CN101338327A - Process for extracting resveratrol with purity higher than 98 0.000000rom giant knotweed - Google Patents
Process for extracting resveratrol with purity higher than 98 0.000000rom giant knotweed Download PDFInfo
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- CN101338327A CN101338327A CNA2008100320678A CN200810032067A CN101338327A CN 101338327 A CN101338327 A CN 101338327A CN A2008100320678 A CNA2008100320678 A CN A2008100320678A CN 200810032067 A CN200810032067 A CN 200810032067A CN 101338327 A CN101338327 A CN 101338327A
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- 244000153955 Reynoutria sachalinensis Species 0.000 title claims abstract description 56
- 235000003202 Reynoutria sachalinensis Nutrition 0.000 title claims abstract description 56
- LUKBXSAWLPMMSZ-OWOJBTEDSA-N Trans-resveratrol Chemical compound C1=CC(O)=CC=C1\C=C\C1=CC(O)=CC(O)=C1 LUKBXSAWLPMMSZ-OWOJBTEDSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title abstract description 17
- QNVSXXGDAPORNA-UHFFFAOYSA-N Resveratrol Natural products OC1=CC=CC(C=CC=2C=C(O)C(O)=CC=2)=C1 QNVSXXGDAPORNA-UHFFFAOYSA-N 0.000 title abstract description 6
- 229940016667 resveratrol Drugs 0.000 title abstract description 6
- 235000021283 resveratrol Nutrition 0.000 title abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 108090000790 Enzymes Proteins 0.000 claims abstract description 19
- 102000004190 Enzymes Human genes 0.000 claims abstract description 19
- 238000002425 crystallisation Methods 0.000 claims abstract description 15
- 230000008025 crystallization Effects 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000001953 recrystallisation Methods 0.000 claims abstract description 12
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 5
- 238000007670 refining Methods 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 235000018991 trans-resveratrol Nutrition 0.000 claims description 48
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 238000005516 engineering process Methods 0.000 claims description 18
- 229940088598 enzyme Drugs 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 17
- 238000005189 flocculation Methods 0.000 claims description 15
- 230000016615 flocculation Effects 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000012043 crude product Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 230000009849 deactivation Effects 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 108010059892 Cellulase Proteins 0.000 claims description 5
- 229940106157 cellulase Drugs 0.000 claims description 5
- 229940059442 hemicellulase Drugs 0.000 claims description 5
- 108010002430 hemicellulase Proteins 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 4
- 108010047754 beta-Glucosidase Proteins 0.000 claims description 3
- 102000006995 beta-Glucosidase Human genes 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 239000000796 flavoring agent Substances 0.000 claims description 3
- 235000019634 flavors Nutrition 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 230000011218 segmentation Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
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- 230000001131 transforming effect Effects 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- FYGDTMLNYKFZSV-URKRLVJHSA-N (2s,3r,4s,5s,6r)-2-[(2r,4r,5r,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5r,6s)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1[C@@H](CO)O[C@@H](OC2[C@H](O[C@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-URKRLVJHSA-N 0.000 claims description 2
- 229920002498 Beta-glucan Polymers 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 22
- 238000009776 industrial production Methods 0.000 abstract description 3
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- 239000003086 colorant Substances 0.000 abstract 1
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- 101710130006 Beta-glucanase Proteins 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
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- 239000003960 organic solvent Substances 0.000 description 3
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- 229920005989 resin Polymers 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
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- OEGPRYNGFWGMMV-UHFFFAOYSA-N (3,4-dimethoxyphenyl)methanol Chemical compound COC1=CC=C(CO)C=C1OC OEGPRYNGFWGMMV-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
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- 101710081598 Beta-glucosidase 30 Proteins 0.000 description 1
- 101710081293 Beta-glucosidase 40 Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
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- 239000002699 waste material Substances 0.000 description 1
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- Coloring Foods And Improving Nutritive Qualities (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a technique for extracting resveratrol with a purity more than 98 percent from a giant knotweed which includes as follows: using ethanol to extract after cracking the medicine of the giant knotweed, using the special enzyme of the giant knotweed for enzymolysis for 4 to 5 days under the constant temperature of 45 to 50 DEG C after condensing and recycling the ethanol; rising the temperature to 85 to 100 DEG C and maintaining for 2 minutes, then deactivating the special enzyme of the giant knotweed; filtering and the filter residue is the crude resveratrol that is converted; then using the special flocculant of the giant knotweed, to flocculate, deposit and filter; carrying out chromatography and refining on the clear liquid by an aluminum oxide layer; then the finished product is obtained by carrying out alcohol-purified water crystallization and recrystallization as well as vacuum drying on an eluent. The technique of the invention realizes to improve the purity of the resveratrol by more than 98 percent, improve the yield of the product from 0.4 -0.5 percent to 0.6 percent, lead the color of the resveratrol to be white without other colors and improve the product quality; besides, the technique of the invention can be really used for industrial production, can shorten the production period, improve the working efficiency and reduce the production cost.
