.1-6.0mol/L acid water/alcohol solution; (2) adsorbing extract through adsorbing column with large-hole resin adsorbent; (3) eluting through water until pH value is 7 first and hydrophilic solvent then; collecting 3-5 column bulks to elute tanshinone completely; (4) evaporating; adding organic solvent; heating; dissolving; crystallizing; or adopting polyamide, gluglucosan gel Sephadex LH-20, MCI GEL CHP20P, C4, C8 or C18 bond phase; obtaining the product.

Description

technical field [0001] The invention belongs to the field of herbal medicines, in particular to a preparation method of high-purity danshensu. Background technique [0002] Salvia miltiorrhiza is a plant of the genus Salvia in the family Labiatae. As a commonly used traditional Chinese medicine in my country, it has a long history of clinical application and plays an important role in the treatment of cardiovascular diseases. Its remarkable curative effect has been widely recognized clinically. Years of research results show that danshensu is an important active ingredient (Yuan Hengjie, new progress in the study of the pharmacological effects of danshensu. Chinese Journal of Hospital Pharmacy 2006, 26(5), 604-606). The structural formula of Danshensu is as follows: [0003] [0004] The scientific name of Danshensu is D(+)-(3,4-dihydroxyphenyl) lactic acid. It not only has the functions of dilating blood vessels, improving myocardial contractility, and reducing red bloo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/47C07C59/52A61K36/53A61K125/00
Inventor 周长新朱志彬张相宜尹金瑶
Owner 上海朗萨医药科技有限公司
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