CN102863496A - Extraction method of Zhankuic acid A - Google Patents
Extraction method of Zhankuic acid A Download PDFInfo
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- CN102863496A CN102863496A CN2012103666621A CN201210366662A CN102863496A CN 102863496 A CN102863496 A CN 102863496A CN 2012103666621 A CN2012103666621 A CN 2012103666621A CN 201210366662 A CN201210366662 A CN 201210366662A CN 102863496 A CN102863496 A CN 102863496A
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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
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Abstract
The invention discloses an extraction method of Zhankuic acid A, belonging to the field of natural drug chemistry. The method comprises the following steps: adding the raw material Antrndia cinnamomea Chang & Chou,sp.nov. sporophore into a flash extractor, carrying out flash extraction by using a 95% ethanol solution as an extraction solvent, filtering to obtain an extracting solution, concentrating, extracting the concentrated solution through a double-water-phase solvent system, collecting the organic phase, concentrating, separating by high-speed counter-current chromatography, and concentrating the fraction under reduced pressure by using chloroform-methanol-water as a solvent system, thereby obtaining the Zhankuic acid A. By adopting the techniques of flash extraction, double-water-phase solvent system extraction and high-speed counter-current chromatography separation, the invention has the advantages of high efficiency and environmental protection, and is suitable for industrial large-scale production.
Description
Technical field
The invention belongs to the extractive technique field of crude substance, relate to a kind of extracting method of opening up storehouse acid A.
Background technology
Exhibition storehouse acid A(Zhankuic acid A), molecular formula is C
29H
40O
5, molecular weight is 468.63, is from the beautiful osmanthus of polyporaceae (Polyporaceae) Antrodia
Antrndia cinnamomeaChang ﹠amp; Chou separates a kind of activeconstituents that obtains in the sp.nov. sporophore.Research is found, opens up storehouse acid A _ Lymphoid Leukemic Cells P388 is cytotoxic activity, and IC50 is 1.8 μ g/ml.
By literature search, the domestic industrial extraction method relevant report of not yet finding exhibition storehouse acid A.
Summary of the invention
The extracting method that the purpose of this invention is to provide a kind of exhibition storehouse acid A of efficient, environmental protection.
For achieving the above object, the present invention is by the following technical solutions:
(1) take beautiful osmanthus Antrodia sporophore as raw material, be dried to constant weight in 65 ℃, pulverize, add in the flash extracter, take 95% ethanolic soln as extracting solvent, carry out the sudden strain of a muscle formula and extract, filter and obtain extracting solution;
(2) extracting solution obtains crude extract after concentrating, and extracts with the double water-phase solvent systems, collects organic extractant phase liquid, and decompression and solvent recovery gets concentrated solution;
(3) concentrated solution is used the high speed adverse current chromatogram separation and purification, with chloroform-methanol-water two-phase solvent system, upper is stationary phase mutually, and lower is moving phase mutually, collects composition according to collection of illustrative plates, and cryoconcentration is drying to obtain exhibition storehouse acid A.
Sudden strain of a muscle formula extraction voltage is 140-160V in the described step (1), and extraction time is 90s-120s.
The double water-phase solvent systems is the ethanol/ammonium sulfate double-aqueous phase system in the described step (2), takes by weighing 22g ammonium sulfate and adds in the 65ml water, and dissolving finishes to add the 32ml dehydrated alcohol.
Chloroform-methanol-water volume ratio is (12-14) in the described step (3): (8-10): (5-8).
The invention has the beneficial effects as follows: (1) the present invention adopts sudden strain of a muscle formula extraction method, rapidly and efficiently, low power consuming, environmental protection; (2) the used ethanol/ammonium sulfate double-aqueous phase system of the present invention can reclaim, reuse, and has saved reagent, has reduced cost; (3) the present invention utilizes high speed adverse current chromatogram to separate exhibition storehouse acid A, the loss of sepn process product-free, and efficient, preparation cycle is short.
