CN1544458A - High purity astragaloside IV preparation method - Google Patents
High purity astragaloside IV preparation method Download PDFInfo
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- CN1544458A CN1544458A CNA2003101089156A CN200310108915A CN1544458A CN 1544458 A CN1544458 A CN 1544458A CN A2003101089156 A CNA2003101089156 A CN A2003101089156A CN 200310108915 A CN200310108915 A CN 200310108915A CN 1544458 A CN1544458 A CN 1544458A
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Abstract
The invention relates to a process for preparing high purity Astragaloside by using traditional Chinese medicinal astragalus root as raw material comprising the steps of extraction, desugaring, dewatering and purifying. The purity of the prepared Astragloside can reach 90-100%, thus facilitating the production of various preparations using Astragloside as active ingredient.
Description
Technical field
The invention belongs to medical technical field, being specifically related to a kind of is the method for feedstock production high-purity astragaloside with the Chinese medicinal materials Radix Astragali.
Background technology
The Radix Astragali (Radix Astragali) is the dry root of leguminous plants Radix Astagali Astragalus membranaceus (Fisch) Bge.Var.mongholicus (Bge.) Hsiao or Radix Astragali Astragalus membranaceus (Fisch) Bge., be tonic commonly used, it is sweet to distinguish the flavor of, slightly warm in nature, traditional medicine thinks that it has the effect of invigorating QI to consolidate the body surface resistance, diuresis holder poison, expelling pus and promoting granulation, and medicinal history is long.Modern study shows that the Radix Astragali has enhancing immunity, metabolism, step-down and diuretic properties, and wherein Radix Astragali saponin, especially Cyclosiversioside F are its major physiological activeconstituentss.
Summary of the invention
The purpose of this invention is to provide a kind of easy and simple to handle, productive rate is high, purity is high Cyclosiversioside F preparation method.
Among the present invention, the structure of the Cyclosiversioside F of indication is as follows:
The preparation method of the Cyclosiversioside F that the present invention proposes is a raw material with the Chinese medicinal materials Radix Astragali, comprises extraction, desugar, dehydration, all steps of purifying.Detailed process is as follows: astragalus root is pulverized, and in the atmospheric pressure reflux extraction element, the water thermal backflow is extracted 2-5 time, each refluxing extraction 30-90 minute; The water extract that merges each several part, filter, supernatant liquor directly adds on the macroporous adsorptive resins, deionized-distilled water wash-out carbohydrate part with 10-15 times of volume, 0.05～2.0% alkaline aqueous solution with 5-10 times of volume carries out wash-out again, decolours with 20～40% alcohol wash-out of 5-7 times of volume; With 70～80% alcohol wash-out, elutriant is concentrated to small volume again, and the centrifugal precipitation that obtains is Cyclosiversioside F, and its purity is 90-100%.
Among the present invention, the alkaline aqueous solution that dehydration is adopted can be the aqueous solution of sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium bicarbonate or yellow soda ash.Used macroporous adsorbent resin can have multiple, for example AB-8, D101, ZTC-1, DidaionHP20 etc.
For a better understanding of the present invention, below principle of the present invention is described as follows:
Macroporous adsorbent resin is a class organic polymer sorbent material that grows up the sixties in 20th century, has the good adsorption performance, is applied to the separation of herbal medicine chemical ingredients and the development of new Chinese medicine gradually over year surplus in the of nearly ten.Macroporous adsorbent resin be a class to be adsorbed as characteristics, organism is had the high molecular polymer of concentrating and separating effect.In the aqueous solution, macroporous adsorbent resin has the good adsorption selectivity to organism, and method that can Solid-Phase Extraction is removed carbohydrate content in the absorption Cyclosiversioside F.The physico-chemical property of macroporous adsorbent resin is stable, is insoluble to acid, alkali and organic solvent, and is better to organic selectivity, is not subjected to the influence of inorganic salts and strong ion low molecular compound.Generally speaking, acidic cpd in basic solution by desorption, basic cpd in acidic solution by desorption.Radix Astragali saponin is a neutral compound, and the pigment composition in the plant milk extract mostly is acidic cpd.Therefore, the present invention adopts dilute alkaline soln to the macroporous adsorptive resins wash-out, can be to greatest extent with the pigment impurity wash-out, and also Cyclosiversioside F is unaffected, and improve the purity of product.The adsorptive capacity of macroporous adsorbent resin is general to be inversely proportional to last sample strength of solution, adsorbs comparatively favourable usually with low concentration.The present invention takes the water extract without concentration, directly goes up the method for macroporous adsorptive resins, and Cyclosiversioside F is attracted on the resin column to greatest extent, has improved the rate of transform and the product yield of Cyclosiversioside F greatly.Cyclosiversioside F is at 70～80% alcohol wash-out positions of macroporous adsorptive resins, and after concentrating, Cyclosiversioside F is separated out owing to solubleness is less in the lower concentration alcoholic solution, and the present invention passes through the centrifugal highly purified Cyclosiversioside F that obtains, and content reaches 90～100%.
