CN102532241A - Method for purifying sodium aescinate - Google Patents
Method for purifying sodium aescinate Download PDFInfo
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- CN102532241A CN102532241A CN2010106039172A CN201010603917A CN102532241A CN 102532241 A CN102532241 A CN 102532241A CN 2010106039172 A CN2010106039172 A CN 2010106039172A CN 201010603917 A CN201010603917 A CN 201010603917A CN 102532241 A CN102532241 A CN 102532241A
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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:
The invention belongs to the crude drug field, particularly relate to a kind of method of the aescine of purifying.
Background technology:
Aescine is to extract the saponin(e sodium salt that obtains in the Wilsom Buckeye Seed, has anti-inflammatory, impervious, repercussive effect, is widely used in treatment disturbance of blood circulation and rheumatism etc.
Aescine is the effective constituent of Wilsom Buckeye Seed, belongs to triterpene saponin compound, according to the definition of Ph.G; Its main effective constituent is aescine A, B, C and D; Be dissolved in methyl alcohol, ethanol, chloroform, be insoluble to acetone, ether, sherwood oil etc., high-content aescine solubleness in the aqueous solution is relatively poor; In order to increase solubleness, often process injection and use with sodium-salt form.
Present domestic aescine preparation technology is: Wilsom Buckeye Seed is pulverized 50-70% methyl alcohol or alcohol reflux, the extracting solution concentrating under reduced pressure, and the liquid concentrator chloroform extraction reclaims chloroform and obtains crude extract, and the hot water dissolving adds Na
+The type Zeo-karb, the crystallization of lower column liquid concentrating under reduced pressure, the crystallisate dissolve with ethanol solution adds activated carbon decolorizing and repeats crystallization, and crystallisate is drying to obtain.Technology is used a large amount of chloroforms, and production cost is higher, also is difficult for producing in enormous quantities.
The Aescine purifying process has the reagent precipitator method and Amberlyst process.Like document " Aescine Study on extraction in the Wilsom Buckeye Seed ", the method that the document adopts is that 95% ethanol temperature is soaked, extracting solution activated carbon decolorizing, liquid concentrator chloroform extraction, the dry Aescine that gets." extraction separation of Aescine and purifying in the Wilsom Buckeye Seed " for another example, document disclosed method is alcoholic extraction, extracts respectively with ETHYLE ACETATE and propyl carbinol successively, uses macroporous resin and reverse chromatography column separation and purification again.As stated, existing technology also is to exist two types of organic reagent kinds to use too much, and the control dissolvent residual is difficult.
Summary of the invention:
The technical problem that the present invention will solve provides simply the purify method of aescine of a kind of technology, and this method is few at the organic consumption of production toxicity, and operator are easy to operate.
To achieve these goals, technical scheme of the present invention is following:
A kind of method of the aescine of purifying is characterized in that may further comprise the steps:
1) Wilsom Buckeye Seed is pulverized, added 5-15 and doubly measure the 80-95% alcohol reflux 2-3 time, the extracting solution decompression recycling ethanol; Mother liquor adds suitable quantity of water and disperses to filter, and adds macroporous resin column absorption, 4-6BV50-70% ethanolic soln wash-out; Collect the elutriant decompression recycling ethanol, get liquid concentrator;
2) above-mentioned liquid concentrator adds cation exchange resin column, and lower column liquid is regulated pH7.5-8.5 and added macroporous resin column absorption again, and lower column liquid adds acetone soln and fully stirs, and crosses and filters throw out;
3) above-mentioned throw out is used dissolve with ethanol solution, and peroxo-aluminium short column is crossed post liquid decompression recycling ethanol to small volume, places crystallization, and crystallisate is ethanolic soln backflow dissolving-recrystallization 1-3 time again, and crystallisate is drying to obtain the aescine product, and content is not less than 95%.
A kind of among the optional LSA-21 of macroporous resin model, S-8 or the ADS-7 in the said step 1).
Said step 2) alkali of the adjusting pH in is the aqueous sodium hydroxide solution of 0.5-2%.
Said step 2) Zeo-karb in is Na
+The type Zeo-karb, the optional AB-8 of macroporous resin model, SPD100 or HZ816's is a kind of.
Aluminum oxide in the said step 3) is a neutral alumina.
