CN105541954A - Radix astragali extract with high purity astragaloside - Google Patents
Radix astragali extract with high purity astragaloside Download PDFInfo
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- CN105541954A CN105541954A CN201510876069.5A CN201510876069A CN105541954A CN 105541954 A CN105541954 A CN 105541954A CN 201510876069 A CN201510876069 A CN 201510876069A CN 105541954 A CN105541954 A CN 105541954A
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- radix astragali
- astragaloside
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- purity
- extract
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J53/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by condensation with a carbocyclic rings or by formation of an additional ring by means of a direct link between two ring carbon atoms, including carboxyclic rings fused to the cyclopenta(a)hydrophenanthrene skeleton are included in this class
- C07J53/002—Carbocyclic rings fused
- C07J53/004—3 membered carbocyclic rings
Abstract
The invention relates to a radix astragali extract with high purity astragaloside, and the extract is prepared from radix astragali. The preparation method comprises the following steps: extracting radix astragali, carrying out elution to remove saccharide, discoloring the extract, and purifying the extract. In the elution and saccharide removal step, the water extract obtained in the radix astragali extraction step is filtered, then obtained supernate is pressurized into a macroporous resin column, and purified water is used to wash the macroporous resin column so as to remove saccharide impurities, wherein the volume ratio of the purified water to macroporous resin column is 10-15:1. In the discoloring step, an alkaline water solution with a volume 5 to 10 times bigger than that of the macroporous resin column is used to carry out elution, then an alcohol solution with a volume 5 to 10 times bigger than that of the macroporous resin column is used to carry out elution, finally an alcohol solution with a volume 5 to 10 times bigger than that of the macroporous resin column is used to carry out elution, three eluents are merged and concentrated to minimize the volume, then the concentrate is subjected to centrifugation, and the precipitate is the coarse product of astragaloside. In the purification step, the coarse product of astragaloside is dissolved in a proper amount of ethanol under heating, then the solution is filtered, the filtrate is stored at a temperature of 2 to 8 DEG C for 24 to 48 hours, and then the filtrate is subjected to centrifugation to obtain refined astragaloside with a purity of 98% or more.
Description
Technical field
The invention belongs to medical art, be specifically related to a kind of Radix Astragali extract containing high-purity astragaloside and preparation method thereof.
Background technology
The Radix Astragali (RadixAstragali) is the dry root of leguminous plants Radix Astagali Astragalusmembranaceus (Fisch) Bge.Var.mongholicus (Bge.) Hsiao or Radix Astragali Astragalusmembranaceus (Fisch) Bge., for conventional tonic, taste is sweet, slightly warm in nature, traditional medicine thinks that it has 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, the Radix Astragali has enhancing immunity, metabolism, step-down and diuretic properties, wherein Cyclosiversioside F, and especially Cyclosiversioside F is its major physiological activeconstituents.But the Cyclosiversioside F purity at present in Radix Astragali extract is low, and extracting method is also loaded down with trivial details.
Summary of the invention
An object of the present invention is to provide a kind of Radix Astragali extract containing high-purity astragaloside.
As the Radix Astragali extract containing high-purity astragaloside of the present invention, it is prepared from by following methods: with the Chinese medicinal materials Radix Astragali for raw material, comprises medicinal material extract step, wash-out desaccharification step, decolorization process and purification step; Wherein said wash-out desaccharification step is in the supernatant liquor pressurization input macroporous adsorptive resins obtained after the Aqueous extracts described medicinal material extract step obtained filters, and removes carbohydrate impurity with the purified water wash-out of 10 ~ 15 times of column volumes; Described decolorization process is that the alkaline aqueous solution being first 0.2 ~ 0.5% with the mass percent concentration of 5 ~ 10 times of column volumes carries out wash-out, then be the alcoholic solution wash-out of 30 ~ 60% with the mass percent concentration of 5 ~ 10 times of column volumes, be the alcoholic solution wash-out of 70 ~ 80% again with the mass percent concentration of 5 ~ 10 times of column volumes, small volume is concentrated to after three elutriants in described decolorization process merge, centrifugally to be precipitated, to be Cyclosiversioside F crude product; Described purification step, by Cyclosiversioside F crude product ethanol in proper amount heating for dissolving, filters, and filtrate carries out 2 ~ 8 DEG C of refrigerations 24 ~ 48 hours, and centrifugally obtain Cyclosiversioside F, its purity is more than 98%.
