CN102477354A - Process of extracting volatile oils and alpinetin from Alpinia katsumadai - Google Patents
Process of extracting volatile oils and alpinetin from Alpinia katsumadai Download PDFInfo
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- CN102477354A CN102477354A CN2010105577498A CN201010557749A CN102477354A CN 102477354 A CN102477354 A CN 102477354A CN 2010105577498 A CN2010105577498 A CN 2010105577498A CN 201010557749 A CN201010557749 A CN 201010557749A CN 102477354 A CN102477354 A CN 102477354A
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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
Abstract
The invention relates to a process of extracting volatile oils and alpinetin from Alpinia katsumadai. The process comprises the following steps of: grinding Alpinia katsumadai material, loading to an extraction kettle; performing supercritical CO2 extraction; filtering to obtain a volatile oil product; mixing the extraction residues with an appropriate amount of entrainers; performing supercritical CO2 extraction again to obtain flavonoids; diluting the flavonoid extract; subjecting to membrane separation; purifying by polyamide column chromatography; eluting with alcohols; concentrating to crystallize the eluate; re-crystallizing with anhydrous methanol; filtering out crystals; and drying to obtain an alpinetin product. The process is simple, has less pollution and low energy consumption, and is better in extraction rate and purity.
Description
Technical field
The present invention relates to a kind of plain technology of volatile oil alpinia japonica of from one's early teens, extracting.
Background technology
Alpinia japonica plain (Alpinetin);
Chemical name: (S)-7-hydroxy-5-methyl oxygen base flavones;
Molecular formula: C
16H
14O
4Molecular weight: 270.27996;
Molecular structural formula:
Be the zingiberaceous plant dry near maturate seed of Alpinia katsumadai Hayata in one's early teens in one's early teens,, have warming spleen and stomach for dispelling cold, promoting the circulation of QI to relieve pain for one of aromatic damp resolving drug commonly used; Drying damp and strengthening spleen effect cures mainly trusted subordinate's crymodynia, and ruffian is completely eaten stagnant; Dysphagia and regurgitation, cold-dampness are vomited and diarrhoea, and phlegm and retained fluid is gathered etc.Seed contains flavonoid compound such as Alpinia japonica plain (Alpinetin) and Cardamonin (Carda-monin) and volatile oil compound; Effects such as that Alpinia japonica have is antibiotic, anti-oxidant, anticancer, antithrombotic, hypotensive, reducing blood-fat, hypoglycemic, antiemetic, analgesia; Decoction is excited to guinea pig in vitro intestinal tube lower concentration in one's early teens, is higher than 1% concentration and volatile oil saturated aqueous solution and then all is restraining effect; With the Pavlov's pouch test, 10% infusion 60-80ml pours into main stomach in one's early teens, surveys microgastria secretion situation, and the result does not have influence and the pepsic activity that significantly raises to the total acid output of stomach.1979, reports such as ItokawaH, the alcohol extractive of seed is to several no antagonistic actions of mouse ascites sarcoma 180 in one's early teens.Lee in 1980 carries out chronic pharmacological evaluation at reports such as coloured glazes through having threeway Pavlov's pouch dog, and leach liquor does not have tangible influence to total acid output in one's early teens, but peptic activity of stomach is obviously raise.
At present; Alpinia japonica Study on extraction plain and Semen Alpiniae Katsumadai volatile oil is less; Wherein Wang Xiu celery etc. " plain preferred with the Cardamonin extraction process of Alpinia japonica in one's early teens " plain process for extracting of disclosed Alpinia japonica is to measure 95% alcohol reflux twice for 8 times with medicinal material; Each 2h, it is many that this method efficient part extracts loss, and extraction yield is low.After the process for extracting of the disclosed Cardamonin of Shi Daohua etc. " in one's early teens in Cardamonin extraction process improve " is 95% extraction using alcohol, extract, silicagel column and gel filtration chromatography isolation and purification.
Summary of the invention
The technical problem that the present invention will solve provides a kind of plain technology of volatile oil alpinia japonica of from one's early teens, extracting.