The present invention adopts the high density ethanol-extracted, can reduce polysaccharide and proteic stripping; Secondly with behind the polar macroporous resin concentration,, regulate in the pH weakly alkaline solution through non-polar macroporous resin absorption impurity by its salify through resin cation(R.C.), solved loaded down with trivial details that the organic reagent of existing technology extracts, also reduced production cost; Also have method to adopt alumina removal of impurities and further decolouring, specific activity carbon decoloring yield is high, operates also simple.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment:
Embodiment 1
The Wilsom Buckeye Seed pulverizing medicinal materials is got 1kg, adds the 8L95% alcohol reflux 2 times; Filter the extracting solution decompression recycling ethanol, mother liquor adds suitable quantity of water and disperses to filter, and adds the absorption of 1LLSA-21 macroporous resin column; Absorption finishes, and with 6L50% ethanolic soln wash-out resin column, collects the elutriant decompression recycling ethanol; Get liquid concentrator, liquid concentrator is added Na
+The exchange of type cation exchange resin column makes the transition into sodium salt, collects lower column liquid and regulates pH7.5 with 0.5% sodium hydroxide solution, adds AB-8 macroporous resin column absorption impurity again; Lower column liquid adds 1/3 volume acetone soln and fully stirs, and places deposition, crosses and filters throw out 63g; Use 90% dissolve with ethanol solution, peroxo-aluminium short column (neutral alumina, 120-200 order; Blade diameter length ratio 1: 3), crosses post liquid decompression recycling ethanol, place crystallization to 100ml; Crystallisate is 95% ethanolic soln backflow dissolving again, is concentrated into 1/4 volume, recrystallization 2 times; Crystallisate is drying to obtain white aescine product 18g, through performance liquid detection level 96.3% (aescine A, B, C, D sum).
Embodiment 2
The Wilsom Buckeye Seed pulverizing medicinal materials is got 1kg, adds the 10L80% alcohol reflux 2 times; Filter the extracting solution decompression recycling ethanol, mother liquor adds suitable quantity of water and disperses to filter, and adds the absorption of 1L ADS-7 macroporous resin column; Absorption finishes, and with 4L70% ethanolic soln wash-out resin column, collects the elutriant decompression recycling ethanol; Get liquid concentrator, liquid concentrator is added Na
+The exchange of type cation exchange resin column makes the transition into sodium salt, collects lower column liquid and regulates pH8 with 2% sodium hydroxide solution, adds SPD100 macroporous resin column absorption impurity again; Lower column liquid adds 1/2 volume acetone soln and fully stirs, and places deposition, crosses and filters throw out 75g; Use 95% dissolve with ethanol solution, peroxo-aluminium short column (neutral alumina, 200-300 order; Blade diameter length ratio 1: 2), crosses post liquid decompression recycling ethanol, place crystallization to 120ml; Crystallisate is 90% ethanolic soln backflow dissolving again, is concentrated into 1/10 volume, recrystallization 3 times; Crystallisate is drying to obtain white aescine product 23g, through performance liquid detection level 95.2% (aescine A, B, C, D sum).
Embodiment 3:
The Wilsom Buckeye Seed pulverizing medicinal materials is got 1kg, adds the 5L90% alcohol reflux 3 times; Filter the extracting solution decompression recycling ethanol, mother liquor adds suitable quantity of water and disperses to filter, and adds the absorption of 1L X-5 macroporous resin column; Absorption finishes, and with 5L60% ethanolic soln wash-out resin column, collects the elutriant decompression recycling ethanol; Get liquid concentrator, liquid concentrator is added Na
+The exchange of type cation exchange resin column makes the transition into sodium salt, collects lower column liquid and regulates pH8.5 with 1% sodium hydroxide solution, adds HZ816 macroporous resin column absorption impurity again; Lower column liquid adds 2/3 volume acetone soln and fully stirs, and places deposition, crosses and filters throw out 82g; Use 90% dissolve with ethanol solution, peroxo-aluminium short column (neutral alumina, 120-300 order; Blade diameter length ratio 1: 3), crosses post liquid decompression recycling ethanol, place crystallization to 150ml; Crystallisate is 95% ethanolic soln backflow dissolving again, is concentrated into 1/8 volume, recrystallization 2 times; Crystallisate is drying to obtain white aescine product 21g, through performance liquid detection level 95.7% (aescine A, B, C, D sum).
