CN1621401A - Method for extracting high purity resveratrol from giant knotweed rhizome - Google Patents
Method for extracting high purity resveratrol from giant knotweed rhizome Download PDFInfo
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- CN1621401A CN1621401A CN 200310108968 CN200310108968A CN1621401A CN 1621401 A CN1621401 A CN 1621401A CN 200310108968 CN200310108968 CN 200310108968 CN 200310108968 A CN200310108968 A CN 200310108968A CN 1621401 A CN1621401 A CN 1621401A
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Abstract
The present invention is method of extracting high purity resveratrol from giant knotweed. Pre-treated dry coarse giant knotweed powder is added with certain amount of organic solvent for reflux extraction, and after the organic solvent is recovered, it is extracted with different kinds of polar solvent. Through further recovering partial solvent, centrifugation, and precipitate treatment with water and adsorbent, high purity resveratrol crystal is obtained. The present invention has the advantages of flexible technological process, simple operation, simple apparatus, less solvent consumption and high product yield.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity resveratrol, particularly from giant knotweed, prepare the method for high-purity resveratrol.
Technical background
Trans-resveratrol is one of effective constituent in the traditional Chinese medicine giant knotweed, has anticancer, anti-oxidant, reducing blood-fat, protection liver and removes effect such as free radical, long hyperlipidemia, the atherosclerotic assisting therapy of being used for; Also as the functional ingredient in the superior cosmetics, the effect that has the class of dispelling to whiten.The existing trans-resveratrol that obtains is mainly by two kinds of approach: the one, and synthetic; The 2nd, from plant, extract.The former technical difficulty height, the equipment complexity, products obtained therefrom purity is not high, and biological activity is relatively low.Latter's extraction efficiency is low, and the production cycle is long, the technology relative complex.At publication number CN1277954A, name is called that disclosed technical scheme is in the patent of " preparation method of trans-resveratrol and polidatin ": with the giant knotweed rhizome with organic solvent through extract, extraction, concentrated, silica gel column chromatography, crystallization, recrystallization and obtain trans-resveratrol; Publication number CN1384088A, name is called that disclosed technical scheme is in the patent of " a kind of preparing resveratrol of extracting " from giant knotweed: after the methodology of organic synthesis enrichment, utilize chloroform and ethyl acetate to pressurize wash-out and obtain trans-resveratrol with composite filler by proportioning, in the special high-pressure tomography devices giant knotweed.Aforesaid method all needs the special layers desorption device, and solvent loss is big, the technical process complexity, so its industrialization degree is not high, cost is high.
Summary of the invention
For overcoming existing preparation method's deficiency, the present invention adopts ordinary method to produce high-purity resveratrol, has extraction efficiency height, technology is simple, product purity is high, production cost is low advantage.
Basic technology method of the present invention is as follows:
1. medicinal material pre-treatment:
With the water of giant knotweed medicinal material by 2 times of amounts of its volume proportion adding, soaked 48-72 hour, pull out and dry, pulverize standby.
2. extract:
Treated medicinal material fine powder is added the organic solvent refluxing extraction 2 times, the 3-5 that consumption of organic solvent is respectively raw material by its volume proportion doubly, 2-4 doubly, extraction time was respectively 1,0.5 hour, merged each extracting solution, the reclaim under reduced pressure organic solvent gets solid residue;
To the used organic solvent of giant knotweed medicinal material extract is any and any mixed solvent of proportioning thereof in ethanol, ethyl acetate, propyl acetate, the butylacetate.
3. separate:
The solid residue of gained is added the ethanolic soln of 100 times of amounts by its volume proportion, refluxing extraction 15 minutes, cold filtration, filtrate recycling ethanol obtains the trans-resveratrol coarse crystallization, obtains the coarse crystallization precipitation after centrifugal;
It is the mixed solvent of any proportioning of second alcohol and water that solid residue is extracted agents useful for same.
