CN103421074A - Method for preparing high purity astragaloside from radix astragali - Google Patents
Method for preparing high purity astragaloside from radix astragali Download PDFInfo
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- CN103421074A CN103421074A CN2012101505697A CN201210150569A CN103421074A CN 103421074 A CN103421074 A CN 103421074A CN 2012101505697 A CN2012101505697 A CN 2012101505697A CN 201210150569 A CN201210150569 A CN 201210150569A CN 103421074 A CN103421074 A CN 103421074A
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Abstract
The present invention relates to a method for preparing high purity astragaloside by using Chinese medicine of radix astragali as a raw material, and the method comprises steps of extraction, hydrolysis, sugar removal, impurity removal and purification. The astragaloside prepared by the method has a purity of 95-100%, and is convenient for preparation of various preparations with the astragaloside as an effective component. The method of the invention has high yield and low production cost, and is convenient for industrial application.
Description
Technical field
The invention belongs to medical technical field, specific design is a kind of take the Chinese medicinal materials Radix Astragali and prepares the method for high-purity astragaloside as raw material.
Background technology
The Radix Astragali (Radix Astragali) is the dry root of leguminous plants Radix Astagali Astragalus menbranaceus (Fisch) Bge.Var.mongholicus (Bge) Hsiao or Radix Astragali Astragalus menbranaceus (Fisch) Bge., for tonic commonly used, distinguish the flavor of sweet, slightly warm in nature, traditional medicine thinks that it has invigorating QI to consolidate the body surface resistance, diuresis holder poison, the effect of expelling pus and promoting granulation, medicinal history is long.Modern study shows, the Radix Astragali has the immunity of enhancing, 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.
The preparation method of the Cyclosiversioside F that the present invention proposes, take the Chinese medicinal materials Radix Astragali as raw material, comprises extraction, hydrolysis, desugar, removal of impurities, all steps of purifying.Detailed process is as follows: astragalus root pulverized, and in the atmospheric pressure reflux extraction element, water heating and refluxing extraction 2-5 time, each refluxing extraction 90-150 minute; The water extraction liquid that merges each several part, filter, supernatant liquor directly adds alkali lye, standing 2-5 hour, it is neutral regulating pH value with dilute hydrochloric acid, adsorbed with macroporous adsorptive resins, with the deionized-distilled water wash-out carbohydrate part of 10-15 times of volume, then decoloured with 30～50% alcohol wash-out of 5-7 times of volume; With 70～90% alcohol wash-out, elutriant is concentrated to small volume again, centrifugal being precipitated, and precipitation is used the 5-20% ethyl alcohol recrystallization, is Cyclosiversioside F, and its purity is 95-100%.
In the present invention, what hydrolysis adopted is that alkaline aqueous solution can be the aqueous solution for sodium hydroxide, potassium hydroxide, calcium hydroxide.Macroporous adsorbent resin used can have a variety of, such as AB-8, D101, ZTC-1 etc.
For a better understanding of the present invention, below principle of the present invention is described as follows:
Contain the similar saponin(e of a large amount of Cyclosiversioside Fs in Radix Astragali extractive solution, mostly by adding low concentration alkali lye to place long-time (being generally more than 12 hours), or reflux in traditional technology, so that its analogue hydrolysis obtains Cyclosiversioside F as much as possible.This technique is found through research, adopts the alkali lye of higher concentration, utilizes the natural temperature of liquid, places about two hours and can reach desirable hydrolysis effect.
Macroporous adsorbent resin is the class organic polymer sorbent material grown up the sixties in 20th century, has good absorption property, is applied to gradually in the recent decade the separation of Chemical Constituents of Chinese Traditional And Folk Medicine and developing of new Chinese medicine.Macroporous adsorbent resin be a class to be adsorbed as characteristics, organism is had to the high molecular polymer of concentrating and separating effect.In the aqueous solution, macroporous adsorbent resin has good adsorption selectivity to organism, method that can Solid-Phase Extraction, in the absorption Cyclosiversioside F, carbohydrate content is removed, the physico-chemical property of macroporous adsorbent resin is stable, be insoluble to acid, alkali and organic solvent, better to organic selectivity, be not subject to the impact of inorganic salts and strong ion low molecular compound.General and the loading strength of solution of the adsorptive capacity of macroporous adsorbent resin is inversely proportional to, and usually with lower concentration, is adsorbed comparatively favourable.The present invention takes aqueous extract without concentration, directly goes up the method for macroporous adsorptive resins, and Cyclosiversioside F is attracted on resin column to greatest extent, has improved greatly the rate of transform and the product yield of Cyclosiversioside F.Cyclosiversioside F is at 70～90% alcohol wash-out positions of macroporous adsorptive resins, after concentrated, Cyclosiversioside F is separated out because in the lower concentration alcoholic solution, resolution is less, the present invention is through centrifugal being precipitated, obtain highly purified Cyclosiversioside F via lower concentration alcohol recrystallization again, content reaches 95～100%.
Cyclosiversioside F prepared by the inventive method is of light color, purity is high, and the preparation method has that yield is high, production cost is low, the characteristics of industrial easy standard.