Description
Technical field
The present invention relates to a kind of from giant knotweed the technology of the trans-resveratrol of dna purity more than 98%.
Background technology
The classical operational path that present domestic production enterprise produces trans-resveratrol is: giant knotweed medicinal material → pulverizing → fermentation (natural or enzyme-added) → alcohol extracting → concentrate → organic solvent extraction → recovery solvent and concentrated → pure molten → column chromatography (silica gel or aluminum oxide) → activated carbon decolorizing → crystallization and recrystallization.The yield of the finished product trans-resveratrol of this operational path generally has only 0.4%～0.5%, and color is cream colour or grey slightly, and the purity of trans-resveratrol all about 97%, is sold as 98% trans-resveratrol on the market.These data and theoretical yield have bigger discrepancy, how further to improve product yield, simultaneously color is done white, improve the quality of products be this area really the technician expect the problem that solves.The report that at present also has some to produce 98% trans-resveratrol, but these technology majorities also just rest on laboratory level, have bigger problem in actual applications, as (1) Zhou Jinke etc. at " supercritical CO
2The technical study of trans-resveratrol in the extraction giant knotweed " in reported employing supercritical CO 2 technology extraction trans-resveratrol, this is a kind of new and high technology that is applicable to lipophilic composition and thermo-sensitivity composition, but the trans-resveratrol as the resvertrol compounds is not the lipotropy chemical ingredients, and during in temperature≤60 ℃, trans-resveratrol is stable, and the physico-chemical property of this technology and trans-resveratrol is not inconsistent.And equipment has high input in the actual production, and cost is difficult to reclaim, and adding needs high-tension apparatus, has potential safety hazard again, does not therefore see have producer that this technology is used for suitability for industrialized production at present.(2) application number 200510019788.1 disclosed employing macroporous adsorbent resin separation and purification trans-resveratrols and application number 200310112538.3 disclosed employing polymeric amide chromatography method separation and purification trans-resveratrols.These two kinds of separating and purifying technologies are to the water-soluble technology of having relatively high expectations of material, and in water insoluble trans-resveratrol and water insoluble ingredients, the dissolving properties of this technology and trans-resveratrol is not inconsistent.When these two kinds of technology of employing, trans-resveratrol more than 80% can be removed as impurity in washed resin removal of impurities process, if with alcohol dissolving trans-resveratrol, the phenomenon that can in these resins, exist desorb and absorption to carry out simultaneously again, do not have the purpose of separation and purification trans-resveratrol at all.So not seeing in the historical facts or anecdotes border has manufacturing enterprise to adopt these two kinds of technology the industrialization of being unrealized.(3) fermentation or enzymolysis are the key techniques of industrial production trans-resveratrol in the reality, also are the core technology places.Report adopts aging process to transform in Qu Weilin " enzymolysis process improves veratryl alcohol Study on content in the giant knotweed ", and report adopts the prozyme solution to transform in the scientific and technological achievement of Liangshanzhou Biology Inst., Sichuan Prov. " trans-resveratrol The technique of extracting in the giant knotweed ".Adopt aging process or additional enzyme solution that polygonin is changed into trans-resveratrol, this method is feasible in theory, and reality manufacturing enterprise generally adopt this method to produce.But the method with medicinal material fermentation is earlier extracted again need take bigger production space, and about 1T medicinal material needs 3m
3The fermentative production space, caused the waste in production place; In addition, the transformation efficiency of this method is low, has 30% trans-resveratrol to be lost in the conversion process approximately; Fermentation time is long, and a general production cycle needs about 6～7 days, adds the bigger space of original needs, causes production efficiency low, and production capacity is low.