The objective of the invention is to realize through following technical solution:
A kind of plain technology of volatile oil alpinia japonica of from one's early teens, extracting is characterized in that this technology may further comprise the steps:
1) pulverize: medicinal material is removed impurity in one's early teens, is ground into meal, and is subsequent use;
2) supercritical CO
2Extraction: medicinal material coarse powder is dropped in the extraction kettle, the debugging extraction kettle, separating still, warming apparatus and refrigeration plant works better are opened the compression pump pressurization, pumping liquid CO
2Extract volatile oil component, from separating still, resolve extract, collect extract, filter and promptly get the volatile oil product, the dregs of a decoction after the above-mentioned extraction are added the entrainment agent that 0.1-0.2 doubly measures, supercritical CO
2The flavones ingredient extract is collected in extraction;
3) membrane sepn: above-mentioned extract adds 70% ethanol and disperses, and filters through ultra-filtration membrane, must see through liquid;
4) polyamide column purifying: the above-mentioned an amount of polyamide resin of liquid adding that sees through stirs, and volatilizes solvent, the dry method upper prop, and the alcoholic solution wash-out, the HPLC monitoring is collected and is rich in the plain flow point of Alpinia japonica;
5) recrystallization: the plain flow point decompression and solvent recovery of above-mentioned Alpinia japonica, crystallization adds anhydrous methanol backflow dissolving, puts cold crystallization, leaches crystallizing and drying and promptly gets the plain product of Alpinia japonica.
Said step 2) volatile oil component supercritical CO in
2Extraction conditions is: extraction temperature is 35-45 ℃, and extracting pressure is 18-25MPa, CO
2Flow is 25-40L/h, and the extraction time is 1.5-3h, and the separation reactor I temperature is 30-40 ℃, and pressure is 5.5-7.5MPa, and separation reactor I I temperature is 30-45 ℃, and pressure is 5-6.5MPa.
Said step 2) flavones ingredient supercritical CO in
2The condition of extracting is: extraction temperature is 55-75 ℃, and extracting pressure is 30-45MPa, CO
2Flow is 25-45L/h, and the extraction time is 2-5h, and entrainment agent is the 85%-95% methanol solution, and the separation reactor I temperature is 40-45 ℃, and pressure is 7-10MPa, and separation reactor I I temperature is 30-45 ℃, and pressure is 5-6.5MPa.
The ultra-filtration membrane that uses in the said step 3) is the hollow composite package of molecular weight cut-off 3000-10000, pressure 0.5-1MPa.
Elutriant is the methanol solution of 75-90% in the said step 4), and consumption is a 4-8 times of column volume.
The present invention adopts supercritical extraction, can improve the plain yield of volatile oil alpinia japonica, reduces purification step, reduces the toxic agent consumption.Compare with existing process for extracting, the inventive method technology is simple, and is easy and simple to handle, and product purity is high, and has improved the utilization ratio that medicinal material is arranged.
Embodiment
Following embodiment can make those skilled in the art understand the present invention better, but is not limitation of the present invention.
Embodiment 1:
Medicinal material is removed impurity in one's early teens, is ground into meal, and get 500g and drop in the extraction kettle, the debugging extraction kettle, extraction temperature is 45 ℃, extracting pressure is 18MPa, CO
2Flow is 40L/h, and the extraction time is 1.5h, and the separation reactor I temperature is 40 ℃, and pressure is 6.5MPa; Separation reactor I I temperature is 45 ℃, and pressure is 5.5MPa, from separating still, resolves extract; Collect extract, filter and promptly get the volatile oil product, the dregs of a decoction after the above-mentioned extraction are added the 0.1L85% methanol solution; Regulate the extraction parameter: extraction temperature is 55 ℃, and extracting pressure is 45MPa, CO
2Flow is 35L/h, and the extraction time is 2.5h, and the separation reactor I temperature is 40 ℃, and pressure is 9MPa, and separation reactor I I temperature is 45 ℃, and pressure is 6.5Mpa, carries out supercritical CO
2The flavones ingredient extract is collected in extraction, and extract adds 70% ethanol and disperses, through the hollow composite package of 3000-10000, pressure 0.5MPa; Collect and see through liquid, add the 10g polyamide resin and stir, volatilize solvent, polyamide column on the dry method is with the methanol solution of 5 times of column volumes 75%; The HPLC monitoring is collected the plain flow point of Alpinia japonica, decompression and solvent recovery, crystallization; Add anhydrous methanol backflow dissolving, put cold crystallization, leach crystallizing and drying and promptly get the plain product 3.2g of Alpinia japonica, content is 98.53%.