In a preferred embodiment of the invention, described medicinal material extract step is that decocting method extracts or heating reflux method extracts.
In a preferred embodiment of the invention, it is that Milkvetch Root segment 0 ~ 3cm is long that described heating reflux method extracts, in atmospheric pressure reflux extraction element, by purified water heating and refluxing extraction 2 ~ 3 times, and each refluxing extraction 90 ~ 120 minutes; Merge the Aqueous extracts of each several part.
In a preferred embodiment of the invention, the alkaline aqueous solution in described decolorization process is the aqueous solution of sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium bicarbonate or sodium carbonate.
In a preferred embodiment of the invention, the described alcoholic solution in described decolorization process is the one in methanol solution, ethanolic soln or propanol solution.
In a preferred embodiment of the invention, described macroporous adsorptive resins is AB-8, D101, HPD100, XAD-2, XAD-4, XAD-7 or DidaionHP20.
In a preferred embodiment of the invention, in described purification step, it is 55 ~ 75 DEG C by the temperature of ethanol in proper amount heating for dissolving.
For a better understanding of the present invention, below principle of the present invention is described as follows:
Macroporous adsorbent resin is the class organic polymer sorbent material grown up the sixties in 20th century, has good absorption property, is now applied to the separation of chemical composition of Chinese materia medica and developing of new Chinese medicine gradually.Macroporous adsorbent resin be a class to be adsorbed as feature, organism is had to the high molecular polymer of concentrating and separating effect.In aqueous, macroporous adsorbent resin has good adsorption selectivity to organism, can the method for Solid-Phase Extraction, is removed by carbohydrate content while absorption Cyclosiversioside F.The stable in physicochemical property of macroporous adsorbent resin, is insoluble to acid, alkali and organic solvent, better to organic selectivity, is not subject to the impact of inorganic salts and strong ion low molecular compound.Generally speaking, acidic cpd is desorbed attached in basic solution, and basic cpd is desorbed attached in an acidic solution.Cyclosiversioside F is neutral compound, and the pigment composition in plant milk extract mostly is acidic cpd.Therefore, the present invention adopts dilute alkaline soln to macroporous adsorptive resins wash-out, can to greatest extent by pigment impurity wash-out, and Cyclosiversioside F is unaffected, and improves the purity of product through the dissolving of crude product and the principle of similar crystallization.The present invention takes Aqueous extracts without concentration, directly goes up the method for macroporous adsorptive resins, and Cyclosiversioside F is attracted on resin column to greatest extent, greatly improves the rate of transform and the product yield of Cyclosiversioside F.Cyclosiversioside F macroporous adsorptive resins 70 ~ 80% alcohol wash-out position, after concentrated, Cyclosiversioside F due in low concentration alcohol solution solubleness less and separate out, centrifugally obtain crude product, again by crude product heating for dissolving in alcoholic solution, the principle separated out because Cyclosiversioside F solubleness is little after refrigeration, obtain highly purified Cyclosiversioside F through centrifugal, content reaches more than 98%.
Embodiment:
Content of the present invention is further illustrated below in conjunction with embodiment:
Embodiment 1:
After Milkvetch Root lOkg segment 2cm is long, with purifying water boiling and extraction 2 times (98 DEG C, 100min) in heating and refluxing extraction tank.United extraction liquid, 200 eye mesh screens filter, and filtered liquid joins on D101 macroporous adsorptive resins, remove carbohydrate impurity, then carry out wash-out with the aqueous sodium hydroxide solution of 60 liter 0.2%, continue with the ethanolic soln wash-out of 60 liter 30% with the purified water wash-out of 150 liters.Again with the ethanol elution of 50 liter 70%, the elutriant of latter three times is concentrated to small volume after merging, and centrifugally obtains Cyclosiversioside F crude product, crude product is added 1L ethanol and be heated to 55 DEG C of stirring and dissolving, filter, filtrate carries out 3 DEG C of refrigerations 25 hours, centrifugally obtain Cyclosiversioside F 8.2 grams, purity is 99.1%.
