CN102295670A - Method for extracting buddlenoid A from buddleia - Google Patents
Method for extracting buddlenoid A from buddleia Download PDFInfo
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- CN102295670A CN102295670A CN2011103038986A CN201110303898A CN102295670A CN 102295670 A CN102295670 A CN 102295670A CN 2011103038986 A CN2011103038986 A CN 2011103038986A CN 201110303898 A CN201110303898 A CN 201110303898A CN 102295670 A CN102295670 A CN 102295670A
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- glucoside
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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
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Saccharide Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting buddlenoid A from buddleia. The method comprises the following steps of: crushing the buddleia to be 40-mesh to 80-mesh; adding in a supercritical extraction kettle; performing supercritical CO2 gradient extraction under the environment of extraction pressure of 15-30MPa and temperature of 40-50 DEG C; analyzing an extract; collecting an effective extract recovery reagent; dissolving obtained extractum in hot water; adding polyamide resin for adsorption; performing gradient elution with ethanol aqueous solution; collecting active ingredients to concentrate under reduced pressure; crystallizing concentrated solution; filtering crystal out; dissolving with ethanol; recrystallizing; and drying to obtain the buddlenoid A. The method adopted by the invention has the advantages of high extraction efficiency, low energy consumption, low pollution and simple process steps and is suitable for industrial production.
Description
Technical field
The invention belongs to biological technical field, particularly relate to a kind of method of from Lindley Butterflybush Herb, extracting buddleo-glucoside A.
Background technology
The principle of supercritical carbon dioxide extraction (SFE) sepn process is to utilize the dissolving power of supercutical fluid and the relation of its density, promptly utilizes pressure and temperature that the influence of supercutical fluid dissolving power is carried out.Under supercritical state, supercutical fluid is contacted with material to be separated, it is extracted the composition of polarity size, boiling point height and molecular weight size selectively successively.Because supercritical carbon dioxide extraction has efficient, free of contamination characteristics, is used widely in natural product production.
Buddleo-glucoside A(Buddlenoid A) be flavonoid glycoside, CAS:142750-32-1, molecular formula: C30H26O13, molecular structural formula:
The plain A of Lindley Butterflybush Herb has the effect of restraint of tyrosinase, thereby has suppressed melanic formation.Therefore be widely used in the skin-lightening cosmetic.
Lindley Butterflybush Herb is the herb of loganiaceae plant Lindley Butterflybush Herb, and traditional medicine is thought that it has and dispeled the wind desinsection, the effect of invigorating blood circulation.Modern study is found, not only dispels the wind in the Lindley Butterflybush Herb, and desinsection, the isoreactivity composition of invigorating blood circulation also has whitening composition buddleo-glucoside A.
By literature search, the method for extracting the plain A of Lindley Butterflybush Herb from Lindley Butterflybush Herb discloses less, and especially the industrial method public affairs are still unexposed.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of efficient industrial method that extracts buddleo-glucoside A from Lindley Butterflybush Herb.
The objective of the invention is to be achieved through the following technical solutions: a kind of method of from Lindley Butterflybush Herb, extracting the plain A of Lindley Butterflybush Herb, it is characterized in that: get Lindley Butterflybush Herb and pulverize the 40-80 order, add in the supercritical extraction reactor, at extracting pressure 15-30MPa, under temperature 40-50 ℃ the environment, the extraction of supercritical CO 2 gradient, resolve extract, collect effective extract and reclaim reagent, gained medicinal extract hot water dissolving adds polyamide resin absorption, the aqueous ethanolic solution gradient elution, collect the effective constituent concentrating under reduced pressure, the concentrated solution crystallization leaches crystallisate dissolve with ethanol recrystallization, is drying to obtain buddleo-glucoside A.
Described gradient extraction is: feed liquid CO 2 extraction 1-3 hour earlier, behind the parsing extract, feed liquid CO 2 and entrainment agent extraction 1-3 hour again, the methyl alcohol of the optional 50-90% of entrainment agent, ethanol or acetone.
Described analysis condition: resolve pressure 5-10MPa, temperature 45-60 ℃.
Described aqueous ethanolic solution gradient elution is: use the ethanolic soln wash-out impurity of the 10-40% of 4-6BV earlier, use the ethanolic soln wash-out effective constituent of the 40-90% of 3-5BV again.
