Method for preparing sodium tanshinol

A technology of danshensu sodium and exchange resin, which is applied in the preparation of carboxylate, the preparation of carboxylic anhydride, and medical preparations containing active ingredients, etc., can solve the problems of cumbersome steps, low selectivity, general purification effect, etc. The introduction of metal ions, the effect of saving production costs and shortening the process flow

Inactive Publication Date: 2008-10-22
NANJING ZELANG MEDICAL TECH
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AI Technical Summary

Problems solved by technology

[0005] 1. In the process of preparing Danshensu, adsorption resin, ion exchange resin, etc. are used as the main purification means. Because the properties of water-soluble impurities and Danshensu are similar, the selectivity of the above method is low, and the purification effect is general
[0006] 2. In the method disclosed in CN1868994A, too much lye is used, and a large amount of metal ions are brought in. These ions form salts with other acid radicals except danshensu in the subsequent operation process, and are precipitated together with danshensu sodium salt. affect the purity of the product
[0007] 3. In the method disclosed in CN1868994A, the steps of purifying Danshensu and preparing sodium salt are carried out separately, the steps are cumbersome, the preparation cycle is long, and the reaction conditions are not easy to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take 1 kg of Danshen medicinal material, heat and reflux twice with 0.5 mol / L hydrochloric acid aqueous solution in 8 times the amount, each time for 1.5 hours, combine the medicinal liquids, filter, and concentrate the filtrate to 5 L. Put it into a multi-stage countercurrent extractor, carry out 3-stage extraction with n-hexane-ethyl acetate (1:2) mixed solvent, remove the phase solution, add 201×7 type strong basic anion exchange resin column for adsorption, use 1mol / Elute with LNaOH solution, collect 5 times the column volume eluate, concentrate, refrigerate at 0°C, precipitate crystals, and separate the crystals to obtain the final product. This example obtains Danshensu sodium 25g (yield 2.5%), and through high performance liquid phase detection, the content of this product (calculated as Danshensu) is 98.3%.

Embodiment 2

[0038] Take 1 kg of Danshen medicinal material, heat and reflux twice with 0.5 mol / L hydrochloric acid aqueous solution with 10 times the amount, each time for 2 hours, combine the medicinal liquids, filter, and concentrate the filtrate to 5 L. All the other operations are the same as in Example 1. This example obtains Danshensu sodium 26g (yield 2.6%), and through HPLC detection, the content of this product (calculated as Danshensu) is 94.6%.

Embodiment 3

[0040] Take 1 kg of Danshen medicinal material, heat and reflux twice with 0.5 mol / L hydrochloric acid aqueous solution in 8 times the amount, each time for 1.5 hours, combine the medicinal liquids, filter, and concentrate the filtrate to 5 L. Put it into a multi-stage countercurrent extractor, carry out 3-stage extraction with n-hexane-ethyl acetate (1:1) mixed solvent, remove the phase solution, add 201×7 type strong basic anion exchange resin column for adsorption, use 1mol / Elute with LNaOH solution, collect 5 times the column volume eluate, concentrate, refrigerate at 0°C, precipitate crystals, and separate the crystals to obtain the final product. This example obtains Danshensu sodium 18g (yield 1.8%), and through HPLC detection, the content of this product (calculated as Danshensu) is 91.3%.

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PUM

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Abstract

The invention relates to a preparation method of sodium Danshensu with high purity which has simple steps and good purifying effect and which is suitable for industrialized production. The technical steps comprise: (1) extraction: the medicinal materials of salvia is heated and refluxed by a 0.5 mol / L aqueous hydrochloric solution; (2) multi-stage counter-current extraction: medical solution is infiltrated into a multi-stage counter-current extractor, multi-stage extraction is carried out by a n-hexane ethyl acetate (1:1-5) mixed solution; (3) refined salifying: the lower phase solution is taken and is added into alkaline anion exchange resin column to absorb, and uses an alkali solution containing sodium ions to elute, eluent is collected, concentrated and freezed, then sodium Danshensu is obtained after the crystallization is precipitated and separated. The preparation method of Danshensu sodium with high purity has the advantages of simple technology, high yield efficiency and good purity of products.

Description

technical field [0001] The invention relates to a preparation method of danshensu sodium, in particular to a method for extracting danshensu from danshen medicinal material and preparing its sodium salt. Background technique [0002] Danshensu sodium is the sodium salt of salvianic acid A, and Danshensu is a water-soluble component contained in the traditional Chinese medicine Salvia Miltiorrhiza Bge. It has various pharmacological activities. Because it is an unstable free acid, it is often made into salt when used [Zhang Jingze, et al. Research overview on the chemical constituents of Danshensu. Tianjin Pharmacy, 2000, 12 (4)]. [0003] CN1868994A discloses a preparation method of danshensu sodium, the method is that the lye extract of salvia miltiorrhiza is absorbed by a weakly basic ion exchange resin, eluted with alcohol and alkali respectively, the eluent is adjusted to a pH value of 1-4, and the weakly polar resin Adsorption under acidic conditions, elution with pure...

Claims

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Application Information

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IPC IPC(8): C07C59/52C07C51/41C07C51/54A61K36/53
Inventor 刘东锋范淦彬杨成东
Owner NANJING ZELANG MEDICAL TECH
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