CN101993354A - Method for extracting resveratrol - Google Patents
Method for extracting resveratrol Download PDFInfo
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- CN101993354A CN101993354A CN2009100701053A CN200910070105A CN101993354A CN 101993354 A CN101993354 A CN 101993354A CN 2009100701053 A CN2009100701053 A CN 2009100701053A CN 200910070105 A CN200910070105 A CN 200910070105A CN 101993354 A CN101993354 A CN 101993354A
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- extraction
- resveratrol
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- giant knotweed
- enzymolysis
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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 discloses a method for extracting resveratrol, belongs to a method for preparing a compound by extracting and distilling. The method comprises the following steps of: soaking traditional Chinese medicine material of giant knotweed in water, drying and crushing into giant knotweed powder; adding water, which is 10 times as much as the giant knotweed powder in volume ratio, processing with 300w ultrasonic for 10-15min; adding 1wt%-5wt% of cellulase and carrying out enzymolysis reaction at constant temperature of 40-60 DEG C to obtain giant knotweed powder subjected to enzymolysis; adding a mixed solution of absolute ethyl alcohol and 2-propanol, which is 10 times as much as the giant knotweed powder and used as a modifier; supercritically extracting with CO2 and collecting extracts; carrying out vacuum decompressed concentration to obtain a concentrated filtrate containing resveratrol; and finally chromatographing and refining by using macroporous adsorption resin. By using the method, the consumption of an extraction solvent can be greatly reduced, the cost can be reduced, the process is easy to operate, the extraction solvent CO2 can be recycled, little pollution to environment can be caused.
Description
Technical field
The present invention relates to prepare with extractive distillation the method for compound, specifically is the method that enzyme process-supercritical extraction is handled the extraction trans-resveratrol of giant knotweed.
Background technology
Giant knotweed (Polygonum Cuspidatum Sieb.et Zucc) is a polygonaceae Polygonum undershrub, is the traditional Chinese medicine of China, mainly is distributed in ground such as East China, Central-South, Liaoning, Shaanxi, Gansu, Sichuan, Guizhou and Yunnan.Have the analgesic therapy of invigorating blood circulation, clearing heat and promoting diuresis, relieving cough and reducing sputum effect.Trans-resveratrol (Resveratrol) is one of effective constituent in the traditional Chinese medicine giant knotweed, and its chemistry is called 3,4 ', and 5-trihydroxy--anti--stilbene (3,4 ', 5-trihydroxystilbene), molecular formula C
14H
12O
3, molecular weight 228, its structure is as follows:
Trans-resveratrol is a kind of human health to be had the natural active matter of significant curative effect effect, has now caused the common concern of international community.Prove through scientific research and clinical application; it is anticancer, anti-oxidant and prevent thrombosis that trans-resveratrol has; protection liver and remove effect such as free radical all has prevention and therapeutic action preferably to the elderly's degenerative disorders such as parkinsonism, dementia, presenile dementia, rheumatism etc.Aspect makeup, the effect that it has eliminating chloasma and brightens; It is to lipid metabolism and hematoblasticly solidify also all influentially, can prevent and treat diseases such as coronary heart disease and atherosclerosis.Therefore, trans-resveratrol has become the active skull cap components that scientists is paid much attention to, has very big pharmaceutical use and market outlook.
Chinese patent CN1621401A, it is that the giant knotweed dry rhizome meal through pre-treatment is added the certain amount of organic solvent refluxing extraction to disclose " a kind of method of extracting high-purity resveratrol from giant knotweed ", after reclaiming solvent, adopt the solvent of opposed polarity to carry out reflux operation, the recovery part solvent, centrifugal, precipitation obtains the high-purity resveratrol crystallization after water and sorbent treatment.
This method is used a large amount of organic solvents, and environment is had serious harm, and product yield is lower, and cost is very high, is unfavorable for suitability for industrialized production.
Chinese patent CN100340536C, disclosed " supercritical CO
2Extract giant knotweed trans-resveratrol technology ", be the employing supercritical CO
2Extraction process, and make properties-correcting agent with dehydrated alcohol and 2-propyl alcohol mixed solvent, can reduce the extraction solvent load greatly, reduce cost, technology is simple, the yield height, superior product quality is extracted solvent C O
2Can be recycled, environmental pollution is little.
Chinese patent CN1090603C disclosed " a kind of trans-resveratrol technology of from Chinese medicine tiger battle, extracting ", described extraction process is: add cellulase in the Powdered giant knotweed raw material, carry out obtaining in enzyme digestion reaction 48-72 hour the enzymolysis raw material under constant temperature; Solubilizing agent extraction again, the concentrated work in-process that obtain to contain trans-resveratrol are again through making with extra care promptly.It is rich to have raw material sources, and technology is simple and direct, yield is high, the advantage at the bottom of the cost.