Embodiment:
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 1:
Get beautiful osmanthus Antrodia sporophore 100g, be dried to constant weight in 65 ℃, pulverize, add in the flash extracter, take 95% ethanolic soln as extracting solvent, extraction voltage is 150V, and extraction time is 100s, carry out the sudden strain of a muscle formula and extract, filter and obtain extracting solution, obtain crude extract after extracting solution is concentrated; Take by weighing 22g ammonium sulfate and add in the 65ml water, dissolving finishes to add the 32ml dehydrated alcohol, sets up the ethanol/ammonium sulfate double-aqueous phase system, crude extract is added in the 3L ethanol/ammonium sulfate double-aqueous phase system, and vibration shakes up, and leaves standstill, phase in the collection, decompression and solvent recovery gets concentrated solution; Get chloroform, methyl alcohol, water in the mixing of 13:8:7 ratio, standing demix is got and is pumped into mutually chromatotube, open high-speed counter-current chromatograph, the adjustment rotating speed is 900rpm, pumps into the 2.5ml/min flow velocity lower simultaneously, injects concentrated solution, the UV-detector monitoring, the monitoring wavelength is 266nm, collects flow point, behind the concentrating under reduced pressure, be drying to obtain exhibition storehouse acid A, content 96.4%.
Embodiment 2:
Get beautiful osmanthus Antrodia sporophore 100g, be dried to constant weight in 65 ℃, pulverize, add in the flash extracter, take 95% ethanolic soln as extracting solvent, extraction voltage is 160V, and extraction time is 120s, carry out the sudden strain of a muscle formula and extract, filter and obtain extracting solution, obtain crude extract after extracting solution is concentrated; Take by weighing 22g ammonium sulfate and add in the 65ml water, dissolving finishes to add the 32ml dehydrated alcohol, sets up the ethanol/ammonium sulfate double-aqueous phase system, crude extract is added in the 2.5L ethanol/ammonium sulfate double-aqueous phase system, and vibration shakes up, and leaves standstill, phase in the collection, decompression and solvent recovery gets concentrated solution; Get chloroform, methyl alcohol, water in the mixing of 14:9:8 ratio, standing demix is got and is pumped into mutually chromatotube, open high-speed counter-current chromatograph, the adjustment rotating speed is 850rpm, pumps into the 3ml/min flow velocity lower simultaneously, injects concentrated solution, the UV-detector monitoring, the monitoring wavelength is 266nm, collects flow point, behind the concentrating under reduced pressure, be drying to obtain exhibition storehouse acid A, content 94.6%.
Embodiment 3:
Get beautiful osmanthus Antrodia sporophore 100g, be dried to constant weight in 65 ℃, pulverize, add in the flash extracter, take 95% ethanolic soln as extracting solvent, extraction voltage is 160V, and extraction time is 90s, carry out the sudden strain of a muscle formula and extract, filter and obtain extracting solution, obtain crude extract after extracting solution is concentrated; Take by weighing 22g ammonium sulfate and add in the 65ml water, dissolving finishes to add the 32ml dehydrated alcohol, sets up the ethanol/ammonium sulfate double-aqueous phase system, crude extract is added in the 3L ethanol/ammonium sulfate double-aqueous phase system, and vibration shakes up, and leaves standstill, phase in the collection, decompression and solvent recovery gets concentrated solution; Get chloroform, methyl alcohol, water in the mixing of 12:10:5 ratio, standing demix is got and is pumped into mutually chromatotube, open high-speed counter-current chromatograph, the adjustment rotating speed is 800rpm, pumps into the 3ml/min flow velocity lower simultaneously, injects concentrated solution, the UV-detector monitoring, the monitoring wavelength is 266nm, collects flow point, behind the concentrating under reduced pressure, be drying to obtain exhibition storehouse acid A, content 94.9%.
Embodiment 4:
Get beautiful osmanthus Antrodia sporophore 100g, be dried to constant weight in 65 ℃, pulverize, add in the flash extracter, take 95% ethanolic soln as extracting solvent, extraction voltage is 140V, and extraction time is 120s, carry out the sudden strain of a muscle formula and extract, filter and obtain extracting solution, obtain crude extract after extracting solution is concentrated; Take by weighing 22g ammonium sulfate and add in the 65ml water, dissolving finishes to add the 32ml dehydrated alcohol, sets up the ethanol/ammonium sulfate double-aqueous phase system, crude extract is added in the 2L ethanol/ammonium sulfate double-aqueous phase system, and vibration shakes up, and leaves standstill, phase in the collection, decompression and solvent recovery gets concentrated solution; Get chloroform, methyl alcohol, water in the mixing of 13:10:5 ratio, standing demix is got and is pumped into mutually chromatotube, open high-speed counter-current chromatograph, the adjustment rotating speed is 850rpm, pumps into the 3ml/min flow velocity lower simultaneously, injects concentrated solution, the UV-detector monitoring, the monitoring wavelength is 266nm, collects flow point, behind the concentrating under reduced pressure, be drying to obtain exhibition storehouse acid A, content 95.5%.
