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Method for refining tanshinoneIIA sodium sulfonate

A refining method and sodium sulfonate technology are applied in the preparation of steroids, chemical instruments and methods, steroidal compounds, etc., which can solve the problems of large solvent usage, ineffective effect, and insufficient purity for injections, etc., and achieve low cost, The effect of simple method and easy operation

Inactive Publication Date: 2008-06-18
YAOPHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At room temperature, Tanshinone II A The solubility of sodium sulfonate in general organic solvents (such as methanol, ethanol, acetone, etc.) and polar solvents (such as water) is very small, even if the temperature is raised to reflux temperature such as 70-80 ° C, the solubility increases slightly, but it is carried out with a single solvent. The recrystallization effect is not obvious, and the amount of solvent used is large. After the refined sample is analyzed by HPLC, the content can only be about 93-97%, and the purity cannot meet the requirements of injections

Method used

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  • Method for refining tanshinoneIIA sodium sulfonate
  • Method for refining tanshinoneIIA sodium sulfonate
  • Method for refining tanshinoneIIA sodium sulfonate

Examples

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Effect test

Embodiment 1

[0031] In a 100ml reaction bottle, add Tanshinone II A Sodium sulfonate crude product 1.0g (commercially available, HPLC method content 93.6%, m.p. = 234 ° C ~ 235 ° C, see attached Figure 1 ,), suspended in a mixed solvent consisting of 7ml of deionized water, 1ml of acetone and 6ml of absolute ethanol, fully stirred, the temperature of the water bath was raised to 50°C to 55°C until all the samples were dissolved, hot filtered, the filter residue was discarded, and the filtrate was slowly cooled to 5 ℃, crystallize for 4 hours, filter, and place the filter cake in a vacuum drying oven A Sodium sulfonate pure product 0.8g, m.p. = 239 ℃ ~ 240 ℃ (measured by X-4 micro melting point apparatus, Shanghai Precision Scientific Instrument Co., Ltd.), the yield is 80.0%, and the content is 100.1% based on dry product.

Embodiment 2

[0033] In a 250ml reaction bottle, add Tanshinone II A Sodium sulfonate crude product 16.0g (same as Example 1), is suspended in the mixed solvent that 80ml deionized water and 80ml acetone form, fully stirs, and water bath is warmed up to 50 ℃~55 ℃ to sample all dissolvings, heat filtration, discard filter residue, Slowly lower the temperature of the filtrate to 0°C, crystallize for 4 hours, filter, and place the filter cake in a vacuum drying oven A 12.9g of pure sodium sulfonate, m.p.=238°C-240°C, yield 80.6%, content of dry product is 99.9%.

Embodiment 3

[0035] In a 250ml reaction bottle, add Tanshinone II A Sodium sulfonate crude product 16.0g (same as Example 1), is suspended in the mixed solvent that 80ml deionized water and 80ml acetone form, fully stirs, and water bath is warmed up to 40 ℃~45 ℃ to all dissolving of sample, heat filtration, discard filter residue, The filtrate was slowly cooled to 30°C, crystallized for 4 hours, filtered, and the filter cake was fully washed with about 10ml of iced deionized water, drained and placed in a stainless steel shallow tray for freeze-drying (-40°C-35°C, 30- 36h), namely Tanshinone II A Sodium sulfonate pure product 12.7g, m.p.=239 ℃~240 ℃ (same as embodiment 1), yield 63.4%, content is 101.3% with dry product.

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Abstract

The invention relates to a refining method of tanshinone II sulfonate. The method comprises the following procedures, firstly the crude tanshinone II sulfonate to be purified is added into the mixture solution of the organic solvent and water, heated to 40 to 60 DEG C, agitated to dissolve and filtered to remove the insoluble particles; secondly, the filtrate is slowly decreased to the temperature of 0 to 30 DEG C and crystallized and filtered; thirdly tanshinone II sulfonate with high purity is obtained after the vacuum drying. The contents of tanshinone II sulfonate can reach 99.5 percent and the quality can meet the purity requirement of raw medicine for injection by HPLC analysis. The method of the invention has the advantages of simple method, easy operation, low refining cost and being suitable for the industrialized production.

Description

technical field [0001] Invention related to Tanshinone II A The refining method of sodium sulfonate bulk drug. Background technique [0002] Salvia miltiorrhiza Bye (Salvia miltiorrhiza Bye) is a traditional Chinese medicinal material commonly used in my country. It has a long history of application and has a history of nearly 2,000 years. It is an important commodity in the domestic and foreign medicinal material markets. This product is the dry root and rhizome of Salvia miltiorr hiza Bye. It is included in the first volume of the 2005 edition of "Pharmacopia of the People's Republic of China". Its application was first recorded in "Shen Nong's Materia Medica" in the Eastern Han Dynasty. The main ingredients are: furophenanthrenequinone pigments Tanshinone I, Tanshinone II A , tanshinone III, cryptotanshinone, salvianic acid, methyl tanshinate, isotanshinone I, isotanshinone II, isotanshinone, tanshinone, tanshinol I and tanshinol II, in addition, it also contains vita...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J73/00C07J75/00
Inventor 刘永红王小霞谭俊杰刘平
Owner YAOPHARMA CO LTD
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