Embodiment 2:
Medicinal material is removed impurity in one's early teens, is ground into meal, and get 500g and drop in the extraction kettle, the debugging extraction kettle, extraction temperature is 35 ℃, extracting pressure is 25MPa, CO
2Flow is 30L/h, and the extraction time is 3h, and the separation reactor I temperature is 30 ℃, and pressure is 7MPa; Separation reactor I I temperature is 35 ℃, and pressure is 6MPa, from separating still, resolves extract; Collect extract, filter and promptly get the volatile oil product, the dregs of a decoction after the above-mentioned extraction are added the 0.1L90% methanol solution; Regulate the extraction parameter: extraction temperature is 75 ℃, and extracting pressure is 30MPa, CO
2Flow is 25L/h, and the extraction time is 5h, and the separation reactor I temperature is 45 ℃, and pressure is 10MPa, and separation reactor I I temperature is 40 ℃, and pressure is 5.5Mpa, carries out supercritical CO
2The flavones ingredient extract is collected in extraction, and extract adds 70% ethanol and disperses, through the hollow composite package of 3000-10000, pressure 0.8MPa; Collect and see through liquid, add the 10g polyamide resin and stir, volatilize solvent, polyamide column on the dry method is with the methanol solution of 6 times of column volumes 80%; The HPLC monitoring is collected the plain flow point of Alpinia japonica, decompression and solvent recovery, crystallization; Add anhydrous methanol backflow dissolving, put cold crystallization, leach crystallizing and drying and promptly get the plain product 3.6g of Alpinia japonica, content is 98.06%.
Embodiment 3:
Medicinal material is removed impurity in one's early teens, is ground into meal, and get 1kg and drop in the extraction kettle, the debugging extraction kettle, extraction temperature is 40 ℃, extracting pressure is 20MPa, CO
2Flow is 25L/h, and the extraction time is 2.5h, and the separation reactor I temperature is 35 ℃, and pressure is 6MPa; Separation reactor I I temperature is 30 ℃, and pressure is 5MPa, from separating still, resolves extract; Collect extract, filter and promptly get the volatile oil product, the dregs of a decoction after the above-mentioned extraction are added the 0.2L95% methanol solution; Regulate the extraction parameter: extraction temperature is 65 ℃, and extracting pressure is 35MPa, CO
2Flow is 45L/h, and the extraction time is 2h, and the separation reactor I temperature is 40-45 ℃, and pressure is 7MPa, and separation reactor I I temperature is 35 ℃, and pressure is 5MPa, carries out supercritical CO
2The flavones ingredient extract is collected in extraction, and extract adds 70% ethanol and disperses, through the hollow composite package of 3000-10000, pressure 0.6MPa; Collect and see through liquid, add the 25g polyamide resin and stir, volatilize solvent, polyamide column on the dry method is with the methanol solution of 4 times of column volumes 90%; The HPLC monitoring is collected the plain flow point of Alpinia japonica, decompression and solvent recovery, crystallization; Add anhydrous methanol backflow dissolving, put cold crystallization, leach crystallizing and drying and promptly get the plain product 7.4g of Alpinia japonica, content is 98.72%.
Embodiment 4:
Medicinal material is removed impurity in one's early teens, is ground into meal, and get 1kg and drop in the extraction kettle, the debugging extraction kettle, extraction temperature is 35 ℃, extracting pressure is 25MPa, CO
2Flow is 28L/h, and the extraction time is 2h, and the separation reactor I temperature is 38 ℃, and pressure is 5.5MPa; Separation reactor I I temperature is 40 ℃, and pressure is 6.5MPa, from separating still, resolves extract; Collect extract, filter and promptly get the volatile oil product, the dregs of a decoction after the above-mentioned extraction are added the 0.25L85% methanol solution; Regulate the extraction parameter: extraction temperature is 60 ℃, and extracting pressure is 40MPa, CO
2Flow is 40L/h, and the extraction time is 3h, and the separation reactor I temperature is 40-45 ℃, and pressure is 8MPa, and separation reactor I I temperature is 40 ℃, and pressure is 6MPa, carries out supercritical CO
2The flavones ingredient extract is collected in extraction, and extract adds 70% ethanol and disperses, through the hollow composite package of 3000-10000, pressure 0.6MPa; Collect and see through liquid, add the 20g polyamide resin and stir, volatilize solvent, polyamide column on the dry method is with the methanol solution of 8 times of column volumes 85%; The HPLC monitoring is collected the plain flow point of Alpinia japonica, decompression and solvent recovery, crystallization; Add anhydrous methanol backflow dissolving, put cold crystallization, leach crystallizing and drying and promptly get the plain product 8.9g of Alpinia japonica, content is 96.67%.