Summary of the invention
The objective of the invention is to overcome above shortcoming, provide a kind of from giant knotweed the method for the trans-resveratrol of dna purity more than 98%.The purity of trans-resveratrol brought up to more than 98% realizing, product yield to be brought up to more than 0.6% from 0.4%～0.5%, and done white the color of trans-resveratrol and non-variegation, improve the quality of products, and can really be applied to industrial production, and can shorten the production cycle, increase work efficiency.
Technical scheme of the present invention may further comprise the steps:
(1) the giant knotweed pulverizing medicinal materials is to sieving 〉=70% by No. 1;
(2) extraction using alcohol; 60% ethanol that adds 5～6 times of giant knotweed weight; Extract each 1-2 hour three times; " 60% ethanol that adds 5～6 times of giant knotweed medicinal material weight ";
(3) concentrate and recovery ethanol; 3 giant knotweed extracting solutions are reclaimed ethanol to there not being the alcohol flavor by prior art, be concentrated into relative density about 1.15.
(4) enzymolysis and deactivation: giant knotweed is extracted concentrated solution be cooled to 45 ℃～50 ℃, within 45 ℃～50 ℃; Adding citric acid or citric acid, to regulate the pH value of concentrated solution be 4.5～5.0, adds giant knotweed medicinal material weight 0.2%～0.5% giant knotweed specific enzyme again 45 ℃～50 ℃ constant temperature enzymolysis 4～5 days; Be warming up to 85-100 ℃, kept 2 minutes, with the deactivation of giant knotweed specific enzyme; Filter, filter residue is the crude product trans-resveratrol through transforming;
(5) flocculation sediment: the crude product trans-resveratrol with 65%～85% dissolve with ethanol, is filtered; Add the special-purpose flocculation agent of giant knotweed of 0.8～1.0 times of crude product trans-resveratrol weight in wet base, fully stir 10min, leave standstill 2h then, make fully precipitation of precipitation, the supernatant liquor layering is good; Filter, get filtrate;
(6) chromatography is refining: filtrate is advanced alumina chromatographic column, and own liquid begins to collect when flowing out; Liquid is carried out segmentation, flow out the red alumina column of changing during to black liquor certainly; Treat that whole filtrates have advanced after the alumina column,, be eluted to effluent liquid always and add 2 times of water and do not produce only muddy again with 65%～85% ethanol elution;
(7) crystallization and recrystallization: the effluent liquid on the alumina column is added water carry out crystallization and recrystallization, regulating alcohol concn is 10%～20%, leaves standstill 1h, filters then, and recrystallization is till the crystallization color is pure white;
(8) crystallization vacuum-drying is got finished product, finished product is a white powder, trans-resveratrol 〉=98%.
Described giant knotweed specific enzyme is mixed by following component and weight part: beta-glucosidase 30-50, beta glucan enzyme 20-40, cellulase and hemicellulase 10-30, zytase 5-20;
Special-purpose following component of flocculation agent of described giant knotweed and weight part constitute: silica gel 30-60, aluminum oxide 20-40, gac 10-30;
Advantage of the present invention: (1) has solved the key substance basis of improving trans-resveratrol output, be the composition and the proportioning of giant knotweed specific enzyme system, can effectively the polygonin in the giant knotweed be changed into trans-resveratrol, lose, improve output more than 30% than the conversion that conventional fermentation process reduces more than 25%; Transformation time is foreshortened to 4～5 days, reduced in comparison transformation time 2～3 days from 6～8 days of former technology.(2) improved the output of finished product 98% trans-resveratrol, output is brought up to 0.60%～0.75% from 0.4%～0.5%, compare and improve 0.1%～0.25%, equal raw material promptly per ton can get 98% trans-resveratrol 1kg～2.5kg more, creates 3000 yuan～7000 yuan of new value.(3) improved the color and luster of finished product 98% trans-resveratrol, removed common variety with beige to grey, further improved product colour, make the finished product become the high-quality trans-resveratrol of white non-variegation.(4) do not re-use harmful organic solvents such as ethyl acetate in the variation route; replace with special-purpose flocculation sediment behind the dissolve with ethanol; be very easy to operation; also reduced simultaneously production cost widely; no longer need to reclaim organic solvent; simplify production operation and production link, made that production is controlled easily and realized greatly, improved labor safety and protection.(5) the production space has greatly been saved in the technical process of extracting the back enzymolysis earlier that the present invention set up, and can fully effectively utilize the production place.Calculate by raw material giant knotweed per ton, produce required place and be reduced to 0.8m3, compare the space of saving more than 65%, thereby help production operation and control, enhance productivity by 3m3.(6) whole piece production process route of the present invention, fully combine the physico-chemical property characteristics of trans-resveratrol and coexistent impurity, adopt flocculation earlier, the rear oxidation aluminium lamination is analysed, and then the route of crystallization and recrystallization, has saved the operation that the gac that ordinary method adopted carries out secondary decolourization, not only saved production operation, as save insulation and micro-pore-film filtration link, and finished color is improved, produced 98% high-quality trans-resveratrol.
