CN102320959A - The preparation method of a kind of chrysanthemumic acid B that goes to the field - Google Patents
The preparation method of a kind of chrysanthemumic acid B that goes to the field Download PDFInfo
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- CN102320959A CN102320959A CN201110263991A CN201110263991A CN102320959A CN 102320959 A CN102320959 A CN 102320959A CN 201110263991 A CN201110263991 A CN 201110263991A CN 201110263991 A CN201110263991 A CN 201110263991A CN 102320959 A CN102320959 A CN 102320959A
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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 the preparation method of a kind of chrysanthemumic acid B that goes to the field, it is characterized in that comprising steps such as supercritical extraction, polyamide column chromatography, alumina column chromatography and recrystallization.The inventive method mild condition has avoided traditional method localized hyperthermia to the active disadvantageous effect of product, and technology is reasonable, can realize rapid extraction, separation, purifying, is a kind of method that is suitable for large-scale production.
Description
Technical field
The invention belongs to natural medicine field, be specifically related to the preparation method of a kind of chrysanthemumic acid B that goes to the field.
Background technology
Common Adenostema Herb is a composite family Common Adenostema Herb platymiscium Common Adenostema Herb
Adenostemma lavenia(L.) herb of O.Ktze; Be annual herb, have another name called Radix Alangii (Simao, Yunnan), water pepper, Herba Adenostemmatis, sweat Soviet Union fiber crops etc., main product is on the south the Yangtze valley and coastal and southwestern various places; Has clearing away heat-damp and promoting diuresis; The effect of removing toxic substances and promoting subsidence of swelling, carbuncle scabies ulcer, venom etc. are controlled in the treatment of be used to catch a cold high heat, bronchitis, pharyngolaryngitis, tonsillitis, icterohepatitis outward.The chemical ingredients of Common Adenostema Herb mainly contains volatile oil and diterpene-kind compound.The chrysanthemumic acid B that wherein goes to the field separates a kind of diterpene compound that obtains, molecular weight 348.44, molecular formula C from Common Adenostema Herb
20H
28O
5, be colourless needle (chloroform-methanol), mp.273-274 ℃.Pharmacological research shows that the chrysanthemumic acid B that goes to the field has cytotoxic activity, is CDCC to the L-5178Y cell toxicant.
In the prior art, Shang Weiyou is applicable to the go to the field technology report of chrysanthemumic acid B of a large amount of preparations.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of chrysanthemumic acid B that goes to the field, adopt supercritical CO
2Steps such as extraction, polyamide column chromatography, alumina column chromatography and recrystallization separate obtaining crying the highly purified chrysanthemumic acid B that goes to the field from Common Adenostema Herb, the chrysanthemumic acid B purity height of going to the field that this method is extracted, be produced on a large scale.
The present invention realizes through following technical scheme:
The preparation method of a kind of chrysanthemumic acid B that goes to the field is characterized in that may further comprise the steps:
1) supercritical extraction: get the Common Adenostema Herb pulverizing medicinal materials, put into supercritical CO
2In the extraction kettle, add an amount of organic solvent again, feed CO as entrainment agent
2,, extract CO under the extraction temperature 30-50 ℃ of condition at extracting pressure 20-35MPa
2Flow velocity is 10-30L/h, extracts 1-3h, collects extract;
2) polyamide column chromatography: extract is added in the polyamide resin column, control flow velocity 0.5-1.5BV/h, first water is eluted to colourless, uses the 30-90% ethanol gradient elution again, collects elutriant, is concentrated into specific density 1.08-1.12, the chrysanthemumic acid B crude extract of must going to the field;
3) alumina column chromatography: the acidic alumina absorption that the chrysanthemumic acid B crude extract of will going to the field is doubly measured with 3-4, oven drying at low temperature below 50 ℃, dry column-packing; Use the mixed solvent gradient elution, collect and to contain the go to the field flow point of chrysanthemumic acid B of high-content, be evaporated to small volume; Crystallization gets coarse-grain;
4) recrystallization: coarse-grain with ETHYLE ACETATE-acetone mixing solutions recrystallization, is obtained the highly purified chrysanthemumic acid B monomeric compound of going to the field.
The said entrainment agent of step (1) is ethanol or the acetone soln of 60-90%, and add-on is the 5-15% that is equivalent to raw material weight.