Embodiment 4:
The Wilsom Buckeye Seed pulverizing medicinal materials is got 10kg, adds the 100L85% alcohol reflux 2 times; Filter the extracting solution decompression recycling ethanol, mother liquor adds suitable quantity of water and disperses to filter, and adds the absorption of 10L LSA-21 macroporous resin column; Absorption finishes, and with 50L65% ethanolic soln wash-out resin column, collects the elutriant decompression recycling ethanol; Get liquid concentrator, liquid concentrator is added Na
+The exchange of type cation exchange resin column makes the transition into sodium salt, collects lower column liquid and regulates pH7.5 with 0.5% sodium hydroxide solution, adds HZ816 macroporous resin column absorption impurity again; Lower column liquid adds 1/2 volume acetone soln and fully stirs, and places deposition, crosses and filters throw out 785g; Use 80% dissolve with ethanol solution, peroxo-aluminium short column (neutral alumina, 200-300 order; Blade diameter length ratio 1: 2), crosses post liquid decompression recycling ethanol, place crystallization to 1.3L; Crystallisate is 90% ethanolic soln backflow dissolving again, is concentrated into 1/7 volume, recrystallization 3 times; Crystallisate is drying to obtain white aescine product 207g, through performance liquid detection level 96.3% (aescine A, B, C, D sum).
Claims (5)
1. the method for the aescine of purifying is characterized in that may further comprise the steps:
1) Wilsom Buckeye Seed is pulverized, added 5-15 and doubly measure the 80-95% alcohol reflux 2-3 time, the extracting solution decompression recycling ethanol; Mother liquor adds suitable quantity of water and disperses to filter, and adds macroporous resin column absorption, 4-6BV50-70% ethanolic soln wash-out; Collect the elutriant decompression recycling ethanol, get liquid concentrator;
2) above-mentioned liquid concentrator adds cation exchange resin column, and lower column liquid is regulated pH7.5-8.5 and added macroporous resin column absorption again, and lower column liquid adds acetone soln and fully stirs, and crosses and filters throw out;
3) above-mentioned throw out is used dissolve with ethanol solution, and peroxo-aluminium short column is crossed post liquid decompression recycling ethanol to small volume, places crystallization, and crystallisate is ethanolic soln backflow dissolving-recrystallization 1-3 time again, and crystallisate is drying to obtain the aescine product, and content is not less than 95%.
2. according to the method for the said purification aescine of claim 1, it is characterized in that a kind of among the optional LSA-21 of macroporous resin model, S-8 or the ADS-7 in the said step 1).
3. according to the method for the said purification aescine of claim 1, it is characterized in that said step 2) in the alkali of adjusting pH be the aqueous sodium hydroxide solution of 0.5-2%.
4. according to the method for the said purification aescine of claim 1, it is characterized in that said step 2) in Zeo-karb be Na+ type Zeo-karb, the optional AB-8 of macroporous resin model, SPD-100 or HZ816's is a kind of.
5. according to the method for the said purification aescine of claim 1, it is characterized in that the aluminum oxide in the said step 3) is a neutral alumina.
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| CN2010106039172A CN102532241A (en) | 2010-12-24 | 2010-12-24 | Method for purifying sodium aescinate |
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| CN2010106039172A CN102532241A (en) | 2010-12-24 | 2010-12-24 | Method for purifying sodium aescinate |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103461599A (en) * | 2013-09-24 | 2013-12-25 | 北京绿源求证科技发展有限责任公司 | Health tea granule for constipation based on diet therapy |
| CN103808665A (en) * | 2012-11-09 | 2014-05-21 | 山东绿叶制药有限公司 | Method for determining content of multi-index components in purification process of Chinese buckeye seed extractive |
| CN104402963A (en) * | 2014-10-29 | 2015-03-11 | 武汉爱民制药有限公司 | Sodium aescinate preparation method |
| CN104804060A (en) * | 2015-05-07 | 2015-07-29 | 西安蓝绿卓生物科技有限公司 | Preparing method of sodium aescinate, external use preparation comprising same and application thereof |