Supercritical CO
2Fluid extraction is the new and high technology that modern age, separation field occurred, and it can reduce the usage quantity of organic solvent effectively, improves extraction efficiency; It is volatile to have selected extraction solvent, and extract is comparatively clean, to characteristics such as the pollution of environment are few.
But in above-mentioned technology, owing to just selected giant knotweed has been carried out simple pre-treatment process, thus influenced the yield of product.
Summary of the invention
The present invention is exactly the above-mentioned defective that exists at prior art, provides the battle of a kind of enzymatic treatment tiger to extract the method for trans-resveratrol.
The present invention is achieved by the following technical solutions:
A kind of method of extracting trans-resveratrol, Chinese medicine material giant knotweed water logging after drying, pulverizing are Powdered giant knotweed raw material, the water that adds 10 times of amounts by volume, through the 300w ultrasonication after 10-15 minute, add 1%～5% cellulase more by weight percentage, carry out under 40～60 ℃ of constant temperature enzyme digestion reaction obtain enzymolysis after Giant Knotweed Rhizome; Be incorporated in the dehydrated alcohol of 10 times of amounts of Giant Knotweed Rhizome and the mixed solution of 2-propyl alcohol and make properties-correcting agent, supercritical CO
2Extract is collected in extraction, and vacuum decompression concentrates to such an extent that contain the concentrated filtrate of trans-resveratrol; Form through macroporous adsorption resin chromatography is refining.
The method of described extraction trans-resveratrol, its Powdered giant knotweed raw material is that the Chinese medicine giant knotweed was soaked 48～72 hours, pulls out and dries, pulverizes, 40 mesh sieves are collected excessively.
The method of described extraction trans-resveratrol, its enzyme digestion reaction are regulated the pH value 4.5～5.5, enzymolysis 60～120min, taking precipitate.
The method of described extraction trans-resveratrol, described supercritical CO
2Extraction is that Giant Knotweed Rhizome behind the enzymolysis is changed in the extraction kettle, the pressure of regulating extraction kettle is 20～35Mpa, extraction temperature is 40～55 ℃, extraction-container pressure is 7～5Mpa, resolution temperature is 40～55 ℃, begin circulation, the mixed solution that added dehydrated alcohol and 2-propyl alcohol volume ratio simultaneously and be 7: 3 to 8: 2 is made properties-correcting agent, carries out supercritical CO
2Behind extraction 60～120min, the pressure of regulating extraction-container is 5～6.5Mpa, and resolution temperature is 40～50 ℃, collects extract.
The method of described extraction trans-resveratrol, described extract are at 40～50 ℃, vacuum tightness-40cmHg～-the 60cmHg condition under, carry out vacuum decompression and concentrate, reclaim properties-correcting agent, collect the concentrated filtrate that contains trans-resveratrol.
The method of described extraction trans-resveratrol, described refining be to carry out chromatographic separation with containing macroporous adsorptive resins cleaned on the concentrated filtrate of trans-resveratrol, concentrating under reduced pressure, lyophilize, the trans-resveratrol of purity 〉=98%.
The invention has the advantages that: 1, the Chinese medicine giant knotweed is adopted enzyme solution and supersound process, raw material is effectively separated, improved the utilization ratio of resource greatly; 2, adopt supercritical CO
2Abstraction technique, technological operation is simple, yield is high, product purity is high, and solvent consumption is few, and organic solvent-free is residual, and the course of processing is less to the harm and the environmental pollution of human body; 3, use the macroporous absorption technical point from purified resveratrol, the separating effect ideal, technology is simple; Resin can repeat regeneration, cost is low, equipment is simple, less investment, industrial prospect are better.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
The present invention will be described in detail below in conjunction with drawings and Examples.
Embodiment 1:
Take by weighing Chinese medicinal materials giant knotweed 10g, add water 20ml and soaked 48 hours, pull out and dry, pulverize the back and cross 40 mesh sieves; Add 100mL distilled water, through 300W ultrasonication 15 minutes, further pulverize, regulate pH value 4.5～4.8, add cellulase 0.1g, keeping temperature is 45～48 ℃, and behind the enzymolysis 60min, branch is got precipitation, is dried to Giant Knotweed Rhizome behind the enzymolysis; With the powder supercritical CO of packing into
2In the extraction kettle, regulating extraction kettle pressure is 20Mpa, and extraction temperature is 40 ℃, extraction-container pressure 5Mpa, temperature is 40 ℃, extract, add the properties-correcting agent that the 2-propyl alcohol by 70ml dehydrated alcohol and 30ml mixes simultaneously, behind the extraction 60min, regulating extraction-container pressure is 5Mpa, resolution temperature is 40 ℃, collects extract, gets the trans-resveratrol crude product; Reclaim properties-correcting agent, at 40 ℃, under vacuum tightness-40cmHg condition vacuum decompression concentrate concentrated filtrate; At last, through macroporous adsorption resin chromatography, further refining purity is 97.8% trans-resveratrol product 0.056g.
