CN103232468A - Method for extracting purified oridonin from rabdosia rubescens - Google Patents
Method for extracting purified oridonin from rabdosia rubescens Download PDFInfo
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- CN103232468A CN103232468A CN201310179293XA CN201310179293A CN103232468A CN 103232468 A CN103232468 A CN 103232468A CN 201310179293X A CN201310179293X A CN 201310179293XA CN 201310179293 A CN201310179293 A CN 201310179293A CN 103232468 A CN103232468 A CN 103232468A
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- rabdosia rubescens
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- rubescensine
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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Abstract
The invention discloses a method for preparing oridonin from rabdosia rubescens. The method comprises the following steps of: (1), crushing rabdosia rubescens material, adding 60%-90% methanol solution for ultrasonically extracting for two to three times with each time being 20-50 minutes, combining and filtering, adding an ultra-filtration membrane for ultra-filtration, concentrating permeate in vacuum under reduced pressure to obtain a concentrated solution; (2), adding the concentrated solution to macroporous resin for adsorbing and evaporating moisture and packing, using a mixed solution of dichloromethane and acetone for eluting, collecting fraction components, and concentrating under reduced pressure; and extracting the concentrated solution by an ethyl acetate solution and collecting the extracting solution; (3), and purifying the concentrated extracting solution by adopting high-speed counter-current chromatography, carrying out online monitoring by an ultraviolet detector, collecting target components according to a figure, recycling a reagent and drying under reduced pressure to obtain the oridonin. The method for preparing the oridonin is simple to operate, high in product yield, high in purity, capable of recycling the reagent and low in production cost.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, particularly a kind of method of utilizing high speed adverse current chromatogram from Rabdosia rubescens, to extract the purifying rubescensine A.
Background technology
Rubescensine A is rubescensin, isodonin again, tetracyclic diterpene class material, and molecular formula C20H28O6, molecular weight 364.43,248 ℃-250 ℃ of fusing points are slightly soluble in water, are dissolved in methyl alcohol, ethyl acetate, acetone etc.
The effect of rubescensine A in cancer therapy caused people's attention, has now found that it all has restraining effect to various kinds of cell strains such as lung cancer, prostate cancer, mammary cancer.
Rabdosia rubescens belongs to perennial herb or undershrub for Labiatae scented tea.The effect that Rabdosia rubescens has is clearing heat and detoxicating, anti-inflammatory analgetic, stomach invigorating are invigorated blood circulation.
Mostly the existing method of openly extracting the purifying rubescensine A is that the extraction separation of rubescensine A mainly contains ether extraction, ethanol reflux extraction and mix reagent extraction method at present.Mostly separation purification method is that silicagel column separates and recrystallization.Be that mixed solvents such as methylene dichloride, propyl alcohol, ethanol extract as patent (application number 02139049.5) " a kind of preparation method of rubescensine A " disclosed method, again with methods such as petroleum ether degreasing, silicagel column separation, recrystallizing methanol.These class methods all adopt silicagel column to separate, and product loss is serious, and complex operation is not suitable for industrialization.
Summary of the invention
The present invention will solve above-mentioned technological deficiency, and a kind of novel method of extracting the purifying rubescensine A is provided.This method can reduce the consumption of toxic reagent, improves product yield, reduces production costs.
In order to solve the problems of the technologies described above, extractive technique scheme of the present invention is as follows: a kind of method for preparing rubescensine A from Rabdosia rubescens is characterized in that comprising following steps:
(1) Rabdosia rubescens raw material pulverizing adds 60-90% methanol solution supersound extraction 2-3 time, and each 20-50 minute, merge and filter, add the ultra-filtration membrane ultrafiltration, see through the liquid vacuum decompression and concentrate, get concentrated solution;
(2) above-mentioned concentrated solution adds in the macropore resin and adsorbs, and volatilizes moisture, and the dress post with methylene dichloride, acetone mixing solutions wash-out, is collected flow point, concentrating under reduced pressure; Concentrated solution with the ethyl acetate solution extraction, is collected extraction liquid again;
(3) above-mentioned extraction liquid concentrates the back and adopts the high speed adverse current chromatogram purifying, and the UV-detector on-line monitoring is collected target component according to collection of illustrative plates, reclaims reagent, and drying under reduced pressure namely.
Described ultra-filtration membrane is the hollow cellulose ultra-filtration membrane of molecular weight cut-off 2000.
The optional AB-8 of described macroporous resin, HZ816, HPD100 and NK-9's is a kind of.