Embodiment 5:
Medicinal material is removed impurity in one's early teens, is ground into meal, and get 5kg and drop in the extraction kettle, the debugging extraction kettle, extraction temperature is 45 ℃, extracting pressure is 25MPa, CO
2Flow is 40L/h, and the extraction time is 3h, and the separation reactor I temperature is 40 ℃, and pressure is 7.5MPa; Separation reactor I I temperature is 35 ℃, and pressure is 5MPa, from separating still, resolves extract; Collect extract, filter and promptly get the volatile oil product, the dregs of a decoction after the above-mentioned extraction are added 1L 90% methanol solution; Regulate the extraction parameter: extraction temperature is 70 ℃, and extracting pressure is 38MPa, CO
2Flow is 40L/h, and the extraction time is 3.5h, and the separation reactor I temperature is 40-45 ℃, and pressure is 10MPa, and separation reactor I I temperature is 35 ℃, and pressure is 6.5MPa, carries out supercritical CO
2The flavones ingredient extract is collected in extraction, and extract adds 70% ethanol and disperses, through the hollow composite package of 3000-10000, pressure 0.6MPa; Collect and see through liquid, add the 100g polyamide resin and stir, volatilize solvent, polyamide column on the dry method is with the methanol solution of 5 times of column volumes 75%; The HPLC monitoring is collected the plain flow point of Alpinia japonica, decompression and solvent recovery, crystallization; Add anhydrous methanol backflow dissolving, put cold crystallization, leach crystallizing and drying and promptly get the plain product 37.1g of Alpinia japonica, content is 98.43%.
Embodiment 6:
Medicinal material is removed impurity in one's early teens, is ground into meal, and get 5kg and drop in the extraction kettle, the debugging extraction kettle, extraction temperature is 35 ℃, extracting pressure is 20MPa, CO
2Flow is 35L/h, and the extraction time is 2.5h, and the separation reactor I temperature is 35 ℃, and pressure is 6.5MPa; Separation reactor I I temperature is 45 ℃, and pressure is 5.5MPa, from separating still, resolves extract; Collect extract, filter and promptly get the volatile oil product, the dregs of a decoction after the above-mentioned extraction are added the 1L85% methanol solution; Regulate the extraction parameter: extraction temperature is 55 ℃, and extracting pressure is 38MPa, CO
2Flow is 42L/h, and the extraction time is 3h, and the separation reactor I temperature is 45 ℃, and pressure is 7MPa, and separation reactor I I temperature is 30 ℃, and pressure is 6.5Mpa, carries out supercritical CO
2The flavones ingredient extract is collected in extraction, and extract adds 70% ethanol and disperses, through the hollow composite package of 3000-10000, pressure 0.6Mpa; Collect and see through liquid, add the 120g polyamide resin and stir, volatilize solvent, polyamide column on the dry method is with the methanol solution of 6 times of column volumes 90%; The HPLC monitoring is collected the plain flow point of Alpinia japonica, decompression and solvent recovery, crystallization; Add anhydrous methanol backflow dissolving, put cold crystallization, leach crystallizing and drying and promptly get the plain product 31.9g of Alpinia japonica, content is 98.88%.
