CN103571891A - Method for extracting resveratrol from polygonum cuspidatum - Google Patents
Method for extracting resveratrol from polygonum cuspidatum Download PDFInfo
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- CN103571891A CN103571891A CN201310531416.1A CN201310531416A CN103571891A CN 103571891 A CN103571891 A CN 103571891A CN 201310531416 A CN201310531416 A CN 201310531416A CN 103571891 A CN103571891 A CN 103571891A
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Abstract
The invention discloses a method for extracting resveratrol from polygonum cuspidatum. The method comprises the following steps: (1), carrying out natural enzymolysis, namely, crushing the polygonum cuspidatum, adding water which is adjusted by using hydrochloric acid so as to have the pH of 4-5, uniformly mixing, sealing in a fermentation tank, carrying out insulation and enzymolysis at a temperature of 40-50 DEG C for 4-5 days to obtain an enzymolysis material; (2), extracting, namely, adding an organic solvent in the enzymolysis material for reflowing and extracting for 2-4 times, and mixing extraction solutions; (3), carrying out column chromatography, namely enabling the mixed extraction solution to pass through a chromatographic column loaded with aluminum oxide resin, and collecting a column passing effluent, wherein the flow velocity of the extraction solution is 1-2BV/h; (4), decoloring, namely, adding active oxide in the effluent, raising the temperature to 60-120 DEG C, stirring for 1-2h, filtering while heating to obtain a filtrate; (5), concentrating and crystallizing, namely, concentrating the filtrate to 1/10-1/15 of the original filtrate in volume, cooling, devitrifying, and filtering to obtain the resveratrol. The method is low in production cost; the resveratrol is high in purity and yield, and is suitable for industrialized large-scale production.
Description
Technical field
The present invention relates to a kind of method of extracting trans-resveratrol, especially relate to a kind of method of extracting trans-resveratrol from giant knotweed.
Background technology
Trans-resveratrol is a kind of natural antioxidant, can reduce blood viscosity, anti-platelet clotting and vasorelaxation, keep unobstructed blood, generation and deterioration that can preventing cancer, have atherosclerosis, the control of coronary heart disease, ischemic heart disease, hyperlipidemia, suppress tumour, estrogen-like effects, can be used for treating the diseases such as mammary cancer.1998, when American scholar is write the anti-ageing canon > of < < > mono-book, trans-resveratrol is classified as to one of " 100 kinds of effective anti-ageing materials the most popular ".
At present, the method for extracting trans-resveratrol from giant knotweed mainly contains three kinds:
1, in raw material, add plant enzyme, polidatin is hydrolyzed to trans-resveratrol under the effect of exogenous enzyme, then use organic solvent extraction.The consumption of this method enzyme is large, and cost is high.
2, use organic solvent extraction raw material, concentrate to obtain medicinal extract, in medicinal extract, add plant enzyme, by polidatin hydrolysis, then use organic solvent extraction.Although the consumption of this method enzyme is little, products obtained therefrom purity is not high, approximately 50% left and right.
3, use organic solvent extraction raw material, concentrated, removal of impurities, refining, obtain polidatin sterling, then be hydrolyzed by chemical process, obtain trans-resveratrol.Although this method products obtained therefrom purity is higher, the production cycle is long, and yield is low, is no more than 70%.
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of cost low, and products obtained therefrom purity is high, the method for extracting trans-resveratrol from giant knotweed that yield is high.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method of extracting trans-resveratrol from giant knotweed, comprises the following steps:
(1) natural enzymolysis: giant knotweed is pulverized, added the water with hydrochloric acid tune pH to 4～5 that is equivalent to 0.5～1.0 times of giant knotweed weight, mix, be placed in fermentor tank and seal, be incubated enzymolysis 4～5 days in 40～50 ℃ of temperature, obtain enzymolysis material;
(2) extract: in step (1) gained enzymolysis material, add organic solvent refluxing extraction 2～4 times (preferably 3 times), the consumption of each refluxing extraction organic solvent is 2～5 times of raw material giant knotweed weight, each reflux extracting time is 2～4 hours, united extraction liquid;
(3) column chromatography: by the chromatography column of aluminum oxide resin is housed, the consumption of aluminum oxide resin is 0.5～1.5 times of raw material giant knotweed weight by step (2) gained extracting solution, and the flow velocity of extracting solution is 1～2BV/ hour, collects post effluent liquid;
(4) decolouring: add gac in step (3) gained effluent liquid, the consumption of gac is 1～10% of effluent liquid weight, is warming up to 60～120 ℃, stirs 1～2 hour, and filtered while hot, obtains filtrate;
(5) condensing crystal: step (4) gained filtrate is concentrated into 1/10～1/15 of former filtrate volume, and cooling crystallization, filters.