The described mixed solvent of step (3) is sherwood oil, ETHYLE ACETATE, methyl alcohol, acetone, alcoholic acid mixing solutions.
Characteristics of the present invention are: the inventive method adopts supercritical fluid extraction; Mild condition has avoided traditional method localized hyperthermia to the active disadvantageous effect of product, and technology is reasonable; Can realize rapid extraction, separation, purifying, be a kind of method that is suitable for large-scale production.
Embodiment
To combine specific embodiment that the present invention is described further below, the following example is intended to describe for example the present invention, rather than limits the present invention by any way.
Embodiment 1:
With the Common Adenostema Herb pulverizing medicinal materials, get 5kg and drop in the supercritical extraction jar, add volume percent and be 80% ethanolic soln as entrainment agent, add-on is 0.3kg (raw material weight 6%), at extracting pressure 25MPa, 45 ℃ of extraction temperature, CO
2Extract 2h under the flow 18L/h condition, get the Common Adenostema Herb extract, extract disperses with hot water, last polyamide resin column; Flow velocity 1.0BV/h, it is colourless that first water is washed till water lotion, uses 30% ethanol elution again, uses 80% ethanol elution at last; Collect 80% ethanol eluate, it is 1.08 that elutriant is evaporated to specific density, and the chrysanthemumic acid B crude extract that obtains going to the field is with the acidic alumina absorption of chrysanthemumic acid B crude extract with 3 times of amounts of going to the field; In 50 ℃ of oven drying at low temperatures, the dry method upper prop, with sherwood oil, petroleum ether-ethyl acetate, the ethanol gradient elution of different ratios, the thin-layer chromatography inspection; Collect the high-content chrysanthemumic acid B flow point of going to the field, be evaporated to small volume, crystallization; Coarse-grain with ETHYLE ACETATE-acetone recrystallization, is obtained the 548mg chrysanthemumic acid B monomeric compound of going to the field, and its content is 98.7%.
Embodiment 2:
With the Common Adenostema Herb pulverizing medicinal materials, get 5kg and drop in the supercritical extraction jar, add volume percent and be 70% ethanolic soln as entrainment agent, add-on is 0.6kg (raw material weight 12%), at extracting pressure 20MPa, 35 ℃ of extraction temperature, CO
2Extract 1h under the flow 20L/h condition, get the Common Adenostema Herb extract, extract disperses with hot water, last polyamide resin column; Flow velocity 1.5BV/h, it is colourless that first water is washed till water lotion, uses 30% ethanol elution again, uses 90% ethanol elution at last; Collect 90% ethanol eluate, it is 1.10 that elutriant is evaporated to specific density, and the chrysanthemumic acid B crude extract that obtains going to the field is with the acidic alumina absorption of chrysanthemumic acid B crude extract with 4 times of amounts of going to the field; In 45 ℃ of oven drying at low temperatures, the dry method upper prop, with sherwood oil, the ETHYLE ACETATE-acetone soln gradient elution of different ratios, the thin-layer chromatography inspection; Collect the high-content chrysanthemumic acid B flow point of going to the field, be evaporated to small volume, crystallization; Coarse-grain with ETHYLE ACETATE-acetone recrystallization, is obtained the 526mg chrysanthemumic acid B monomeric compound of going to the field, and its content is 99.2%.
Embodiment 3:
With the Common Adenostema Herb pulverizing medicinal materials, get 5kg and drop in the supercritical extraction jar, add volume percent and be 90% acetone soln as entrainment agent, add-on is 0.75kg (raw material weight 15%), at extracting pressure 32MPa, 30 ℃ of extraction temperature, CO
2Extract 3h under the flow 10L/h condition, get the Common Adenostema Herb extract, extract disperses with hot water, last polyamide resin column; Flow velocity 1.2BV/h, it is colourless that first water is washed till water lotion, uses 30% ethanol elution again, uses 70% ethanol elution at last; Collect 70% ethanol eluate, it is 1.12 that elutriant is evaporated to specific density, and the chrysanthemumic acid B crude extract that obtains going to the field is with the acidic alumina absorption of chrysanthemumic acid B crude extract with 3 times of amounts of going to the field; In 40 ℃ of oven drying at low temperatures, the dry method upper prop, with sherwood oil, petroleum ether-ethyl acetate, the methyl alcohol gradient elution of different ratios, the thin-layer chromatography inspection; Collect the high-content chrysanthemumic acid B flow point of going to the field, be evaporated to small volume, crystallization; Coarse-grain with ETHYLE ACETATE-acetone recrystallization, is obtained the 532mg chrysanthemumic acid B monomeric compound of going to the field, and its content is 98.6%.