The Cyclosiversioside F of the inventive method preparation is of light color, purity is high, and the preparation method has that yield height, production cost are low, the characteristics of the easy standard of technology.
Embodiment
Further specify content of the present invention below in conjunction with embodiment:
Embodiment 1:
After astragalus root 10kg pulverizes, water refluxing extraction 2 times (60 ℃, 60min) in the heating and refluxing extraction jar.United extraction liquid joins on the AB-8 macroporous adsorptive resins, with 100 liters deionized-distilled water wash-out carbohydrate, carries out wash-out with 50 liter 0.1% aqueous sodium hydroxide solution again, continues to decolour with 50 liter 40% alcohol wash-out.With 25 liter 75% alcohol wash-out Cyclosiversioside F, elutriant is concentrated to small volume again, centrifugally obtains precipitating Cyclosiversioside F 8.9 gram, and purity is 94%.
Embodiment 2:
After astragalus root 10kg pulverizes, water refluxing extraction 4 times (80 ℃, 90min) in the heating and refluxing extraction jar.United extraction liquid joins on the D101 macroporous adsorptive resins, with 140 liters deionized-distilled water wash-out carbohydrate, carries out wash-out with 50 liter 1.0% potassium hydroxide aqueous solution again, continues to decolour with 50 liter 20% alcohol wash-out.With 25 liter 80% alcohol wash-out Cyclosiversioside F, elutriant is concentrated to small volume again, the centrifugal Cyclosiversioside F that obtains, and purity is 91%.
Embodiment 3:
After astragalus root 10kg pulverized, water refluxed and carries (70 ℃, 30min) 3 times in the heating and refluxing extraction jar.United extraction liquid joins on the ZTC-1 macroporous adsorptive resins, with 110 liters deionized-distilled water wash-out carbohydrate, carries out wash-out with 60 liter 2.0% aqueous sodium carbonate again, continues to decolour with 50 liter 30% alcohol wash-out.With 25 liter 70% alcohol wash-out Cyclosiversioside F, elutriant is concentrated to small volume again, the centrifugal Cyclosiversioside F that obtains, and purity is 95%.
Claims (3)
1, a kind of method that from Chinese medicine astragalus, prepares Cyclosiversioside F, comprise extraction, desugar, decolouring, all steps of purifying, it is characterized in that concrete technology is as follows: astragalus root is pulverized, in the atmospheric pressure reflux extraction element, water heating and refluxing extraction 2-5 time, each refluxing extraction 30-90 minute; The water extract that merges each several part, filter, supernatant liquor directly adds on the macroporous adsorptive resins, deionized-distilled water wash-out carbohydrate part with 10-15 times of volume, 0.05～2.0% alkaline aqueous solution with 5-7 times of volume carries out wash-out again, decolours with 20～40% alcohol wash-out of 5-7 times of volume; With 70～80% alcohol wash-out, elutriant is concentrated to small volume again, and the centrifugal precipitation that obtains is Cyclosiversioside F, and its purity is 90-100%.
2, preparation method according to claim 1, the alkaline aqueous solution that adopts that it is characterized in that decolouring is the aqueous solution of sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium bicarbonate or yellow soda ash.
