CN101805755A - Process for extracting and purifying resveratrol from giant knot weed - Google Patents
Process for extracting and purifying resveratrol from giant knot weed Download PDFInfo
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- CN101805755A CN101805755A CN 201010146767 CN201010146767A CN101805755A CN 101805755 A CN101805755 A CN 101805755A CN 201010146767 CN201010146767 CN 201010146767 CN 201010146767 A CN201010146767 A CN 201010146767A CN 101805755 A CN101805755 A CN 101805755A
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Abstract
The invention discloses a process for extracting and purifying resveratrol from giant knot weed. Fresh giant knot weed medicinal material is taken as raw material, water is added for soaking and self biological enzyme is utilized to carry out enzymolysis, alkali extraction and acid precipitation are carried out, the obtained precipitate is subject to destaining, crystal is seeded out, and recrystallization and drying are carried out, thus obtaining the product. Compared with the prior art, the invention directly takes fresh medicinal material as raw material, thus not only being beneficial to smashing of medicinal material but also avoiding the destroy of medicinal material to resveratrol and polydatin in drying process, besides, glucuroide in giant knot weed crude medicinal material is saved from damage, and no biological enzyme is required to be added to promote conversion of polydatin; compared with the traditional extraction process, target ingredient can be saved from damage at the utmost extent, no biological enzyme is required to be added in production process, operation link is reduced, production cost is reduced, thus being more applicable to industrialization production; and meanwhile no organic solvent is used in production process, thus being more beneficial to environmental protection; as the purity of product prepared by the method of the invention can reach more than 99%, yield can reach more than 1.3%.
Description
Technical field
The present invention relates to a kind of technology of from giant knotweed, extracting purified resveratrol, belong to the extractive technique field of active skull cap components in the herbal medicine.
Background technology
Giant knotweed (Rhizome Polygoni Cuspidati) is polygonaceae Polygonaceae plant polygonum cuspidatum Polygonum cuspidatum Sieb.et Zucc., dry rhizome and root, mainly be distributed in Shandong, Henan, Shaanxi, Hubei, Jiangxi, Fujian, Taiwan, Yunnan, Sichuan, Guizhou, Guangxi.
Trans-resveratrol is a kind of secondary metabolite in the giant knotweed, and the content of trans-resveratrol only is 0.1%～0.2% in exsiccant giant knotweed raw material, and the content of Polydatin is about 2.0%, and Polydatin can be converted into trans-resveratrol by enzymolysis.Trans-resveratrol has various biological activity and pharmacological action, have been found that have anticancer, antibiotic, anti-oxidant, preventing heart disease, effect such as reducing blood-fat and antimutagenic.The existing method of extracting trans-resveratrol from giant knotweed comprises solvent extraction, enzymolysis and extraction, microwave extraction etc., used extraction solvent is organic solvent mostly in these methods, and large usage quantity, production cost is higher, has potential safety hazard in the commercial process.Newly having occurred extracting from giant knotweed with alkali the method for trans-resveratrol in recent years, is the Chinese invention patent of CN101348805 as publication number, discloses a kind of trans-resveratrol that extracts from plant, and the preparation Resveratrol content is respectively the novel process of 50% and 98% product.This method is a raw material with plant polygonum cuspidatum, Testa arachidis hypogaeae or Semen Vitis viniferae, uses alkaline extraction, and extracting solution passes through adjust pH, uses flocculation agent, finings processing, enzymolysis, filtration, obtains the product of Resveratrol content 50% after the drying precipitate that obtains earlier; Further this product is washed with sig water, washed with water again, be dissolved in then in a large amount of hot water, water liquid is at room temperature placed, separate out precipitation, promptly obtain Resveratrol content behind the filtration drying and be 98% product to neutrality.This method not with an organic solvent is not suitable for suitability for industrialized production; But its technology is complicated, still need add biological enzyme and carry out enzymolysis in preparation process, and production cost is higher.
Summary of the invention
It is simple that the technical problem to be solved in the present invention provides a kind of technology, is raw material to give birth to the giant knotweed medicinal material, in process of production not with an organic solvent and the low technology of extracting purified resveratrol from giant knotweed of production cost.The purity of this technology products obtained therefrom can reach more than 99%, and yield can reach more than 1.3% and (amount to into dried medicinal material).
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of technology of from giant knotweed, extracting purified resveratrol, it is to be raw material to give birth to the giant knotweed medicinal material, soaks the biological enzyme that utilizes self and carries out enzymolysis, and it is heavy that alkali is proposed back acid, and the decolouring of gained precipitation is handled, crystallization, recrystallization is drying to obtain.
Aforesaid method specifically may further comprise the steps:
1) gets the raw medicinal herbs giant knotweed, pulverize, add water and under 10～50 ℃ of conditions, soaked enzymolysis 2～20 days;
2) gained enzymolysis soup adds the water of 3～10 times of raw material weights, adds alkali and regulates pH value to 8～10, is warming up to 30～60 ℃ and extracts 1～3h, filters, and collects extracting solution;
3) extracting solution adds acid for adjusting pH value to 1～4, collecting precipitation;
4) the gained precipitation is washed to neutral back dissolve with ethanol, crosses the decolorizing resin post, collects effluent liquid;
5) effluent liquid concentrates, and places crystallization, recrystallization, promptly.
Wherein:
In the step 1), the granularity that the raw medicinal herbs giant knotweed is pulverized can be 10～100 orders.The add-on of water is 0.6～1.2 times of raw material weight.The time of enzymolysis is relevant with the temperature of water, when water temperature is low the time of enzymolysis long slightly, the time of enzymolysis was short slightly when water temperature was higher.
Step 2) in, described alkali is yellow soda ash, sodium bicarbonate, sodium hydroxide or calcium hydroxide.