Embodiment 2:
Get Chinese medicinal materials giant knotweed 10g, add water 20ml and soaked 48 hours, pull out and dry, pulverized 40 mesh sieves, add 100mL distilled water, through 300W ultrasonication 15 minutes, further pulverize, regulate pH value 4.8～5.0, add cellulase 0.2g, keeping temperature is 45～50 ℃, behind the enzymolysis 90min, divides and gets precipitation and be dried to Giant Knotweed Rhizome behind the enzymolysis; With the powder supercritical CO of packing into
2In the extraction kettle, regulating extraction kettle pressure is 30Mpa, and extraction temperature is 50 ℃, extraction-container pressure 6Mpa, temperature is 48 ℃, extract, add the dehydrated alcohol of 80ml and the 2-propyl alcohol of 20ml simultaneously and make properties-correcting agent, behind the extraction 90min, regulating extraction-container pressure is 5.8Mpa, resolution temperature is 45 ℃, collects extract, gets the trans-resveratrol crude product; At last, reclaim properties-correcting agent, at 45 ℃, under vacuum tightness-50cmHg condition vacuum decompression concentrate concentrated filtrate; At last, through macroporous adsorption resin chromatography, further refining purity is 98.5% trans-resveratrol product 0.083g.
Embodiment 3:
Get Chinese medicinal materials giant knotweed 10g, add water 20ml and soaked 48 hours, pull out and dry, pulverized 40 mesh sieves, add 100mL distilled water,, further pulverize, make the fiber of tiger battle become loose, help the release of the effective goods and materials of trans-resveratrol through 300W ultrasonication 15 minutes; Regulate pH value 4.6～5.2, add cellulase 0.3g, keeping temperature is 47～52 ℃, and behind the enzymolysis 120min, branch is got precipitation, is dried to Giant Knotweed Rhizome behind the enzymolysis, with the powder supercritical CO of packing into
2In the extraction kettle, regulating extraction kettle pressure is 35Mpa, and extraction temperature is 55 ℃, extraction-container pressure 7Mpa, temperature is 53 ℃, extracts, and the 2-propyl alcohol that adds 80ml dehydrated alcohol and 20ml is simultaneously made properties-correcting agent, behind the extraction 120min, regulating extraction-container pressure is 6.5Mpa, and resolution temperature is 48 ℃.Collect extract, get the trans-resveratrol crude product; At last, reclaim properties-correcting agent, at 50 ℃, under vacuum tightness-60cmHg condition vacuum decompression concentrate concentrated filtrate; At last, through cleaned macroporous adsorption resin chromatography, further refining purity is 98% trans-resveratrol product 0.079g.
Claims (6)
1. method of extracting trans-resveratrol, it is characterized in that: Chinese medicine material giant knotweed water logging after drying, pulverizing are Powdered giant knotweed raw material, the water that adds 10 times of amounts by volume, through the 300w ultrasonication after 10-15 minute, add 1%～5% cellulase more by weight percentage, carry out under 40～60 ℃ of constant temperature enzyme digestion reaction obtain enzymolysis after Giant Knotweed Rhizome; Be incorporated in the dehydrated alcohol of 10 times of amounts of Giant Knotweed Rhizome and the mixed solution of 2-propyl alcohol and make properties-correcting agent, supercritical CO
2Extract is collected in extraction, and vacuum decompression concentrates to such an extent that contain the concentrated filtrate of trans-resveratrol; Form through macroporous adsorption resin chromatography is refining.
2. according to the method for the described extraction trans-resveratrol of claim 1, it is characterized in that Powdered giant knotweed raw material is that the Chinese medicine giant knotweed was soaked 48～72 hours, pull out and dry, pulverize that 40 mesh sieves are collected excessively.
3. according to the method for the described extraction trans-resveratrol of claim 1, it is characterized in that described enzyme digestion reaction adjusting pH value 4.5～5.5, enzymolysis 60～120min, taking precipitate.
4. according to the method for the described extraction trans-resveratrol of claim 1, it is characterized in that through supercritical CO
2Extraction is that Giant Knotweed Rhizome behind the enzymolysis is changed in the extraction kettle, the pressure of regulating extraction kettle is 20～35Mpa, extraction temperature is 40～55 ℃, extraction-container pressure is 7～5Mpa, resolution temperature is 40～55 ℃, begin circulation, the mixed solution that added dehydrated alcohol and 2-propyl alcohol volume ratio simultaneously and be 7: 3 to 8: 2 is made properties-correcting agent, carries out supercritical CO
2Behind extraction 60～120min, the pressure of regulating extraction-container is 5～6.5Mpa, and resolution temperature is 40～50 ℃, collects extract.
