CN102643289A - Calycopterone purification method - Google Patents
Calycopterone purification method Download PDFInfo
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- CN102643289A CN102643289A CN2012101228139A CN201210122813A CN102643289A CN 102643289 A CN102643289 A CN 102643289A CN 2012101228139 A CN2012101228139 A CN 2012101228139A CN 201210122813 A CN201210122813 A CN 201210122813A CN 102643289 A CN102643289 A CN 102643289A
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- extraction
- extracting
- ketone
- calycopteris
- floribunda
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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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Abstract
The invention discloses a calycopterone purification method, which includes the steps: crushing calycopteris floribunda flowers, adding the crushed calycopteris floribunda flowers into a supercritical extraction kettle, performing supercritical CO2 extraction under the extraction pressure of 25-40MPa and at the temperature of 45-60 DEG C, and analyzing to obtain extract; subjecting the extract to polyamide resin column adsorption, eluting with alcohol water, collecting eluent, concentrating and drying to obtain a crude product; and subjecting the crude product to high-speed counter-current chromatography separation and purification, utilizing normal hexane-acetic ether-methanol-water as a solvent system, performing detection with an ultraviolet detector, collecting fraction, recovering reagent, and drying to obtain the calycopterone. The method for purifying the calycopterone is simple in operation, high in efficiency and product purity and suitable for industrial preparation.
Description
Technical field
The invention belongs to the extractive technique field of crude substance, relate to a kind of extracting and purifying method of Calycopteris floribunda ketone.
Background technology
Calycopteris floribunda ketone (Calycopterone), molecular formula are C
35H
34O
10, molecular weight is 614.65, mp.222-223 ℃.Be present in Combretum Racemosum (Combretaceae) Calycopteris floribunda
Calycopteris floribunda(Roxb.) during Lamk. spends.Calycopteris floribunda ketone has the wide spectrum CDCC.ED to following knurl strain
50(μ g/ml) is respectively: BC-1 (5.4), HT (1.8), LU-1 (1.2), COL-2 (0.4), KB (0.8).KBV-1 (9.6), P388 (0.78), A-431 (1.0), U-373 (0.1); IC to SKOV3, SKVLB, HT-29
50(μ M) is respectively 1.0,1.90 and 0.93.
Summary of the invention
The extracting and purifying method that the purpose of this invention is to provide a kind of Calycopteris floribunda ketone.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of extracting and purifying method of Calycopteris floribunda ketone is characterized in that may further comprise the steps: Calycopteris floribunda pollen is broken, add in the supercritical extraction reactor, and be entrainment agent with methyl alcohol, carry out supercritical CO
2Extraction is resolved, and gets extract, uses dissolve with methanol; It is dry to add polyamide resin, the dress post, and the alcohol solution wash-out is collected elutriant; Concentrate drying gets bullion, and through the high speed adverse current chromatogram separation and purification, normal hexane-ETHYLE ACETATE-methanol-water is a solvent systems with bullion; UV-detector detects, and collects flow point and reclaims reagent, is drying to obtain.
Said supercritical CO
2Extraction temperature is 45-60 ℃, and extracting pressure is 25-40MPa, and resolution temperature is 35-48 ℃, and parsing pressure is 6-8.5MPa, extraction time 40-120min, CO
2Flow is 3-5ml/g crude drug/min.
Said alcohol solution is the aqueous ethanolic solution of 20-80%.
Said high speed adverse current chromatogram separation and purification, the volume ratio of solvent systems normal hexane-ETHYLE ACETATE-methanol-water are (2-4): (1-2.5): (1-2.5): (2-4).
The invention has the beneficial effects as follows: (1) supercritical fluid extraction, efficient is high, and extraction yield is high; (2) adopt the high speed adverse current chromatogram separation and purification, the product-free loss, separation is efficient, preparation amount is big, separation system is reusable, and environmental pollution is little.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment
Embodiment 1:
With broken mistake 20 mesh sieves of Calycopteris floribunda pollen, get 10kg and add in the supercritical extraction reactor, be entrainment agent with methyl alcohol, setting extraction temperature is 60 ℃, and extracting pressure is 35MPa, and resolution temperature is 42 ℃, and parsing pressure is 7.5MPa, extraction time, CO
2Flow is 4ml/g crude drug/min, and extraction 80min resolves, and gets extract; Use dissolve with methanol, add polyamide resin and mix appearance, drying, dress post; With 4BV 20% ethanol elution impurity, use the 75% ethanol elution effective constituent of 6BV more earlier, collect effective constituent concentrating under reduced pressure, the dry bullion that gets.Get the 4:2.5:2.5:4 mixing by volume of normal hexane, ETHYLE ACETATE, methyl alcohol, water, after the layering, get the phase that fixes mutually; Be moving phase mutually down, the adjustment rotating speed is 850rpm, pumps into down back control flow velocity 2ml/min mutually; Take off the phased soln bullion,, collect Calycopteris floribunda ketone flow point by the sampling valve sample introduction; Reclaim reagent, be drying to obtain Calycopteris floribunda ketone product, content is 96.7%.
