Method of preparing high-purity tanshinone IIA sodium sulfonate

A technology of tanshinone and sodium sulfonate, applied in steroids, organic chemistry and other directions, can solve the problems of poor tanshinone IIA product purity, low yield of tanshinone IIA sodium sulfonate, and increased patient risk.

Inactive Publication Date: 2014-01-08
KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
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Problems solved by technology

At present, there are few researches on the preparation process conditions of sodium tanshinone IIA sulfonate, and the yield of sodium tanshinone IIA sulfonate obtained is low, and the purity of the obtained tanshino...

Method used

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  • Method of preparing high-purity tanshinone IIA sodium sulfonate
  • Method of preparing high-purity tanshinone IIA sodium sulfonate
  • Method of preparing high-purity tanshinone IIA sodium sulfonate

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Embodiment 1

[0018]

[0019] Add 80 grams of commercially available tanshinone extract (about 60% of tanshinone IIA content) to 140 ml of glacial acetic acid, then add 240 ml of acetic anhydride, and stir and cool the resulting mixture in an ice-water bath. Add 120 ml of a mixture of concentrated sulfuric acid / glacial acetic acid (1 / 1) dropwise to the reaction solution, and keep the temperature of the reaction solution below 5°C during the dropwise addition. After the dropwise addition was completed, stirring was continued for 1.5 hours until the reaction was complete. In an ice-water bath, the reaction solution was slowly poured into an equal volume of distilled water, and 1.2 liters of saturated sodium chloride aqueous solution was added immediately, and solids were precipitated. The solid suspension obtained above is centrifuged, and the precipitate is washed twice with saturated sodium chloride solution, and then washed once with an appropriate amount of water, so that the pH of the...

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Abstract

The invention provides a method of preparing high-purity tanshinone IIA sodium sulfonate. According to the method, a tanshinone IIA crude product is subjected to a sulfonation reaction, side reactions are reduced by means of control over the reaction temperature, and an organic solvent extraction method is used for removing organic soluble impurities which are not reacted so as to obtain the high-purity tanshinone IIA sodium sulfonate. By means of high performance liquid chromatography for measurement, the content of tanshinone IIA sodium sulfonate in the product is above 95%, and the quantity of a single impurity is below 2%.

Description

field of invention [0001] The invention relates to a method for preparing high-purity sodium tanshinone IIA sulfonate, that is, by controlling the reaction temperature, reducing side reactions, and utilizing an organic solvent extraction method to remove unreacted organic soluble impurities to obtain high-purity tanshinone IIA sulfonate Sodium acid. Background technique [0002] Tanshinone IIA is a fat-soluble active ingredient extracted from the traditional Chinese medicine Danshen (Slavia miltiorrhiza Bge.) of the Labiatae family. Its metabolites in the body can participate in various biochemical reactions of the body and exhibit various pharmacological effects. It is often used in the treatment of angina pectoris, high blood pressure and cardiovascular and cerebrovascular diseases. However, because of its poor solubility in water and poor absorption and utilization in the body, the pharmacological effects are not easy to play, the onset time is slow, and the dosage is la...

Claims

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Application Information

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IPC IPC(8): C07J73/00
Inventor 夏成峰李大山王连富
Owner KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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