Embodiment 2:
After Milkvetch Root lOkg segment 3cm is long, with purifying water boiling and extraction 3 times (98 DEG C, 110min) in heating and refluxing extraction tank.United extraction liquid, 200 eye mesh screens filter, and filtered liquid joins on HP20 macroporous adsorptive resins, remove carbohydrate impurity, then carry out wash-out with the potassium hydroxide aqueous solution of 80 liter 0.3%, continue with the ethanolic soln wash-out of 80 liter 50% with the purified water wash-out of 120 liters.Again with the ethanol elution of 70 liter 76%, after the elutriant of latter three times merges, elutriant is concentrated to small volume, centrifugally obtains Cyclosiversioside F crude product, crude product is added 1L ethanol and be heated to 68 DEG C of stirring and dissolving, filter, filtrate carries out 5 DEG C of refrigerations 35 hours, centrifugally obtain Cyclosiversioside F 7.8 grams, purity is 99.7%.
Embodiment 3:
After Milkvetch Root lOkg segment 2.5cm is long, with purifying water boiling and extraction 3 times (98 DEG C, 120min) in heating and refluxing extraction tank.United extraction liquid, 200 eye mesh screens filter, and filtered liquid joins on ZTC-1 macroporous adsorptive resins, remove carbohydrate impurity, then carry out wash-out with the calcium hydroxide aqueous solution of 100 liter 0.3%, continue with the ethanolic soln wash-out of 100 liter 50% with the purified water wash-out of 150 liters.Again with the ethanol elution of 90 liter 80%, after the elutriant of latter three times merges, elutriant is concentrated to small volume, centrifugally obtains Cyclosiversioside F crude product, crude product is added 1L ethanol and be heated to 75 DEG C of stirring and dissolving, filter, filtrate carries out 6 DEG C of refrigerations 48 hours, centrifugally obtain Cyclosiversioside F 8.5 grams, purity is 99.4%.
Claims (7)
1., containing the Radix Astragali extract of high-purity astragaloside, it is characterized in that, be prepared from by following methods: with the Chinese medicinal materials Radix Astragali for raw material, comprise medicinal material extract step, wash-out desaccharification step, decolorization process and purification step; Wherein said wash-out desaccharification step is in the supernatant liquor pressurization input macroporous adsorptive resins obtained after the Aqueous extracts described medicinal material extract step obtained filters, and removes carbohydrate impurity with the purified water wash-out of 10 ~ 15 times of column volumes; Described decolorization process is that the alkaline aqueous solution being first 0.2 ~ 0.5% with the mass percent concentration of 5 ~ 10 times of column volumes carries out wash-out, then be the alcoholic solution wash-out of 30 ~ 60% with the mass percent concentration of 5 ~ 10 times of column volumes, then be the alcoholic solution wash-out of 70 ~ 80% with the mass percent concentration of 5 ~ 10 times of column volumes; Three elutriants in described decolorization process are concentrated to small volume after merging, and are centrifugally precipitated, and are Cyclosiversioside F crude product; Described purification step, by Cyclosiversioside F crude product ethanol in proper amount heating for dissolving, filters, and filtrate carries out 2 ~ 8 DEG C of refrigerations 24 ~ 48 hours, and centrifugally obtain Cyclosiversioside F, its purity is more than 98%.
2. the Radix Astragali extract containing high-purity astragaloside as claimed in claim 1, is characterized in that, described medicinal material extract step is that decocting method extracts or heating reflux method extracts.