Embodiment 2:
With broken mistake 20 mesh sieves of Calycopteris floribunda pollen, get 10kg and add in the supercritical extraction reactor, be entrainment agent with methyl alcohol, setting extraction temperature is 50 ℃, and extracting pressure is 30MPa, and resolution temperature is 40 ℃, and parsing pressure is 6.5MPa, CO
2Flow is 3.5ml/g crude drug/min, and extraction 100min resolves, and gets extract; Use dissolve with methanol, add polyamide resin and mix appearance, drying, dress post; With 3BV30% ethanol elution impurity, use the 75% ethanol elution effective constituent of 5BV more earlier, collect effective constituent concentrating under reduced pressure, the dry bullion that gets.Get the 3:2:2:4 mixing by volume of normal hexane, ETHYLE ACETATE, methyl alcohol, water, after the layering, get the phase that fixes mutually; Be moving phase mutually down, the adjustment rotating speed is 900rpm, pumps into down back control flow velocity 2ml/min mutually; Take off the phased soln bullion,, collect Calycopteris floribunda ketone flow point by the sampling valve sample introduction; Reclaim reagent, be drying to obtain Calycopteris floribunda ketone product, content is 96.2%.
Embodiment 3:
With broken mistake 20 mesh sieves of Calycopteris floribunda pollen, get 10kg and add in the supercritical extraction reactor, be entrainment agent with methyl alcohol, setting extraction temperature is 45 ℃, and extracting pressure is 40MPa, and resolution temperature is 48 ℃, and parsing pressure is 6MPa, CO
2Flow is 3ml/g crude drug/min, and extraction 120min resolves, and gets extract; Use dissolve with methanol, add polyamide resin and mix appearance, drying, dress post; With 4BV35% ethanol elution impurity, use the 80% ethanol elution effective constituent of 5BV more earlier, collect effective constituent concentrating under reduced pressure, the dry bullion that gets.Get the 2:1:1:3 mixing by volume of normal hexane, ETHYLE ACETATE, methyl alcohol, water, after the layering, get the phase that fixes mutually; Be moving phase mutually down, the adjustment rotating speed is 750rpm, pumps into down back control flow velocity 3ml/min mutually; Take off the phased soln bullion,, collect Calycopteris floribunda ketone flow point by the sampling valve sample introduction; Reclaim reagent, be drying to obtain Calycopteris floribunda ketone product, content is 97.6%.
Embodiment 4:
With broken mistake 20 mesh sieves of Calycopteris floribunda pollen, get 10kg and add in the supercritical extraction reactor, be entrainment agent with methyl alcohol, setting extraction temperature is 60 ℃, and extracting pressure is 40MPa, and resolution temperature is 35 ℃, and parsing pressure is 8.5MPa, CO
2Flow is 5ml/g crude drug/min, and extraction 40min resolves, and gets extract; Use dissolve with methanol, add polyamide resin and mix appearance, drying, dress post; With 3BV30% ethanol elution impurity, use the 80% ethanol elution effective constituent of 4BV more earlier, collect effective constituent concentrating under reduced pressure, the dry bullion that gets.Get the 3:1.5:1.5:2 mixing by volume of normal hexane, ETHYLE ACETATE, methyl alcohol, water, after the layering, get the phase that fixes mutually; Be moving phase mutually down, the adjustment rotating speed is 800rpm, pumps into down back control flow velocity 2.5ml/min mutually; Take off the phased soln bullion,, collect Calycopteris floribunda ketone flow point by the sampling valve sample introduction; Reclaim reagent, be drying to obtain Calycopteris floribunda ketone product, content is 96.8%.
Claims (4)
1. the extracting and purifying method of a Calycopteris floribunda ketone is characterized in that may further comprise the steps: Calycopteris floribunda pollen is broken, add in the supercritical extraction reactor, and be entrainment agent with methyl alcohol, carry out supercritical CO
2Extraction is resolved, and gets extract, uses dissolve with methanol; It is dry to add polyamide resin, the dress post, and the alcohol solution wash-out is collected elutriant; Concentrate drying gets bullion, and through the high speed adverse current chromatogram separation and purification, normal hexane-ETHYLE ACETATE-methanol-water is a solvent systems with bullion; UV-detector detects, and collects flow point and reclaims reagent, is drying to obtain.
2. the extracting and purifying method of a kind of Calycopteris floribunda ketone as claimed in claim 1 is characterized in that said supercritical CO
2Extraction temperature is 45-60 ℃, and extracting pressure is 25-40MPa, and resolution temperature is 35-48 ℃, and parsing pressure is 6-8.5MPa, extraction time 40-120min, CO
2Flow is 3-5ml/g crude drug/min.
3. the extracting and purifying method of a kind of Calycopteris floribunda ketone as claimed in claim 1 is characterized in that said alcohol solution is the aqueous ethanolic solution of 20-80%.
4. the extracting and purifying method of a kind of Calycopteris floribunda ketone as claimed in claim 1; It is characterized in that said high speed adverse current chromatogram separation and purification, the volume ratio of solvent systems normal hexane-ETHYLE ACETATE-methanol-water is (2-4): (1-2.5): (1-2.5): (2-4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101228139A CN102643289A (en) | 2012-04-25 | 2012-04-25 | Calycopterone purification method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101228139A CN102643289A (en) | 2012-04-25 | 2012-04-25 | Calycopterone purification method |
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|---|---|
| CN102643289A true CN102643289A (en) | 2012-08-22 |
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| CN2012101228139A Pending CN102643289A (en) | 2012-04-25 | 2012-04-25 | Calycopterone purification method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110903297A (en) * | 2019-12-20 | 2020-03-24 | 海南省林业科学研究所 | Macroporous resin extraction method of rotenone and analogue |
-
2012
- 2012-04-25 CN CN2012101228139A patent/CN102643289A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110903297A (en) * | 2019-12-20 | 2020-03-24 | 海南省林业科学研究所 | Macroporous resin extraction method of rotenone and analogue |
| CN110903297B (en) * | 2019-12-20 | 2020-10-13 | 海南省林业科学研究所 | Macroporous resin extraction method of rotenone and analogue |
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Application publication date: 20120822 |