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Method for purifying sodium aescinate

A technique for sodium aescin and extracting solution, which is applied in the field of natural medicinal chemistry, can solve the problems of excessive use of two types of organic reagents, difficulty in controlling solvent residues, etc., so as to solve the cumbersome extraction of organic reagents, reduce production costs, and reduce Dissolution effect

Inactive Publication Date: 2012-07-04
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As mentioned above, there are too many types of second-class organic reagents in the existing process, and it is difficult to control solvent residues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Grind the medicinal material of Sala chinensis, take 1kg, add 8L 95% ethanol to reflux and extract twice, filter the extract to recover ethanol under reduced pressure, add appropriate amount of water to disperse and filter the mother liquor, add 1LLSA-21 macroporous resin column for adsorption, after the adsorption is completed, use 6L 50% The ethanol solution elutes the resin column, collects the eluent and reclaims the ethanol under reduced pressure to obtain a concentrated solution, and adds the concentrated solution to Na + Type cation exchange resin column exchange transformation into sodium salt, collect the lower column liquid and adjust pH7.5 with 0.5% sodium hydroxide solution, then add AB-8 macroporous resin column to absorb impurities, add 1 / 3 volume of acetone solution to the lower column liquid to fully Stir, place the precipitate, filter to obtain 63g of the precipitate, dissolve it with 90% ethanol solution, put a short column of aluminum peroxide (neutral...

Embodiment 2

[0021] Grind the medicinal material of Sala seed, take 1kg, add 10L80% ethanol to reflux and extract twice, filter the extract to recover ethanol under reduced pressure, add appropriate amount of water to disperse and filter the mother liquor, add 1L ADS-7 macroporous resin column for adsorption, after the adsorption is completed, use 4L70 % ethanol solution to elute the resin column, collect the eluate and recover ethanol under reduced pressure to obtain a concentrated solution, and add the concentrated solution to Na + Type cation exchange resin column exchange into sodium salt, collect the lower column liquid and adjust the pH to 8 with 2% sodium hydroxide solution, then add SPD100 macroporous resin column to absorb impurities, add 1 / 2 volume of acetone solution to the lower column liquid and stir well, place it for precipitation , filtered to get 75g of precipitate, dissolved in 95% ethanol solution, aluminum peroxide short column (neutral alumina, 200-300 mesh, diameter-to...

Embodiment 3

[0023] Grind the medicinal material of Sala seed, take 1kg, add 5L of 90% ethanol to reflux and extract 3 times, filter the extract to recover ethanol under reduced pressure, add appropriate amount of water to disperse and filter the mother liquor, add 1L X-5 macroporous resin column for adsorption, after the adsorption is completed, use 5L60 % ethanol solution to elute the resin column, collect the eluate and recover ethanol under reduced pressure to obtain a concentrated solution, and add the concentrated solution to Na + Type cation exchange resin column exchange transformation into sodium salt, collect the lower column liquid and adjust pH8.5 with 1% sodium hydroxide solution, then add HZ816 macroporous resin column to absorb impurities, add 2 / 3 volume of acetone solution to the lower column liquid and stir fully, Place the precipitate, filter to obtain 82g of the precipitate, dissolve it with 90% ethanol solution, put a short column of aluminum peroxide (neutral aluminum o...

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PUM

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Abstract

The invention relates to a method for purifying sodium aescinate. The method comprises the steps of crushing Chinese buckeye seed, adding 80-95% ethanol with amount of 5-10 times than that of the Chinese buckeye seed to carry out circumfluence extraction for 2 to 3 times, pressure-reducing the extraction liquid, recycling the ethanol, dispersing and filtering mother liquor by adding right amount of water, adding macroporous resin columns for absorption, eluting by using 50-70% ethanol solution with 4-6 BV, collecting the eluting liquid, pressure-reducing and recycling the ethanol, adding cation exchange resin columns into concentrated solution, adjusting the pH (potential of hydrogen) value of the lower resin column liquid to be 7.5-8.5, adding the macroporous resin columns again for absorption, adding acetone solution into the lower column liquid, mixing fully to obtain precipitation, dissolving the precipitate by using the ethanol solution, shortening the column by using peroxide aluminum, pressure-reducing the column filtering liquid, recycling the ethanol to be in a small volume, placing for crystallization, carrying out circumfluence dissolving on crystallization products by using the ethanol solution and re-crystallizing for 1-3 times, and drying the crystallization products to obtain sodium aescinate products with content not less than 95%. By using the method for purifying sodium aescinate to produce the sodium aescinate, the process is simple, the operation is easy, the content of obtained products is high, and the method can be directly used on medicine production.

Description

Technical field: [0001] The invention belongs to the field of natural medicinal chemistry, in particular to a method for purifying sodium aescinate. Background technique: [0002] Sodium aescinate is a saponin sodium salt extracted from the seeds of salsa. It has anti-inflammatory, anti-osmotic, and detumescent effects, and is widely used in the treatment of blood circulation disorders and rheumatism. [0003] Aescin is the active ingredient of Salu, which belongs to triterpenoid saponin compounds. According to the definition of German Pharmacopoeia, its main active ingredients are aescin A, B, C and D, soluble in methanol, ethanol, chloroform, insoluble in acetone , ether, petroleum ether, etc. High-content sodium aescinate has poor solubility in aqueous solution. In order to increase solubility, it is often used as an injection in the form of sodium salt. [0004] At present, the domestic preparation process of sodium aescinate is as follows: reflux extraction of 50-70% m...

Claims

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Application Information

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IPC IPC(8): C07J63/00C07H15/256C07H1/08
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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