3. the Radix Astragali extract containing high-purity astragaloside as claimed in claim 2, it is characterized in that, it is that Milkvetch Root segment 0 ~ 3cm is long that described heating reflux method extracts, in atmospheric pressure reflux extraction element, by purified water heating and refluxing extraction 2 ~ 3 times, each refluxing extraction 90 ~ 120 minutes; Merge the Aqueous extracts of each several part.
4. the Radix Astragali extract containing high-purity astragaloside as claimed in claim 1, it is characterized in that, the alkaline aqueous solution in described decolorization process is the aqueous solution of sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium bicarbonate or sodium carbonate.
5. the Radix Astragali extract containing high-purity astragaloside as claimed in claim 1, it is characterized in that, the described alcoholic solution in described decolorization process is the one in methanol solution, ethanolic soln or propanol solution.
6. the Radix Astragali extract containing high-purity astragaloside as claimed in claim 1, it is characterized in that, be AB-8, D101, HPD100, XAD-2, XAD-4, XAD-7 or DidaionHP20 at described macroporous adsorptive resins.
7. the Radix Astragali extract containing high-purity astragaloside as claimed in claim 1, it is characterized in that, in described purification step, be 55 ~ 75 DEG C by the temperature of ethanol in proper amount heating for dissolving.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739675A (en) * | 2017-10-18 | 2018-02-27 | 凤台县年丰农业发展有限责任公司 | A kind of anti-inflammatory low sugar secondary fermentation leaf of bamboo preparation of wine |
| CN111777656A (en) * | 2020-07-21 | 2020-10-16 | 山西大学 | Method for extracting astragaloside from fresh astragalus |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544458A (en) * | 2003-11-27 | 2004-11-10 | 上海博泰医药科技有限公司 | High purity astragaloside IV preparation method |
| CN1869060A (en) * | 2005-05-26 | 2006-11-29 | 中国科学院成都生物研究所 | Method for preparing purity astragaloside |
| CN101343305A (en) * | 2007-07-11 | 2009-01-14 | 上海新康制药厂 | Preparation method for astragaloside |
| CN101817861A (en) * | 2009-12-09 | 2010-09-01 | 江苏省中国科学院植物研究所 | Method for preparing high-purity astragaloside for treating diabetes nephropathy and peripheral neuritis of diabetes complications |
| CN102559828A (en) * | 2010-12-30 | 2012-07-11 | 复旦大学 | Method for preparing astragaloside IV by converting total saponins of astragalus by microorganisms |
| CN102746362A (en) * | 2011-04-19 | 2012-10-24 | 河北以岭医药研究院有限公司 | Method for extracting refined astragaloside from astragaliradix |
-
2015
- 2015-12-02 CN CN201510876069.5A patent/CN105541954A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544458A (en) * | 2003-11-27 | 2004-11-10 | 上海博泰医药科技有限公司 | High purity astragaloside IV preparation method |
| CN1869060A (en) * | 2005-05-26 | 2006-11-29 | 中国科学院成都生物研究所 | Method for preparing purity astragaloside |
| CN101343305A (en) * | 2007-07-11 | 2009-01-14 | 上海新康制药厂 | Preparation method for astragaloside |
| CN101817861A (en) * | 2009-12-09 | 2010-09-01 | 江苏省中国科学院植物研究所 | Method for preparing high-purity astragaloside for treating diabetes nephropathy and peripheral neuritis of diabetes complications |
| CN102559828A (en) * | 2010-12-30 | 2012-07-11 | 复旦大学 | Method for preparing astragaloside IV by converting total saponins of astragalus by microorganisms |
| CN102746362A (en) * | 2011-04-19 | 2012-10-24 | 河北以岭医药研究院有限公司 | Method for extracting refined astragaloside from astragaliradix |
Non-Patent Citations (1)
| Title |
|---|
| 杨晓雷等: "从黄芪生药中提取黄芪甲苷的工艺研究", 《现代化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739675A (en) * | 2017-10-18 | 2018-02-27 | 凤台县年丰农业发展有限责任公司 | A kind of anti-inflammatory low sugar secondary fermentation leaf of bamboo preparation of wine |
| 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: 20160504 |