| CN106491672A (en) * | 2016-11-04 | 2017-03-15 | 哈尔滨珍宝制药有限公司 | Otoginsenoside composition of sodium and preparation method thereof |
| CN106554384A (en) * | 2016-11-04 | 2017-04-05 | 陕西省西安植物园 | A kind of method that otoginsenoside is purified in the medicinal extract from buckeye |
| CN106589045A (en) * | 2016-12-06 | 2017-04-26 | 北京中医药大学 | Method for preparing aescin of Chinese buckeye seeds |
| CN106866775A (en) * | 2017-01-22 | 2017-06-20 | 张伯庆 | A kind of preparation method of Sodium Aescinate |
| CN107759656A (en) * | 2016-08-22 | 2018-03-06 | 黑龙江迪龙制药有限公司 | A kind of preparation method of Sodium Aescinate |
| WO2018113285A1 (en) * | 2016-12-22 | 2018-06-28 | 深圳翰宇药业股份有限公司 | Method for preparing sodium aescinate |
| CN110862429A (en) * | 2018-08-28 | 2020-03-06 | 无锡凯夫制药有限公司 | Preparation method of sodium aescinate |
| CN111363000A (en) * | 2020-04-13 | 2020-07-03 | 武汉爱民制药股份有限公司 | Method for separating and preparing two trace components from sodium aescinate |
| CN111454319A (en) * | 2020-04-13 | 2020-07-28 | 湖北李时珍药物研究有限公司 | Method for separating and preparing trace components from sodium aescinate |
| CN112724192A (en) * | 2020-12-31 | 2021-04-30 | 上海珈凯生物科技有限公司 | Method for extracting and preparing aescine sodium from buckeye seeds |
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Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103808665A (en) * | 2012-11-09 | 2014-05-21 | 山东绿叶制药有限公司 | Method for determining content of multi-index components in purification process of Chinese buckeye seed extractive |
| CN103461599A (en) * | 2013-09-24 | 2013-12-25 | 北京绿源求证科技发展有限责任公司 | Health tea granule for constipation based on diet therapy |
| CN104402963A (en) * | 2014-10-29 | 2015-03-11 | 武汉爱民制药有限公司 | Sodium aescinate preparation method |
| CN104804060A (en) * | 2015-05-07 | 2015-07-29 | 西安蓝绿卓生物科技有限公司 | Preparing method of sodium aescinate, external use preparation comprising same and application thereof |
| CN107759656A (en) * | 2016-08-22 | 2018-03-06 | 黑龙江迪龙制药有限公司 | A kind of preparation method of Sodium Aescinate |
| CN106554384B (en) * | 2016-11-04 | 2018-09-28 | 陕西省西安植物园 | A method of purifying otoginsenoside from buckeye medicinal extract |
| CN106491672A (en) * | 2016-11-04 | 2017-03-15 | 哈尔滨珍宝制药有限公司 | Otoginsenoside composition of sodium and preparation method thereof |
| CN106554384A (en) * | 2016-11-04 | 2017-04-05 | 陕西省西安植物园 | A kind of method that otoginsenoside is purified in the medicinal extract from buckeye |
| CN106491672B (en) * | 2016-11-04 | 2019-02-26 | 哈尔滨珍宝制药有限公司 | Otoginsenoside composition of sodium and preparation method thereof |
| CN106589045A (en) * | 2016-12-06 | 2017-04-26 | 北京中医药大学 | Method for preparing aescin of Chinese buckeye seeds |
| CN106589045B (en) * | 2016-12-06 | 2018-11-02 | 北京中医药大学 | The preparation method of buckeye otoginsenoside |
| CN108218948A (en) * | 2016-12-22 | 2018-06-29 | 深圳翰宇药业股份有限公司 | A kind of preparation method of Sodium Aescinate |
| WO2018113285A1 (en) * | 2016-12-22 | 2018-06-28 | 深圳翰宇药业股份有限公司 | Method for preparing sodium aescinate |
| CN108218948B (en) * | 2016-12-22 | 2021-01-15 | 深圳翰宇药业股份有限公司 | Preparation method of sodium aescinate |
| CN106866775A (en) * | 2017-01-22 | 2017-06-20 | 张伯庆 | A kind of preparation method of Sodium Aescinate |
| CN110862429A (en) * | 2018-08-28 | 2020-03-06 | 无锡凯夫制药有限公司 | Preparation method of sodium aescinate |
| CN111363000A (en) * | 2020-04-13 | 2020-07-03 | 武汉爱民制药股份有限公司 | Method for separating and preparing two trace components from sodium aescinate |
| CN111454319A (en) * | 2020-04-13 | 2020-07-28 | 湖北李时珍药物研究有限公司 | Method for separating and preparing trace components from sodium aescinate |
| CN111363000B (en) * | 2020-04-13 | 2021-05-18 | 武汉爱民制药股份有限公司 | Method for separating and preparing two trace components from sodium aescinate |
| CN111454319B (en) * | 2020-04-13 | 2021-08-20 | 湖北李时珍药物研究有限公司 | Method for separating and preparing trace components from sodium aescinate |
| CN112724192A (en) * | 2020-12-31 | 2021-04-30 | 上海珈凯生物科技有限公司 | Method for extracting and preparing aescine sodium from buckeye seeds |
| CN112724192B (en) * | 2020-12-31 | 2021-11-30 | 上海珈凯生物科技有限公司 | Method for extracting and preparing aescine sodium from buckeye seeds |
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Application publication date: 20120704 |