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A kind of preparation method of high-purity danshensu sodium

A high-purity technology of danshensu sodium, which is applied in the preparation of carboxylate salts, medical preparations containing active ingredients, and pharmaceutical formulas, can solve problems such as low purity, small preparation volume, and difficult control of steps, and achieve economical and energy-saving Obvious, simple and controllable steps, and obvious effects

Inactive Publication Date: 2012-02-01
HEFEI ZIJIN PHARMA TECHNOLOGICAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Above method, either preparation amount is little, and cost is high, can't industrialized production on a large scale, exactly purity is not high, and step is difficult to control, can't produce a large amount of high-purity (more than 99%) danshensu sodium products

Method used

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  • A kind of preparation method of high-purity danshensu sodium

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Experimental program
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Effect test

Embodiment 1

[0027] Salvia miltiorrhiza medicinal material 10kg, superfine pulverization, micropowder soaks 30 minutes with the ethyl acetate of 20kg, filters, filter residue leaching 30 minutes with 60kg 50 ℃ of water, filters, after the filtrate is fully absorbed by AB-8 resin, 40% (V / V) Elute with 90L of ethanol solution, collect the eluate, concentrate the recovered ethanol to 6L, adjust the pH value to 7-8 with NaOH solution, and heat at 110-130°C for 30 minutes.

[0028] After filtering, the filtrate was adjusted to a pH value of 1-3 with hydrochloric acid, adsorbed on an AB-8 resin column treated with 0.2% hydrochloric acid solution, and eluted with 90 L of pure water. The eluate was adjusted to pH 7-8 with NaOH solution, concentrated, dried to obtain Danshensu sodium solid, dissolved by heating with methanol, decolorized with activated carbon, filtered, and allowed to stand for crystallization. The crystals were collected by filtration and dried in vacuum below 80°C to obtain 127 ...

Embodiment 2

[0030] Salvia miltiorrhiza medicinal material 10kg, superfine pulverization, micropowder soaks 30 minutes with 20kg ethyl acetate, filters, and filter residue is leached with 60kg 60 ℃ of water 30 minutes, filters, and after the filtrate is fully absorbed by AB-8 resin, 40% (V / V) Elute with 90L of ethanol solution, collect the eluate, concentrate the recovered ethanol to 6L, adjust the pH value to 7-8 with NaOH solution, and heat at 110-130°C for 30 minutes.

[0031] After filtering, the filtrate was adjusted to a pH value of 1-3 with hydrochloric acid, adsorbed on an AB-8 resin column treated with 0.2% hydrochloric acid solution, and eluted with 90 L of pure water. The eluate was adjusted to pH 7-8 with NaOH solution, concentrated, dried to obtain Danshensu sodium solid, dissolved by heating with methanol, decolorized with activated carbon, filtered, and allowed to stand for crystallization. The crystals were collected by filtration and dried in vacuum below 80°C to obtain 1...

Embodiment 3

[0033] Salvia miltiorrhiza medicinal material 10kg, superfine pulverization, micropowder soaks 30 minutes with 20kg ethyl acetate, filters, filter residue leaching 30 minutes with 60kg 70 ℃ of water, filters, after the filtrate is fully absorbed by AB-8 resin, 40% (V / V) Elute with 90L of ethanol solution, collect the eluate, concentrate the recovered ethanol to 6L, adjust the pH value to 7-8 with NaOH solution, and heat at 110-130°C for 30 minutes.

[0034] After filtering, the filtrate was adjusted to a pH value of 1-3 with hydrochloric acid, adsorbed on an AB-8 resin column treated with 0.2% hydrochloric acid solution, and eluted with 90 L of pure water. The eluate was adjusted to pH 7-8 with NaOH solution, concentrated, dried to obtain Danshensu sodium solid, dissolved by heating with methanol, decolorized with activated carbon, filtered, and allowed to stand for crystallization. The crystals were collected by filtration and dried in vacuum below 80°C to obtain 132 g of Da...

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Abstract

The invention relates to a preparation method of high-purity salvia miltiorrhiza, which comprises superfine grinding of salvia miltiorrhiza medicinal material, soaking and extracting in ethyl acetate, soaking and extracting medicinal dregs in water, absorbing the extract by AB-8 resin, eluting and eluting After the solution is concentrated, adjust the pH to 7-8, heat at 110°C-130°C for 30 minutes, filter, adjust the pH of the filtrate to 1-3, let stand, precipitate, filter, the filtrate is adsorbed by AB-8 resin under acidic conditions, and eluted with pure water , the eluate was adjusted to a pH value of 7-8, concentrated and dried to obtain a solid Danshensu sodium, which was recrystallized from methanol to obtain a high-purity Danshensu sodium.

Description

technical field [0001] The invention relates to a pharmaceutical technology, in particular to a preparation method of high-purity danshensu sodium. Background technique [0002] Danshen is the dry root and rhizome of Salvia miltiorrhiza Bge., which has the functions of dispelling blood stasis and relieving pain, promoting blood circulation and promoting menstruation, clearing heart and eliminating troubles. (Chinese Pharmacopoeia edition one P52 page in 2005). Salvianic acid A is an important active ingredient in its water-soluble component salvianolic acid. Its structure is β-(3,4-dihydroxyphenyl) lactic acid and it has various pharmacological activities. Because it is an unstable free acid, it is often made into sodium salt——danshensu sodium. The structure is as follows: [0003] [0004] At present, the methods for preparing high-purity Danshensu sodium include: [0005] 1. Pan Jian, Xu Tao. Preparation of Danshensu Sodium by Liquid Chromatography [J], Chinese Herb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/52C07C51/41C07C51/42A61K36/53
Inventor 於琦汪仁权
Owner HEFEI ZIJIN PHARMA TECHNOLOGICAL
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