Embodiment
Further illustrate content of the present invention below in conjunction with embodiment:
Embodiment 1:
After astragalus root 10kg pulverizes, water refluxing extraction 2 times (100 ℃, 90min) in the heating and refluxing extraction tank.United extraction liquid, add 5%NaOH100L, and standing 2 hours, regulate PH to 7 left and right with dilute hydrochloric acid, with the AB-8 macroporous adsorptive resins, adsorbed, with the deionized-distilled water wash-out carbohydrate of 100 liters, then decoloured with the alcohol wash-out of 50 liter 40%.With the alcohol wash-out Cyclosiversioside F of 25 liter 85%, elutriant is concentrated to small volume again, and centrifugal being precipitated, with 500ml10% Cyclosiversioside F recrystallization, obtains Cyclosiversioside F 9.4 grams, and purity is 97%.
Embodiment 2:
After astragalus root 10kg pulverizes, water refluxing extraction 2 times (100 ℃, 120min) in the heating and refluxing extraction tank.United extraction liquid, add 10%NaOH100L, and standing 2 hours, regulate PH to 7 left and right with dilute hydrochloric acid, with the AB-8 macroporous adsorptive resins, adsorbed, with the deionized-distilled water wash-out carbohydrate of 150 liters, then decoloured with the alcohol wash-out of 80 liter 30%.With the alcohol wash-out Cyclosiversioside F of 40 liter 80%, elutriant is concentrated to small volume again, and centrifugal being precipitated, with 1000ml5% Cyclosiversioside F recrystallization, obtains Cyclosiversioside F 12.1 grams, and purity is 96%.
Embodiment 3:
After astragalus root 10kg pulverizes, water refluxing extraction 3 times (100 ℃, 90min) in the heating and refluxing extraction tank.United extraction liquid, add 10%CaOH200L, and standing 4 hours, regulate PH to 7 left and right with dilute hydrochloric acid, with the D101 macroporous adsorptive resins, adsorbed, with the deionized-distilled water wash-out carbohydrate of 150 liters, then decoloured with the alcohol wash-out of 60 liter 35%.With the alcohol wash-out Cyclosiversioside F of 50 liter 80%, elutriant is concentrated to small volume again, and centrifugal being precipitated, with 1000ml5% Cyclosiversioside F recrystallization, obtains Cyclosiversioside F 11.3 grams, and purity is 98%.
Claims (3)
1. a method for preparing high-purity astragaloside from the Radix Astragali, comprise extraction, hydrolysis, desugar, removal of impurities, 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 90-150 minute; The water extraction liquid that merges each several part, filter, supernatant liquor directly adds alkali lye, standing 2-5 hour, it is neutral regulating pH value with dilute hydrochloric acid, adsorbed with macroporous adsorptive resins, with the deionized-distilled water wash-out carbohydrate part of 10-15 times of volume, then decoloured with 30～50% alcohol wash-out of 5-7 times of volume; With 70～90% alcohol wash-out, elutriant is concentrated to small volume again, centrifugal being precipitated, and precipitation is used the 5-20% ethyl alcohol recrystallization, is Cyclosiversioside F, and its purity is 95-100%.
2. preparation method according to claim 1, is characterized in that the aqueous solution that alkaline aqueous solution that hydrolysis adopts is sodium hydroxide, potassium hydroxide, calcium hydroxide.
3. preparation method according to claim 1, is characterized in that macroporous adsorbent resin used is AB-8, D101, ZTC-1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104117044A (en) * | 2014-07-25 | 2014-10-29 | 河南科技大学第一附属医院 | Preparation method of traditional Chinese medicine (TCM) decoction for treating constipation |
| CN104127844A (en) * | 2014-07-25 | 2014-11-05 | 河南科技大学第一附属医院 | Preparation method for traditional Chinese medicine preparation used for treating senile constipation |
| CN105399795A (en) * | 2015-11-02 | 2016-03-16 | 黑龙江中医药大学 | Method for extracting astragaloside from radix astragali |
| CN107365344A (en) * | 2017-07-21 | 2017-11-21 | 安徽龙津生物科技有限公司 | A kind of method of the extraction purification Astragaloside IV from astragalus root |
| CN111777656A (en) * | 2020-07-21 | 2020-10-16 | 山西大学 | Method for extracting astragaloside from fresh astragalus |
-
2012
- 2012-05-16 CN CN2012101505697A patent/CN103421074A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104117044A (en) * | 2014-07-25 | 2014-10-29 | 河南科技大学第一附属医院 | Preparation method of traditional Chinese medicine (TCM) decoction for treating constipation |
| CN104127844A (en) * | 2014-07-25 | 2014-11-05 | 河南科技大学第一附属医院 | Preparation method for traditional Chinese medicine preparation used for treating senile constipation |
| CN105399795A (en) * | 2015-11-02 | 2016-03-16 | 黑龙江中医药大学 | Method for extracting astragaloside from radix astragali |
| CN107365344A (en) * | 2017-07-21 | 2017-11-21 | 安徽龙津生物科技有限公司 | A kind of method of the extraction purification Astragaloside IV from astragalus root |
| CN111777656A (en) * | 2020-07-21 | 2020-10-16 | 山西大学 | Method for extracting astragaloside from fresh astragalus |
| CN111777656B (en) * | 2020-07-21 | 2023-04-18 | 山西大学 | Method for extracting astragaloside from fresh astragalus |
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Application publication date: 20131204 |