Claims (5)
1. one kind is extracted the plain technology of volatile oil alpinia japonica from one's early teens, it is characterized in that this technology may further comprise the steps:
1) pulverize: medicinal material is removed impurity in one's early teens, is ground into meal, and is subsequent use;
2) supercritical CO
2Extraction: medicinal material coarse powder is dropped in the extraction kettle, and debugging extraction kettle, separating still, warming apparatus and refrigeration plant works better are opened the compression pump pressurization, pumping liquid CO
2Extract volatile oil component, from separating still, resolve extract, collect extract, filter and promptly get the volatile oil product, the dregs of a decoction after the above-mentioned extraction are added the entrainment agent that 0.1-0.2 doubly measures, supercritical CO
2The flavones ingredient extract is collected in extraction;
3) membrane sepn: above-mentioned extract adds 70% ethanol and disperses, and filters through ultra-filtration membrane, must see through liquid;
4) polyamide column purifying: the above-mentioned an amount of polyamide resin of liquid adding that sees through stirs, and volatilizes solvent, the dry method upper prop, and the alcoholic solution wash-out, the HPLC monitoring is collected and is rich in the plain flow point of Alpinia japonica;
5) recrystallization: the plain flow point decompression and solvent recovery of above-mentioned Alpinia japonica, crystallization adds anhydrous methanol backflow dissolving, puts cold crystallization, leaches crystallizing and drying and promptly gets the plain product of Alpinia japonica.
2. a kind of plain technology of volatile oil alpinia japonica of from one's early teens, extracting according to claim 1 is characterized in that said step 2) middle volatile oil component supercritical CO
2Extraction conditions is: extraction temperature is 35-45 ℃, and extracting pressure is 18-25MPa, CO
2Flow is 25-40L/h, and the extraction time is 1.5-3h, and the separation reactor I temperature is 30-40 ℃, and pressure is 5.5-7.5MPa, and separation reactor I I temperature is 30-45 ℃, and pressure is 5-6.5MPa.
3. a kind of plain technology of volatile oil alpinia japonica of from one's early teens, extracting according to claim 1 is characterized in that said step 2) middle flavones ingredient supercritical CO
2The condition of extracting is: extraction temperature is 55-75 ℃, and extracting pressure is 30-45MPa, CO
2Flow is 25-45L/h, and the extraction time is 2-5h, and entrainment agent is the 85%-95% methanol solution, and the separation reactor I temperature is 40-45 ℃, and pressure is 7-10MPa, and separation reactor I I temperature is 30-45 ℃, and pressure is 5-6.5MPa.
4. a kind of plain technology of volatile oil alpinia japonica of from one's early teens, extracting according to claim 1, the ultra-filtration membrane that it is characterized in that using in the said step 3) is the hollow composite package of molecular weight cut-off 3000-10000, pressure 0.5-1MPa.
5. a kind of plain technology of volatile oil alpinia japonica of from one's early teens, extracting according to claim 1 is characterized in that elutriant is the methanol solution of 75-90% in the said step 4), and consumption is a 4-8 times of column volume.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104068211A (en) * | 2014-06-14 | 2014-10-01 | 塔里木大学 | Preparation method and application of oxytropis glabra DC flavone |
| CN105837546A (en) * | 2016-04-27 | 2016-08-10 | 聊城大学 | Method for separating and purifying alnustone, pinocembrin, cardamomin and alpinetin from alpinia katsumadai |
| CN106190579A (en) * | 2016-08-22 | 2016-12-07 | 鹰潭华宝香精香料有限公司 | The method extracting Herba Schizonepetae spice |
| CN106823454A (en) * | 2017-03-22 | 2017-06-13 | 广州国草夏方生物科技有限公司 | A kind of continuous selective extraction method of volatile oil and flavones in cacumen biotae |
| CN113318135A (en) * | 2021-05-25 | 2021-08-31 | 湖南省国方中医药科技有限公司 | External formula for treating pain and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104068211A (en) * | 2014-06-14 | 2014-10-01 | 塔里木大学 | Preparation method and application of oxytropis glabra DC flavone |
| CN105837546A (en) * | 2016-04-27 | 2016-08-10 | 聊城大学 | Method for separating and purifying alnustone, pinocembrin, cardamomin and alpinetin from alpinia katsumadai |
| CN106190579A (en) * | 2016-08-22 | 2016-12-07 | 鹰潭华宝香精香料有限公司 | The method extracting Herba Schizonepetae spice |
| CN106823454A (en) * | 2017-03-22 | 2017-06-13 | 广州国草夏方生物科技有限公司 | A kind of continuous selective extraction method of volatile oil and flavones in cacumen biotae |
| CN113318135A (en) * | 2021-05-25 | 2021-08-31 | 湖南省国方中医药科技有限公司 | External formula for treating pain and preparation method and application thereof |
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Application publication date: 20120530 |