Advantage of the present invention is that method has adopted the extraction of supercritical CO 2 gradient, the extraction efficiency height, and energy consumption is low, and is pollution-free, and gained crude extract content height be easy to purifying, and whole process flow is simple to operate, is easy to suitability for industrialized production.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1:
Lindley Butterflybush Herb raw material pulverizing 60 orders, get 5kg and add in the supercritical extraction reactor, feed liquid CO 2, be arranged on extracting pressure 15MPa, 40 ℃ of temperature, after reaching above-mentioned parameter, adjusting the liquid CO 2 flow velocity is 20kg/h, and dynamic extraction 2 hours is at pressure 6MPa, temperature is transferred part to resolve extract down for 60 ℃ and is discarded, re-adjustment pressure 25MPa feeds entrainment agent 60% methanol solution, flow velocity 3L/h simultaneously, extracted two hours, resolve extract, reclaim reagent, gained medicinal extract hot water dissolving, add to be equipped with in the 300g polyamide resin and adsorb, get 40% the ethanolic soln wash-out impurity of 4BV earlier, use 90% the ethanolic soln wash-out target component of 3BV again, collect the target component concentrating under reduced pressure, the concentrated solution crystallization, leach the hot dehydrated alcohol recrystallization of crystallisate, the dry buddleo-glucoside A7.2g that gets, purity is 83.7% after testing.
Embodiment 2:
Lindley Butterflybush Herb raw material pulverizing 80 orders, get 5kg and add in the supercritical extraction reactor, feed liquid CO 2, be arranged on extracting pressure 30MPa, 50 ℃ of temperature, after reaching above-mentioned parameter, adjusting the liquid CO 2 flow velocity is 25kg/h, and dynamic extraction 2 hours is at pressure 8MPa, temperature is transferred part to resolve extract down for 50 ℃ and is discarded, re-adjustment pressure 25MPa feeds entrainment agent 70% acetone soln, flow velocity 2L/h simultaneously, extracted two hours, resolve extract, reclaim reagent, gained medicinal extract hot water dissolving, add to be equipped with in the 200g polyamide resin and adsorb, get 40% the ethanolic soln wash-out impurity of 4BV earlier, use 50% the ethanolic soln wash-out target component of 3BV again, collect the target component concentrating under reduced pressure, the concentrated solution crystallization, leach crystallisate heat 70% ethyl alcohol recrystallization, the dry buddleo-glucoside A5.2g that gets, purity is 89.4% after testing.
Claims (4)
1. method of from Lindley Butterflybush Herb, extracting buddleo-glucoside A, it is characterized in that: get Lindley Butterflybush Herb and pulverize the 40-80 order, add in the supercritical extraction reactor, under extracting pressure 15-30MPa, temperature 40-50 ℃ environment, the extraction of supercritical CO 2 gradient, resolve extract, collect effective extract and reclaim reagent, gained medicinal extract hot water dissolving adds polyamide resin absorption, the aqueous ethanolic solution gradient elution, collect the effective constituent concentrating under reduced pressure, the concentrated solution crystallization leaches crystallisate dissolve with ethanol recrystallization, is drying to obtain buddleo-glucoside A.
2. the method for from Lindley Butterflybush Herb, extracting buddleo-glucoside A according to claim 1, it is characterized in that described gradient extraction is: feed liquid CO 2 extraction 1-3 hour earlier, after resolving extract, feed liquid CO 2 and entrainment agent extraction 1-3 hour again, the methyl alcohol of the optional 50-90% of entrainment agent, ethanol or acetone.
3. the method for extracting buddleo-glucoside A from Lindley Butterflybush Herb according to claim 1 is characterized in that described analysis condition: resolve pressure 5-10MPa, temperature 45-60 ℃.
4. the method for from Lindley Butterflybush Herb, extracting buddleo-glucoside A according to claim 1, it is characterized in that described aqueous ethanolic solution gradient elution is: use the ethanolic soln wash-out impurity of the 10-40% of 4-6BV earlier, use the ethanolic soln wash-out effective constituent of the 40-90% of 3-5BV again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103038986A CN102295670A (en) | 2011-10-10 | 2011-10-10 | Method for extracting buddlenoid A from buddleia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103038986A CN102295670A (en) | 2011-10-10 | 2011-10-10 | Method for extracting buddlenoid A from buddleia |
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| CN102295670A true CN102295670A (en) | 2011-12-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011103038986A Pending CN102295670A (en) | 2011-10-10 | 2011-10-10 | Method for extracting buddlenoid A from buddleia |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108991024A (en) * | 2018-07-21 | 2018-12-14 | 安溪县凤城建金产品外观设计服务中心 | A kind of technique that effective component in Lindley Butterflybush Herb is enriched with by solvent extraction method |
| CN109498521A (en) * | 2018-12-23 | 2019-03-22 | 广州素颜皮肤管理科技有限公司 | It is a kind of to have effects that the plant extracts of antiallergy and its application |
-
2011
- 2011-10-10 CN CN2011103038986A patent/CN102295670A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108991024A (en) * | 2018-07-21 | 2018-12-14 | 安溪县凤城建金产品外观设计服务中心 | A kind of technique that effective component in Lindley Butterflybush Herb is enriched with by solvent extraction method |
| CN109498521A (en) * | 2018-12-23 | 2019-03-22 | 广州素颜皮肤管理科技有限公司 | It is a kind of to have effects that the plant extracts of antiallergy and its application |
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Application publication date: 20111228 |