5. according to the method for claim 1 or 4 described extraction trans-resveratrols, it is characterized in that described extract is at 40～50 ℃, vacuum tightness-40cmHg～-the 60cmHg condition under, carry out vacuum decompression and concentrate, reclaim properties-correcting agent, collect the concentrated filtrate that contains trans-resveratrol.
6. according to the method for the described extraction trans-resveratrol of claim 1, it is characterized in that described making with extra care is to carry out chromatographic separation with containing macroporous adsorptive resins cleaned on the concentrated filtrate of trans-resveratrol, concentrating under reduced pressure, lyophilize, the trans-resveratrol of purity 〉=98%.
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| CN2009100701053A CN101993354A (en) | 2009-08-11 | 2009-08-11 | Method for extracting resveratrol |
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| CN2009100701053A CN101993354A (en) | 2009-08-11 | 2009-08-11 | Method for extracting resveratrol |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102329366A (en) * | 2011-07-26 | 2012-01-25 | 苏州宝泽堂医药科技有限公司 | Method for extracting arundoin from imperata cylindrica |
| CN102649723A (en) * | 2011-02-25 | 2012-08-29 | 苏州宝泽堂医药科技有限公司 | Method for extracting irisquinone from Chinese iris seed coat |
| CN102924239A (en) * | 2012-10-23 | 2013-02-13 | 南方医科大学 | Method for separating trans-resveratrol from giant knotweed |
| CN103396214A (en) * | 2013-07-23 | 2013-11-20 | 苏州仁成生物科技有限公司 | Microcapsule fertilizer rich in phosphorus and preparation method thereof |
| CN103396213A (en) * | 2013-07-23 | 2013-11-20 | 苏州仁成生物科技有限公司 | Potassium-rich microcapsule fertilizer and preparation method thereof |
| CN104341277A (en) * | 2014-11-18 | 2015-02-11 | 白心亮 | Method for extracting resveratrol from Polygonum cuspidatum |
| CN105420293A (en) * | 2015-11-06 | 2016-03-23 | 贵州天豪民族药业有限公司 | Method for separating and purifying resveratrol from traditional Chinese medicine polygonum cuspidatum extraction solution |
| CN108033874A (en) * | 2017-12-28 | 2018-05-15 | 长沙善道新材料科技有限公司 | Biological extraction method of resveratrol |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649723A (en) * | 2011-02-25 | 2012-08-29 | 苏州宝泽堂医药科技有限公司 | Method for extracting irisquinone from Chinese iris seed coat |
| CN102329366A (en) * | 2011-07-26 | 2012-01-25 | 苏州宝泽堂医药科技有限公司 | Method for extracting arundoin from imperata cylindrica |
| CN102924239A (en) * | 2012-10-23 | 2013-02-13 | 南方医科大学 | Method for separating trans-resveratrol from giant knotweed |
| CN103396214A (en) * | 2013-07-23 | 2013-11-20 | 苏州仁成生物科技有限公司 | Microcapsule fertilizer rich in phosphorus and preparation method thereof |
| CN103396213A (en) * | 2013-07-23 | 2013-11-20 | 苏州仁成生物科技有限公司 | Potassium-rich microcapsule fertilizer and preparation method thereof |
| CN103396214B (en) * | 2013-07-23 | 2016-03-09 | 苏州仁成生物科技有限公司 | A kind of rich phosphorus microcapsule fertilizer and preparation method thereof |
| CN103396213B (en) * | 2013-07-23 | 2016-03-09 | 苏州仁成生物科技有限公司 | Fertilizer of a kind of rich potassium microcapsule and preparation method thereof |
| CN104341277A (en) * | 2014-11-18 | 2015-02-11 | 白心亮 | Method for extracting resveratrol from Polygonum cuspidatum |
| CN104341277B (en) * | 2014-11-18 | 2016-08-31 | 内蒙古昶辉生物科技股份有限公司 | A kind of method extracting resveratrol from Rhizoma Polygoni Cuspidati |
| CN105420293A (en) * | 2015-11-06 | 2016-03-23 | 贵州天豪民族药业有限公司 | Method for separating and purifying resveratrol from traditional Chinese medicine polygonum cuspidatum extraction solution |
| CN108033874A (en) * | 2017-12-28 | 2018-05-15 | 长沙善道新材料科技有限公司 | Biological extraction method of resveratrol |
| CN108033874B (en) * | 2017-12-28 | 2020-11-20 | 亓云吉 | Biological extraction method of resveratrol |
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Application publication date: 20110330 |