Described methylene dichloride, acetone mixing solutions ratio are 7:5.
The optional sherwood oil of the solvent systems of described high speed adverse current chromatogram, ethyl acetate, methyl alcohol, water, blending ratio 1-3:4-5:2-9:5-7 gets the phase that fixes mutually, does moving phase down mutually.
Adopt present method to extract the high purity rubescensine A, technological operation is simple, and the product yield height is easy to realize industrialization.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
Get 5 kilograms of pulverizing of Rabdosia rubescens raw material, add 6 times of amount 70% methanol solutions, supersound extraction 3 times, each 30 minutes, extracting solution merged the hollow cellulose ultra-filtration membrane ultrafiltration that filters adding molecular weight cut-off 2000, see through the liquid concentrating under reduced pressure, concentrated solution adds in the 1L HZ816 macroporous resin and adsorbs, and volatilizes moisture, the dress post, with methylene dichloride, the acetone mixing solutions wash-out of 6 times of amount blending ratio 7:5, collect wash-out and be evaporated to the medicinal extract shape.Get sherwood oil, ethyl acetate, methyl alcohol, water, 1:4:3:5 mixes in proportion, get the phase that fixes mutually, inject the high speed adverse current chromatogram pipe, drive alternation of hosts's machine, rotating speed 800rpm is set, pumps into down simultaneously and do moving phase mutually, flow velocity 3ml/min is set, after treating system balancing, dissolve medicinal extract with moving phase, injecting chromatograph, collect flow point according to UV-detector, preparation continuously, flow point drying under reduced pressure, get rubescensine A 5.8g, after testing, content 98.6%.
Embodiment 2:
Get 5 kilograms of pulverizing of Rabdosia rubescens raw material, add 7 times of amount 80% methanol solutions, supersound extraction 2 times, each 30 minutes, extracting solution merged the hollow cellulose ultra-filtration membrane ultrafiltration that filters adding molecular weight cut-off 2000, see through the liquid concentrating under reduced pressure, concentrated solution adds in the 1L AB-8 macroporous resin and adsorbs, and volatilizes moisture, the dress post, with methylene dichloride, the acetone mixing solutions wash-out of 5 times of amount blending ratio 7:5, collect wash-out and be evaporated to the medicinal extract shape.Get sherwood oil, ethyl acetate, methyl alcohol, water, 1:5:7:5 mixes in proportion, get the phase that fixes mutually, inject the high speed adverse current chromatogram pipe, drive alternation of hosts's machine, rotating speed 800rpm is set, pumps into down simultaneously and do moving phase mutually, flow velocity 2ml/min is set, after treating system balancing, dissolve medicinal extract with moving phase, injecting chromatograph, collect flow point according to UV-detector, preparation continuously, flow point drying under reduced pressure, get rubescensine A 7.5g, after testing, content 96.8%
Embodiment 3:
Get 5 kilograms of pulverizing of Rabdosia rubescens raw material, add 5 times of amount 9% methanol solutions, supersound extraction 3 times, each 30 minutes, extracting solution merged the hollow cellulose ultra-filtration membrane ultrafiltration that filters adding molecular weight cut-off 2000, see through the liquid concentrating under reduced pressure, concentrated solution adds in the 1L HPD100 macroporous resin and adsorbs, and volatilizes moisture, the dress post, with methylene dichloride, the acetone mixing solutions wash-out of 7 times of amount blending ratio 7:5, collect wash-out and be evaporated to the medicinal extract shape.Get sherwood oil, ethyl acetate, methyl alcohol, water, 2:5:9:7 mixes in proportion, get the phase that fixes mutually, inject the high speed adverse current chromatogram pipe, drive alternation of hosts's machine, rotating speed 800rpm is set, pumps into down simultaneously and do moving phase mutually, flow velocity 1ml/min is set, after treating system balancing, dissolve medicinal extract with moving phase, injecting chromatograph, collect flow point according to UV-detector, preparation continuously, flow point drying under reduced pressure, get rubescensine A 6.3g, after testing, content 98.1%.