Further, in step (1), it is 60～100 orders that giant knotweed is crushed to granular size.
Further, in step (2), extracting is methyl alcohol, ethanol, propyl alcohol, acetone or ethyl acetate etc. with organic solvent, the ethanol of the methyl alcohol of preferred volume mark 80～85% or volume fraction 80～85%.
Further, in step (5), the temperature of cooling crystallization is 0～5 ℃, and the time is 6～8 hours.
Described aluminum oxide resin can be neutral alumina resin, alkali alumina resin or acidic alumina resin, preferably neutral alumina resin.
Compared with prior art, the present invention has the following advantages:
(1) utilize the endogenous enzyme of giant knotweed self that polidatin enzymolysis is become to trans-resveratrol, do not need to use exogenous enzyme, thereby reduce production costs;
(2) reusable after extracting organic solvent used and reclaiming, also reusable after column chromatography aluminum oxide resin activation used, production cost significantly reduces;
(3) aluminum oxide resin has special adsorptive power to impurity such as the Schuttgelb in extracting solution, pigments, and to trans-resveratrol without absorption, can effectively remove impurity, guarantee product yield simultaneously;
(4) effect of separation and purification is remarkable, and product purity is more than 98%;
(5) extract thoroughly, production process loss is little, and product yield is high, reaches more than 95%;
(6) raw material sources are extensive, and equipment requirements is low, are applicable to large-scale industrialization and produce.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
embodiment 1
The present embodiment comprises the following steps:
(1) natural enzymolysis: get giant knotweed 100kg(Resveratrol content 1.29%), be crushed to 80 orders, add hydrochloric acid for 50kg to adjust the water of pH to 5, mix, be placed in fermentor tank and seal, in 50 ℃ of insulation enzymolysis 4 days, obtain enzymolysis material;
(2) extract: to step (1) gained enzymolysis material, add the methanol eddy of volume fraction 85% to extract three times, methanol usage is 400L for the first time, and extraction time is 3 hours; Methanol usage is 300L for the second time, and extraction time is 2 hours; Methanol usage is 300L for the third time, and extraction time is 2 hours, united extraction liquid;
(3) column chromatography: by the chromatography column of neutral alumina resin is housed, the consumption of aluminum oxide resin is 100kg by step (2) gained extracting solution, and the flow velocity of extracting solution is 1.5BV/ hour, collects post effluent liquid;
(4) decolouring: add gac 5kg in step (3) gained effluent liquid, be warming up to 68 ℃, stir 1.5 hours, filtered while hot, obtains filtrate;
(5) condensing crystal: filtrate is concentrated into 70L, is cooled to 5 ℃, crystallization 8 hours, filters, and obtains trans-resveratrol sterling 1.25kg, and purity is 98.60%, and yield is 96.9%.
embodiment 2
The present embodiment comprises the following steps:
(1) natural enzymolysis: get giant knotweed 100kg(Resveratrol content 1.24%), be crushed to 80 orders, add hydrochloric acid for 50kg to adjust the water of pH to 5, mix, be placed in fermentor tank and seal, in 45 ℃ of insulation enzymolysis 5 days, obtain enzymolysis material;
(2) extract: to the alcohol reflux three times that adds volume fraction 80% in step (1) gained enzymolysis material, ethanol consumption is 400L for the first time, and extraction time is 3 hours; Ethanol consumption is 300L for the second time, and extraction time is 2 hours; Ethanol consumption is 300L for the third time, and extraction time is 2 hours, united extraction liquid;
(3) column chromatography: by the chromatography column of neutral alumina resin is housed, the consumption of neutral alumina resin is 100kg by step (2) gained extracting solution, and the flow velocity of extracting solution is 1BV/ hour, collects post effluent liquid;
(4) decolouring: add gac 7kg in step (3) gained effluent liquid, be warming up to 80 ℃, stir 1.5 hours, filtered while hot, obtains filtrate;
(5) condensing crystal: filtrate is concentrated into 75L, is cooled to 0 ℃, crystallization 8 hours, filters, and obtains trans-resveratrol sterling 1.18kg, and purity is 98.52%, and yield is 95.16%.