Embodiment 4:
With the Common Adenostema Herb pulverizing medicinal materials, get 5kg and drop in the supercritical extraction jar, add volume percent and be 60% acetone soln as entrainment agent, add-on is 0.5kg (raw material weight 10%), at extracting pressure 35MPa, 50 ℃ of extraction temperature, CO
2Extract 2h under the flow 30L/h condition, get the Common Adenostema Herb extract, extract disperses with hot water, last polyamide resin column; Flow velocity 0.5BV/h, it is colourless that first water is washed till water lotion, uses 40% ethanol elution again, uses 90% ethanol elution at last; Collect 90% ethanol eluate, it is 1.11 that elutriant is evaporated to specific density, and the chrysanthemumic acid B crude extract that obtains going to the field is with the acidic alumina absorption of chrysanthemumic acid B crude extract with 4 times of amounts of going to the field; In 45 ℃ of oven drying at low temperatures, the dry method upper prop, with the ETHYLE ACETATE-methanol mixed solution gradient wash-out of different ratios, the thin-layer chromatography inspection; Collect the high-content chrysanthemumic acid B flow point of going to the field, be evaporated to small volume, crystallization; Coarse-grain with ETHYLE ACETATE-acetone recrystallization, is obtained the 514mg chrysanthemumic acid B monomeric compound of going to the field, and its content is 98.2%.
Claims (3)
1. preparation method of chrysanthemumic acid B that goes to the field is characterized in that may further comprise the steps:
1) supercritical extraction: get the Common Adenostema Herb pulverizing medicinal materials, put into supercritical CO
2In the extraction kettle, add an amount of organic solvent again, feed CO as entrainment agent
2,, extract CO under the extraction temperature 30-50 ℃ of condition at extracting pressure 20-35MPa
2Flow velocity is 10-30L/h, extracts 1-3h, collects extract;
2) polyamide column chromatography: extract is added in the polyamide resin column, control flow velocity 0.5-1.5BV/h, first water is eluted to colourless, uses the 30-90% ethanol gradient elution again, collects elutriant, is concentrated into specific density 1.08-1.12, the chrysanthemumic acid B crude extract of must going to the field;
3) alumina column chromatography: the acidic alumina absorption that the chrysanthemumic acid B crude extract of will going to the field is doubly measured with 3-4, oven drying at low temperature below 50 ℃, dry column-packing; Use the mixed solvent gradient elution, collect and to contain the go to the field flow point of chrysanthemumic acid B of high-content, be evaporated to small volume; Crystallization gets coarse-grain;
4) recrystallization: coarse-grain with ETHYLE ACETATE-acetone mixing solutions recrystallization, is obtained the highly purified chrysanthemumic acid B monomeric compound of going to the field.
2. the preparation method of a kind of chrysanthemumic acid B that goes to the field according to claim 1 is characterized in that, the said entrainment agent of step (1) is ethanol or the acetone soln of 60-90%, and add-on is the 5-15% that is equivalent to raw material weight.
3. the preparation method of a kind of chrysanthemumic acid B that goes to the field according to claim 1 is characterized in that, the described mixed solvent of step (3) is sherwood oil, ETHYLE ACETATE, methyl alcohol, acetone, alcoholic acid mixing solutions.
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| CN201110263991A CN102320959A (en) | 2011-09-08 | 2011-09-08 | The preparation method of a kind of chrysanthemumic acid B that goes to the field |
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| CN201110263991A CN102320959A (en) | 2011-09-08 | 2011-09-08 | The preparation method of a kind of chrysanthemumic acid B that goes to the field |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020011949A (en) * | 2018-07-10 | 2020-01-23 | 洋 竹森 | Melanogenesis suppressor, production method therefor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020011949A (en) * | 2018-07-10 | 2020-01-23 | 洋 竹森 | Melanogenesis suppressor, production method therefor |
| JP7262319B2 (en) | 2018-07-10 | 2023-04-21 | 洋 竹森 | Melanin production inhibitor and method for producing melanin production inhibitor |
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Application publication date: 20120118 |