Embodiment 4:
Get 5 kilograms of pulverizing of Rabdosia rubescens raw material, add 5 times of amount 75% methanol solutions, supersound extraction 3 times, each 30 minutes, extracting solution merged the hollow cellulose ultra-filtration membrane ultrafiltration that filters adding molecular weight cut-off 2000, see through the liquid concentrating under reduced pressure, concentrated solution adds in the 1L NK-9 macroporous resin and adsorbs, and volatilizes moisture, the dress post, with methylene dichloride, the acetone mixing solutions wash-out of 6 times of amount blending ratio 7:5, collect wash-out and be evaporated to the medicinal extract shape.Get sherwood oil, ethyl acetate, methyl alcohol, water, 1:4:9:5 mixes in proportion, get the phase that fixes mutually, inject the high speed adverse current chromatogram pipe, drive alternation of hosts's machine, rotating speed 800rpm is set, pumps into down simultaneously and do moving phase mutually, flow velocity 2ml/min is set, after treating system balancing, dissolve medicinal extract with moving phase, injecting chromatograph, collect flow point according to UV-detector, preparation continuously, flow point drying under reduced pressure, get rubescensine A 6.3g, after testing, content 99.1%.
Claims (5)
1. method for preparing rubescensine A from Rabdosia rubescens is characterized in that comprising following steps:
(1) Rabdosia rubescens raw material pulverizing adds 60-90% methanol solution supersound extraction 2-3 time, and each 20-50 minute, merge and filter, add the ultra-filtration membrane ultrafiltration, see through the liquid vacuum decompression and concentrate, get concentrated solution;
(2) above-mentioned concentrated solution adds in the macropore resin and adsorbs, and volatilizes moisture, and the dress post with methylene dichloride, acetone mixing solutions wash-out, is collected flow point, concentrating under reduced pressure; Concentrated solution with the ethyl acetate solution extraction, is collected extraction liquid again;
(3) above-mentioned extraction liquid concentrates the back and adopts the high speed adverse current chromatogram purifying, and the UV-detector on-line monitoring is collected target component according to collection of illustrative plates, reclaims reagent, and drying under reduced pressure namely.
2. the method for preparing rubescensine A from Rabdosia rubescens as claimed in claim 1 is characterized in that the ultra-filtration membrane described in the step (1) is the hollow cellulose ultra-filtration membrane of molecular weight cut-off 2000.
3. the method for preparing rubescensine A from Rabdosia rubescens as claimed in claim 1 is characterized in that the optional AB-8 of the described macroporous resin of step (2), HZ816, HPD100 and NK-9's is a kind of.
4. the method for preparing rubescensine A from Rabdosia rubescens as claimed in claim 1 is characterized in that the described methylene dichloride of step (2), acetone mixing solutions ratio are 7:5.
5. the method that from Rabdosia rubescens, prepares rubescensine A as claimed in claim 1, the optional sherwood oil of solvent systems, ethyl acetate, methyl alcohol, the water that it is characterized in that the described high speed adverse current chromatogram of step (3), blending ratio 1-3:4-5:2-9:5-7, get the phase that fixes mutually, do moving phase down mutually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310179293XA CN103232468A (en) | 2013-05-15 | 2013-05-15 | Method for extracting purified oridonin from rabdosia rubescens |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310179293XA CN103232468A (en) | 2013-05-15 | 2013-05-15 | Method for extracting purified oridonin from rabdosia rubescens |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744489A (en) * | 2015-04-19 | 2015-07-01 | 北京化工大学 | Method for preparing high-purity oridonin by taking rabdosia rubescens as raw material |
| CN105732653A (en) * | 2016-02-03 | 2016-07-06 | 河南中医学院 | Method for preparing oridonin from isodon japonica |
| CN110305145A (en) * | 2018-03-27 | 2019-10-08 | 南京工业大学 | A method of removing Oridonin extracts detrimental activity impurity in solution |
-
2013
- 2013-05-15 CN CN201310179293XA patent/CN103232468A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744489A (en) * | 2015-04-19 | 2015-07-01 | 北京化工大学 | Method for preparing high-purity oridonin by taking rabdosia rubescens as raw material |
| CN105732653A (en) * | 2016-02-03 | 2016-07-06 | 河南中医学院 | Method for preparing oridonin from isodon japonica |
| CN105732653B (en) * | 2016-02-03 | 2017-12-15 | 河南中医药大学 | A kind of method that Oridonin is prepared from Isodon Japonica Hara |
| CN110305145A (en) * | 2018-03-27 | 2019-10-08 | 南京工业大学 | A method of removing Oridonin extracts detrimental activity impurity in solution |
| CN110305145B (en) * | 2018-03-27 | 2022-06-24 | 南京工业大学 | Method for concentrating oridonin extracting solution |
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Application publication date: 20130807 |