Claims (4)
1. extracting method of opening up storehouse acid A is characterized in that may further comprise the steps:
(1) take beautiful osmanthus Antrodia sporophore as raw material, be dried to constant weight in 65 ℃, pulverize, add in the flash extracter, take 95% ethanolic soln as extracting solvent, carry out the sudden strain of a muscle formula and extract, filter and obtain extracting solution;
(2) extracting solution obtains crude extract after concentrating, and extracts with the double water-phase solvent systems, collects organic extractant phase liquid, and decompression and solvent recovery gets concentrated solution;
(3) concentrated solution is used the high speed adverse current chromatogram separation and purification, with chloroform-methanol-water two-phase solvent system, upper is stationary phase mutually, and lower is moving phase mutually, collects composition according to collection of illustrative plates, and cryoconcentration is drying to obtain exhibition storehouse acid A.
2. a kind of extracting method of opening up storehouse acid A as claimed in claim 1 is characterized in that sudden strain of a muscle formula extraction voltage is 140-160V in the described step (1), and extraction time is 90s-120s.
3. a kind of extracting method of opening up storehouse acid A as claimed in claim 1 is characterized in that the double water-phase solvent systems is the ethanol/ammonium sulfate double-aqueous phase system in the described step (2), takes by weighing 22g ammonium sulfate and adds in the 65ml water, and dissolving finishes to add the 32ml dehydrated alcohol.
4. a kind of extracting method of opening up storehouse acid A as claimed in claim 1 is characterized in that chloroform-methanol-water volume ratio is (12-14) in the described step (3): (8-10): (5-8).
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012103666621A CN102863496A (en) | 2012-09-28 | 2012-09-28 | Extraction method of Zhankuic acid A |
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| CN2012103666621A CN102863496A (en) | 2012-09-28 | 2012-09-28 | Extraction method of Zhankuic acid A |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008647A (en) * | 2016-07-05 | 2016-10-12 | 汕头大学 | Novel extraction method of momordica saponins |
| TWI598332B (en) * | 2016-05-05 | 2017-09-11 | 葡萄王生技股份有限公司 | Preparation method for isolating antrodin c by high performance centrifugal partition chromatography (hpcpc) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201029658A (en) * | 2009-02-13 | 2010-08-16 | Univ Kaohsiung Medical | Ethanol extract of antrodia camphorata for inducing apoptosis and preparation method thereof |
| CN102614195A (en) * | 2011-01-26 | 2012-08-01 | 高雄医学大学 | Triterpenoid composition of antrodia cinnamomea fruiting body, preparation and analysis method |
-
2012
- 2012-09-28 CN CN2012103666621A patent/CN102863496A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201029658A (en) * | 2009-02-13 | 2010-08-16 | Univ Kaohsiung Medical | Ethanol extract of antrodia camphorata for inducing apoptosis and preparation method thereof |
| CN102614195A (en) * | 2011-01-26 | 2012-08-01 | 高雄医学大学 | Triterpenoid composition of antrodia cinnamomea fruiting body, preparation and analysis method |
Non-Patent Citations (2)
| Title |
|---|
| I-HWA ET AL: "THREE NEW TRITERPENOIDS FROM ANTRODIA CINNAMOMEA", 《JOURNAL OF NATURAL PRODUCTS》, vol. 58, no. 3, 31 March 1995 (1995-03-31), pages 367 - 368, XP008138391 * |
| 罗建平等: "乙醇/硫酸铵双水相体系分离灵芝酸的研究", 《食用菌》, no. 20112, 31 December 2011 (2011-12-31) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI598332B (en) * | 2016-05-05 | 2017-09-11 | 葡萄王生技股份有限公司 | Preparation method for isolating antrodin c by high performance centrifugal partition chromatography (hpcpc) |
| CN106008647A (en) * | 2016-07-05 | 2016-10-12 | 汕头大学 | Novel extraction method of momordica saponins |
| CN106008647B (en) * | 2016-07-05 | 2018-05-08 | 汕头大学 | A kind of extracting method of Momordica charantial |
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Application publication date: 20130109 |