Claims (4)
1. from giant knotweed, extract a method for trans-resveratrol, it is characterized in that, comprise the following steps:
(1) natural enzymolysis: giant knotweed is pulverized, added the water with hydrochloric acid tune pH to 4～5 that is equivalent to 0.5～1.0 times of giant knotweed weight, mix, be placed in fermentor tank and seal, be incubated enzymolysis 4～5 days in 40～50 ℃ of temperature, obtain enzymolysis material;
(2) extract: in step (1) gained enzymolysis material, add organic solvent refluxing extraction 2～4 times, the consumption of each refluxing extraction organic solvent is 2～5 times of raw material giant knotweed weight, and each reflux extracting time is 2～4 hours, united extraction liquid;
(3) column chromatography: by the chromatography column of aluminum oxide resin is housed, the consumption of aluminum oxide resin is 0.5～1.5 times of raw material giant knotweed weight by step (2) gained extracting solution, and the flow velocity of extracting solution is 1～2BV/ hour, collects post effluent liquid;
(4) decolouring: add gac in step (3) gained effluent liquid, the consumption of gac is 1～10% of effluent liquid weight, is warming up to 60～120 ℃, stirs 1～2 hour, and filtered while hot, obtains filtrate;
(5) condensing crystal: step (4) gained filtrate is concentrated into 1/10～1/15 of former filtrate volume, and cooling crystallization, filters.
2. the method for extracting trans-resveratrol from giant knotweed according to claim 1, is characterized in that, in step (1), it is 60～100 orders that giant knotweed is crushed to granular size.
3. the method for extracting trans-resveratrol from giant knotweed according to claim 1 and 2, is characterized in that, in step (2), extracting is methyl alcohol, ethanol, propyl alcohol, acetone or ethyl acetate with organic solvent.
4. the method for extracting trans-resveratrol from giant knotweed according to claim 1 and 2, is characterized in that, in step (5), the temperature of cooling crystallization is 0～5 ℃, and the time is 6～8 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104130110A (en) * | 2014-08-12 | 2014-11-05 | 四川天予植物药业有限公司 | Method for extracting resveratrol as well as obtained resveratrol and drug composition |
| CN107660561A (en) * | 2016-07-27 | 2018-02-06 | 四川利尔作物科学有限公司 | Composition pesticide and its application |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101338327A (en) * | 2008-08-13 | 2009-01-07 | 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 |
| CN101760483A (en) * | 2009-11-20 | 2010-06-30 | 南京泽朗医药科技有限公司 | Method for preparing high-purity resveratrol from fresh giant knotweed rhizome |
| CN101792373A (en) * | 2010-03-18 | 2010-08-04 | 重庆科瑞南海制药有限责任公司 | Process for extracting, separating and purifying high-purity resveratrol |
| CN101805755A (en) * | 2010-04-14 | 2010-08-18 | 卢昶年 | Process for extracting and purifying resveratrol from giant knot weed |
| CN102060887A (en) * | 2009-11-11 | 2011-05-18 | 孔令敏 | Process for extracting polydatin |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338327A (en) * | 2008-08-13 | 2009-01-07 | 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 |
| CN102060887A (en) * | 2009-11-11 | 2011-05-18 | 孔令敏 | Process for extracting polydatin |
| CN101760483A (en) * | 2009-11-20 | 2010-06-30 | 南京泽朗医药科技有限公司 | Method for preparing high-purity resveratrol from fresh giant knotweed rhizome |
| CN101792373A (en) * | 2010-03-18 | 2010-08-04 | 重庆科瑞南海制药有限责任公司 | Process for extracting, separating and purifying high-purity resveratrol |
| CN101805755A (en) * | 2010-04-14 | 2010-08-18 | 卢昶年 | Process for extracting and purifying resveratrol from giant knot weed |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104130110A (en) * | 2014-08-12 | 2014-11-05 | 四川天予植物药业有限公司 | Method for extracting resveratrol as well as obtained resveratrol and drug composition |
| CN107660561A (en) * | 2016-07-27 | 2018-02-06 | 四川利尔作物科学有限公司 | Composition pesticide and its application |
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