Embodiment
Embodiment 1:
Get giant knotweed medicinal material 500kg, be crushed to sieve percent of pass 〉=70% No. 1; 0.2%～0.5%
(2) extraction using alcohol: 60% ethanol of at every turn using 2500L; Extract each 1-2 hour three times;
(3) united extraction liquid, and concentrate and reclaim ethanol; 3 giant knotweed extracting solutions are reclaimed ethanol to there not being the alcohol flavor by prior art, be concentrated into relative density about 1.15;
(4) enzymolysis and deactivation: giant knotweed is extracted concentrated solution be cooled to 45 ℃～50 ℃, within 45 ℃～50 ℃; The pH value that adds citric acid or citric acid adjusting concentrated solution is 4.5～5.0, add 2kg giant knotweed specific enzyme again, the giant knotweed specific enzyme of present embodiment is to be mixed by following component and weight part: beta-glucosidase accounts for 45, beta-glucanase 25, cellulase and hemicellulase 15, zytase accounted for 15,45 ℃～50 ℃ constant temperature enzymolysis 4～5 days; Be warming up to 85 ℃, kept 2 minutes, with the deactivation of giant knotweed specific enzyme; Filter, filter residue is the crude product trans-resveratrol through transforming;
(5) flocculation sediment: the crude product trans-resveratrol with 65%～85% dissolve with ethanol, is filtered; The special-purpose flocculation agent of giant knotweed that adds 0.8 times of weight of crude product trans-resveratrol weight in wet base, the special-purpose flocculation agent of the giant knotweed of present embodiment is to be mixed by following component and weight part: silica gel 50, aluminum oxide 30, gac 20, fully stir 10min, leave standstill 2h then, make fully precipitation of precipitation, the supernatant liquor layering is good; Filter, get filtrate;
(6) chromatography is refining: filtrate is advanced alumina chromatographic column, and own liquid begins to collect when flowing out; Liquid is carried out segmentation, and weak yellow liquid send down the step operation, flows out the red alumina column of changing during to black liquor certainly; Treat that whole filtrates have advanced after the alumina column,, be eluted to effluent liquid always and add 2 times of water and do not produce only muddy again with 65%～85% ethanol elution;
(7) crystallization and recrystallization: the effluent liquid on the alumina column is added water carry out crystallization and recrystallization, regulating alcohol concn is 10%～20%, leaves standstill 1h, filters then, and recrystallization is till the crystallization color is pure white;
(8) crystallization vacuum-drying is got finished product 3.25kg, Resveratrol content in the finished product 〉=98%.Yield 0.65%.
Embodiment 2:
Present embodiment adds giant knotweed specific enzyme 1.5kg as different from Example 1, the giant knotweed specific enzyme is mixed by following component and weight part: beta-glucosidase 30, beta-glucanase 40, cellulase and hemicellulase 22, zytase 8, the special-purpose flocculation agent of the giant knotweed of 0.8 times of weight of adding, the special-purpose flocculation agent of giant knotweed is mixed by following component and weight part: silica gel 40, aluminum oxide 40, gac 20; Finished product 3.15kg and, yield 0.63%.
Embodiment 3:
Present embodiment adds giant knotweed specific enzyme 2.5kg as different from Example 1, the giant knotweed specific enzyme is mixed by following component and weight part: beta-glucosidase 40, beta-glucanase 30, cellulase and hemicellulase 20, zytase 10, the special-purpose flocculation agent of the giant knotweed of 0.9 times of weight of adding, the special-purpose flocculation agent of giant knotweed is mixed by following component and weight part: silica gel 40, aluminum oxide 40, gac 20; Finished product 3.75kg and, yield 0.75%.