4. purifying:
The trans-resveratrol coarse crystallization is added the water that 500-2000 doubly measures by its volume proportion, 0.2 Liang gac doubly, refluxing extraction 15 minutes, rapid while hot suction filtration, white, needle-shaped crystals is separated out in the filtrate cooling, filters and obtains crystallization, mother liquor recovery set usefulness, precipitation promptly gets purity greater than 95% trans-resveratrol product through vacuum-drying.
It is water that the trans-resveratrol coarse crystallization is extracted agents useful for same, and sorbent material is a gac.
Embodiment
Example 1
Get giant knotweed medicinal material 1000 grams, adding water soaked 48 hours for 2000 milliliters, pull out and dry, pulverize the back and cross 60 mesh sieves, added 3000 milliliters of ethyl acetate backflow 1 hour, filter, the dregs of a decoction added 2000 milliliters of ethyl acetate backflow 30 minutes, filtered merging filtrate, reclaim ethyl acetate, solid residue added 1000 milliliter of 40% alcohol reflux 15 minutes, put cold after-filtration, filtrate recycling ethanol to 500 milliliter, putting has brown precipitate to separate out after cold, the centrifugal precipitation that obtains adds 1000 ml waters, 0.2 the gram gac refluxed 30 minutes, rapid while hot suction filtration, separate out white, needle-shaped crystals after the filtrate cooling, suction filtration, mother liquor recovery set usefulness, filter cake was through 60 ℃ of vacuum-dryings 6 hours, pulverize, get 0.98 gram off-white powder.Contain trans-resveratrol 98.8% through the high performance liquid chromatography detection.
Example 2
Get giant knotweed medicinal material 1000 grams, adding water soaked 72 hours for 2000 milliliters, pull out and dry, pulverize the back and cross 60 mesh sieves, added 5000 milliliters of ethyl acetate backflow 1 hour, filter, the dregs of a decoction added 3000 milliliters of ethyl acetate backflow 30 minutes, filtered merging filtrate, reclaim ethyl acetate, solid residue added 1000 milliliter of 60% alcohol reflux 15 minutes, put cold after-filtration, filtrate recycling ethanol to 300 milliliter, putting has brown precipitate to separate out after cold, the centrifugal precipitation that obtains adds 2000 ml waters, 0.2 the gram gac refluxed 30 minutes, rapid while hot suction filtration, separate out white, needle-shaped crystals after the filtrate cooling, suction filtration, mother liquor recovery set usefulness, filter cake was through 60 ℃ of vacuum-dryings 6 hours, pulverize, get 1.12 gram off-white powder.Contain trans-resveratrol 96.7% through the high performance liquid chromatography detection.
In conjunction with above example, the present invention compares with existing technology and has the following advantages:
1. adopt ordinary method to be prepared, required equipment is simple, easy to operate, safety;
2. do not adopt extraction, chromatography operation, the organic solvent loss is little, and environment is not polluted.
Claims (4)
1. method of extracting high-purity resveratrol from giant knotweed is characterized in that with following method realization:
(1). the water logging bubble that the giant knotweed medicinal material is added 2 times of amounts was pulled out and dried after 48-72 hour, was ground into fine powder, and is standby;
(2). add the organic solvent refluxing extraction 2 times, the 3-5 that consumption of organic solvent is respectively raw material by its volume proportion doubly, 2-4 doubly, extraction time was respectively 1,0.5 hour, merged each extracting solution, the reclaim under reduced pressure organic solvent must solid residue;
(3). the solid residue of gained is added the ethanolic soln of 100 times of amounts by its volume proportion, refluxing extraction 15 minutes, cold filtration, filtrate recycling ethanol obtains the trans-resveratrol coarse crystallization, obtains the coarse crystallization precipitation after centrifugal;
(4). the trans-resveratrol coarse crystallization is added the water that 500-2000 doubly measures, the gac of 0.2 times of amount, refluxing extraction 15 minutes by its volume proportion, filtered while hot, white, needle-shaped crystals is separated out in the filtrate cooling, filtration obtains crystallization, promptly gets purity greater than 95% trans-resveratrol product through vacuum-drying.