3, preparation method according to claim 1 is characterized in that used macroporous adsorbent resin is AB-8, D101, ZTC-1, DidaionHP20.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2003101089156A CN1544458A (en) | 2003-11-27 | 2003-11-27 | High purity astragaloside IV preparation method |
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| CNA2003101089156A CN1544458A (en) | 2003-11-27 | 2003-11-27 | High purity astragaloside IV preparation method |
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| CN1544458A true CN1544458A (en) | 2004-11-10 |
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| CNA2003101089156A Pending CN1544458A (en) | 2003-11-27 | 2003-11-27 | High purity astragaloside IV preparation method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009046620A1 (en) * | 2007-09-13 | 2009-04-16 | Tianjin Institute Of Pharmaceutical Research | Cycloastragenol monoglucoside, preparation, pharmaceutical composition and application thereof |
| CN100500686C (en) * | 2006-05-12 | 2009-06-17 | 神威药业有限公司 | Method for extraction and preparation of astragaloside |
| CN100537594C (en) * | 2005-05-26 | 2009-09-09 | 中国科学院成都生物研究所 | Method for preparing purity astragaloside |
| CN101088521B (en) * | 2006-06-14 | 2010-10-27 | 北京四环科宝制药有限公司 | Astragalus medicine prepn and its prepn process |
| CN101781354B (en) * | 2009-01-16 | 2012-01-04 | 劲牌有限公司 | Production method for preparing astragaloside A |
| CN101343305B (en) * | 2007-07-11 | 2012-05-16 | 上海新康制药厂 | Preparation method for astragaloside |
| CN105481934A (en) * | 2015-12-02 | 2016-04-13 | 上海景峰制药有限公司 | Astragaloside bulk drug and preparation method thereof |
| CN105541954A (en) * | 2015-12-02 | 2016-05-04 | 上海景峰制药有限公司 | Radix astragali extract with high purity astragaloside |
-
2003
- 2003-11-27 CN CNA2003101089156A patent/CN1544458A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100537594C (en) * | 2005-05-26 | 2009-09-09 | 中国科学院成都生物研究所 | Method for preparing purity astragaloside |
| CN100500686C (en) * | 2006-05-12 | 2009-06-17 | 神威药业有限公司 | Method for extraction and preparation of astragaloside |
| CN101088521B (en) * | 2006-06-14 | 2010-10-27 | 北京四环科宝制药有限公司 | Astragalus medicine prepn and its prepn process |
| CN101343305B (en) * | 2007-07-11 | 2012-05-16 | 上海新康制药厂 | Preparation method for astragaloside |
| US20110218161A1 (en) * | 2007-09-13 | 2011-09-08 | Tianjin Institute Of Pharmaceutical Research | Cycloastragenol monoglucoside, preparation, pharmaceutical composition and application thereof |
| EP2199402A4 (en) * | 2007-09-13 | 2011-07-06 | Tianjin Inst Pharm Research | Cycloastragenol monoglucoside, preparation, pharmaceutical composition and application thereof |
| WO2009046620A1 (en) * | 2007-09-13 | 2009-04-16 | Tianjin Institute Of Pharmaceutical Research | Cycloastragenol monoglucoside, preparation, pharmaceutical composition and application thereof |
| JP2010538621A (en) * | 2007-09-13 | 2010-12-16 | テンシン インスティチュート オブ ファーマシューティカル リサーチ | Cycloastragenol monoglucoside, process for its production and use as a pharmaceutical composition |
| CN101225424B (en) * | 2007-09-13 | 2013-05-29 | 天津药物研究院 | Single-glucopyranoside of cyclomembranousol, preparation method, medicament combination and uses thereof |
| US8835134B2 (en) | 2007-09-13 | 2014-09-16 | Tianjin Institute Of Pharmaceutical Research | Cycloastragenol monoglucoside, preparation, pharmaceutical composition and application thereof |
| CN101781354B (en) * | 2009-01-16 | 2012-01-04 | 劲牌有限公司 | Production method for preparing astragaloside A |
| CN105481934A (en) * | 2015-12-02 | 2016-04-13 | 上海景峰制药有限公司 | Astragaloside bulk drug and preparation method thereof |
| CN105541954A (en) * | 2015-12-02 | 2016-05-04 | 上海景峰制药有限公司 | Radix astragali extract with high purity astragaloside |
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