Claims (3)
1. the technology of the trans-resveratrol of dna purity more than 98% from giant knotweed is characterized in that, may further comprise the steps:
(1) the giant knotweed pulverizing medicinal materials is to sieving 〉=70% by No. 1;
(2) extraction using alcohol; 60% ethanol that adds 5～6 times of giant knotweed weight; Extract each 1-2 hour three times;
(3) concentrate and recovery ethanol; 3 giant knotweed extracting solutions are reclaimed ethanol to there not being the alcohol flavor by prior art, be concentrated into relative density about 1.15.
(4) enzymolysis and deactivation: giant knotweed is extracted concentrated solution be cooled to 45 ℃ ~ 50 ℃, within 45 ℃ ~ 50 ℃; Adding citric acid or citric acid, to regulate the pH value of concentrated solution be 4.5 ~ 5.0, adds giant knotweed medicinal material weight 0.2% ~ 0.5% giant knotweed specific enzyme again 45 ℃ ~ 50 ℃ constant temperature enzymolysis 4 ~ 5 days; Be warming up to 85-100 ℃, kept 2 minutes, with the deactivation of giant knotweed specific enzyme; Filter, filter residue is the crude product trans-resveratrol through transforming;
(5) flocculation sediment: the crude product trans-resveratrol with 65% ~ 85% dissolve with ethanol, is filtered; Add the special-purpose flocculation agent of giant knotweed of 0.8 ~ 1.0 times of crude product trans-resveratrol weight in wet base, fully stir 10min, leave standstill 2h then, make fully precipitation of precipitation, the supernatant liquor layering is good; Filter, get filtrate;
(6) chromatography is refining: filtrate is advanced alumina chromatographic column, and own liquid begins to collect when flowing out; Liquid is carried out segmentation, flow out the red alumina column of changing during to black liquor certainly; Treat that whole filtrates have advanced after the alumina column,, be eluted to effluent liquid always and add 2 times of water and do not produce only muddy again with 65% ~ 85% ethanol elution;
(7) crystallization and recrystallization: the effluent liquid on the alumina column is added water carry out crystallization and recrystallization, regulating alcohol concn is 10% ~ 20%, leaves standstill 1h, filters then, and recrystallization is till the crystallization color is pure white;
(8) crystallization vacuum-drying is got finished product, trans-resveratrol in the finished product 〉=98%.
2. according to claim 1 from giant knotweed the technology of the trans-resveratrol of dna purity more than 98%, it is characterized in that, described giant knotweed specific enzyme is mixed by following component and weight part: beta-glucosidase 30-50, beta glucan enzyme 20-40, cellulase and hemicellulase 10-30, zytase 5-20.
3. according to claim 1 from giant knotweed the technology of the trans-resveratrol of dna purity more than 98%, it is characterized in that special-purpose following component of flocculation agent of described giant knotweed and weight part constitute: silica gel 30-60, aluminum oxide 20-40, gac 10-30.
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628858A (en) * | 2009-08-11 | 2010-01-20 | 张守力 | Preparation process of resveratrol |
| CN101628859A (en) * | 2009-08-11 | 2010-01-20 | 张守力 | Extraction method of resveratrol |
| CN101805755A (en) * | 2010-04-14 | 2010-08-18 | 卢昶年 | Process for extracting and purifying resveratrol from giant knot weed |
| CN102060397A (en) * | 2010-11-18 | 2011-05-18 | 湘西自治州兴湘科技开发有限责任公司 | Method for treating waste water generated in extraction process of active ingredient of polygonum cuspidatum |
| CN102304028A (en) * | 2011-07-01 | 2012-01-04 | 中山大学 | Method for separating and purifying resveratrol in polygonum cuspidatum |
| CN102627677A (en) * | 2012-03-22 | 2012-08-08 | 聊城大学 | Method for separating and purifying monomer compounds from Rhizoma Polygoni Cuspidati |
| CN102838455A (en) * | 2012-09-17 | 2012-12-26 | 湖南希尔天然药业有限公司 | Method for extracting high-content resveratrol from polygonum cuspidatum |
| CN101698634B (en) * | 2009-06-30 | 2013-03-27 | 三原润禾植化有限公司 | Method for extracting and separating resveratrol from giant knotweed rhizome |
| CN103396295A (en) * | 2013-07-31 | 2013-11-20 | 王喜军 | Extraction method for resveratrol from giant knotweed rhizome |
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