2. preparation method as claimed in claim 1 is characterized in that to the used organic solvent of giant knotweed medicinal material extract be any and any mixed solvent of proportioning thereof in ethanol, ethyl acetate, propyl acetate, the butylacetate.
3. preparation method as claimed in claim 1 is characterized in that it is the mixed solvent of any proportioning of second alcohol and water that solid residue is extracted agents useful for same.
4. preparation method as claimed in claim 1 is characterized in that it is water that the trans-resveratrol coarse crystallization is extracted agents useful for same, and sorbent material is a gac.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310108968 CN1621401A (en) | 2003-11-28 | 2003-11-28 | Method for extracting high purity resveratrol from giant knotweed rhizome |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310108968 CN1621401A (en) | 2003-11-28 | 2003-11-28 | Method for extracting high purity resveratrol from giant knotweed rhizome |
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| CN1621401A true CN1621401A (en) | 2005-06-01 |
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| CN 200310108968 Pending CN1621401A (en) | 2003-11-28 | 2003-11-28 | Method for extracting high purity resveratrol from giant knotweed rhizome |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100338083C (en) * | 2005-09-13 | 2007-09-19 | 河北医科大学 | Method for preparing polygonin through tissue culture and inducement of hairy roots of giant knotweed |
| CN101870640A (en) * | 2010-07-08 | 2010-10-27 | 贵州师范大学 | Method for preparing resveratrol extract from giant knotweed and product |
| CN101338327B (en) * | 2008-08-13 | 2011-03-23 | 长沙华诚生物科技有限公司 | Process for extracting resveratrol with purity higher than 98 0.000000rom giant knotweed |
| CN101195559B (en) * | 2007-12-12 | 2011-04-06 | 汪云 | Process for producing resveratrol nano-crystallization and uses thereof |
| CN106117020A (en) * | 2016-06-14 | 2016-11-16 | 南京华宽信息咨询中心 | The extracting method of a kind of resveratrol and resveratrol extract |
| CN106727346A (en) * | 2016-12-08 | 2017-05-31 | 天津市益倍建生物技术有限公司 | A kind of resveratrol pellet preparation and preparation method thereof |
| CN106890221A (en) * | 2017-01-11 | 2017-06-27 | 广州品红制药有限公司 | A kind of preparation method of the effective ingredient in Chinese for treating hyperlipidemia |
-
2003
- 2003-11-28 CN CN 200310108968 patent/CN1621401A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100338083C (en) * | 2005-09-13 | 2007-09-19 | 河北医科大学 | Method for preparing polygonin through tissue culture and inducement of hairy roots of giant knotweed |
| CN101195559B (en) * | 2007-12-12 | 2011-04-06 | 汪云 | Process for producing resveratrol nano-crystallization and uses thereof |
| CN101338327B (en) * | 2008-08-13 | 2011-03-23 | 长沙华诚生物科技有限公司 | Process for extracting resveratrol with purity higher than 98 0.000000rom giant knotweed |
| CN101870640A (en) * | 2010-07-08 | 2010-10-27 | 贵州师范大学 | Method for preparing resveratrol extract from giant knotweed and product |
| CN106117020A (en) * | 2016-06-14 | 2016-11-16 | 南京华宽信息咨询中心 | The extracting method of a kind of resveratrol and resveratrol extract |
| CN106727346A (en) * | 2016-12-08 | 2017-05-31 | 天津市益倍建生物技术有限公司 | A kind of resveratrol pellet preparation and preparation method thereof |
| CN106890221A (en) * | 2017-01-11 | 2017-06-27 | 广州品红制药有限公司 | A kind of preparation method of the effective ingredient in Chinese for treating hyperlipidemia |
| CN106890221B (en) * | 2017-01-11 | 2020-10-16 | 广州一品红制药有限公司 | Preparation method of traditional Chinese medicine effective part for treating hyperlipidemia |
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