In the step 3), described acid is hydrochloric acid or sulfuric acid.
In the step 4), described decolorizing resin post is macroporous resin column, neutral alumina resin column or activated carbon column.The model of described macroporous resin can be AB-8, HP-20, D101, D102 etc.
In the step 5), effluent liquid is placed crystallization after can being concentrated into 0.02～0.1 times of medicinal material amount.
Crystallization.
Compared with prior art, the invention has the advantages that:
1, the present invention is a raw material with fresh medicinal material directly, not only help the pulverizing of medicinal material, also can avoid medicinal material destruction to trans-resveratrol and Polydatin in drying process, main is the glucuroide of having saved from damage in the giant knotweed raw medicinal herbs, need not to add in addition the conversion that biological enzyme promotes Polydatin again; Compare with traditional extraction technique, can save target component to greatest extent from damage, and, reduce operation link, reduce production costs, be more suitable in industrialized production because need not add any biological enzyme again in the production process;
2, carry the heavy extracting method of acid by alkali and replace conventional organic solvent extraction or extraction, technology is environmental protection more, and cost is lower;
3, the product purity height that is made by the method for the invention can reach (HPLC method mensuration) more than 99%, and yield can reach more than 1.3% and (amount to into dried medicinal material).
Embodiment
The invention will be further described with embodiment below, but the present invention is not limited to these embodiment.
Embodiment 1
Giant knotweed is pulverized, crossed 20 mesh sieves, take by weighing 50kg (dry weight 30kg), carry out enzymolysis after mixing with the water-wet of 0.7 times of raw material weight, temperature is controlled at 30 ℃, enzymolysis time 15 days; The water that adds 8 times of raw material weights in the enzymolysis soup is separated the PH=9 of soup with the sodium bicarbonate regulatory enzyme, is warming up to 50 ℃, stirs and extracts 2h, filtration; Filtrate adds hydrochloric acid and transfers PH=3, take out precipitation, be washed to neutral back dissolve with ethanol, cross the neutral alumina post and decolour, effluent liquid is concentrated into 2.4kg, places 4h, the crystal of separating out carries out recrystallization under the same conditions, drying gets trans-resveratrol white crystal 0.4kg, and HPLC method detection level is 99.2%.
Embodiment 2
Giant knotweed is pulverized, crossed 60 mesh sieves, take by weighing 80kg (dry weight 50kg), carry out enzymolysis after mixing with the water-wet of 1 times of raw material weight, temperature is controlled at 40 ℃, enzymolysis time 8 days; The water that adds 4.4 times of raw material weights in the enzymolysis soup is separated the PH=9 of soup with the sodium hydroxide regulatory enzyme, is warming up to 45 ℃, stirs and extracts 2h, filtration; Filtrate adds hydrochloric acid and transfers PH=4, take out precipitation, be washed to the neutral dissolve with ethanol of using later, cross activated carbon column and decolour, effluent liquid is concentrated into 6.2kg, places 8h, the crystal of separating out carries out recrystallization under the same conditions, drying gets trans-resveratrol white crystal 0.68kg, and HPLC method detection level is 99.1%.
Embodiment 3
Giant knotweed is pulverized, crossed 10 mesh sieves, take by weighing 100kg (dry weight 60kg), carry out enzymolysis after wetting the mixing with 1.2 times of raw material weights, temperature is controlled at 50 ℃, enzymolysis time 6 days; The water that adds 7 times of raw material weights in the enzymolysis soup is separated the PH=9 of soup with the calcium hydroxide regulatory enzyme, is warming up to 50 ℃, stir and extract 2h, filter, filtrate adds hydrochloric acid and transfers PH=1, take out precipitation, be washed to the neutral dissolve with ethanol of using later, cross AB-8 type macroporous type decolorizing resin post and decolour, effluent liquid is concentrated into 5.8kg, places 8h, and the crystal of separating out is used dissolve with ethanol again, concentrate recrystallization, drying, get trans-resveratrol white crystal 0.78kg, HPLC method detection level is 99.5%.
Embodiment 4
Giant knotweed is pulverized, crossed 100 mesh sieves, take by weighing 100kg (dry weight 60kg), carry out enzymolysis after wetting the mixing with 0.6 times of raw material weight, temperature is controlled at 15 ℃, enzymolysis time 20 days; The water that adds 10 times of raw material weights in the enzymolysis soup is separated the PH=8 of soup with the yellow soda ash regulatory enzyme, is warming up to 30 ℃, stir and extract 3h, filter, filtrate adds sulfuric acid and transfers PH=2, take out precipitation, be washed to the neutral dissolve with ethanol of using later, cross activated carbon column and decolour, effluent liquid is concentrated into 4.8kg, place 10h, the crystal of separating out carries out recrystallization, drying under the same conditions, get trans-resveratrol white crystal 0.82kg, HPLC method detection level is 99.0%.
Embodiment 5
Giant knotweed is pulverized, crossed 80 mesh sieves, take by weighing 100kg (dry weight 60kg), carry out enzymolysis after wetting the mixing with 0.8 times of raw material weight, temperature is controlled at 50 ℃, enzymolysis time 3 days; The water that adds 5 times of raw material weights in the enzymolysis soup is separated the PH=10 of soup with the sodium bicarbonate regulatory enzyme, is warming up to 60 ℃, stir and extract 1.5h, filter, filtrate adds sulfuric acid and transfers PH=1.5, take out precipitation, be washed to the neutral dissolve with ethanol of using later, cross D101 type macroporous resin column and decolour, effluent liquid is concentrated into 5.6kg, place 2h, the crystal of separating out carries out recrystallization, drying under the same conditions, get trans-resveratrol white crystal 0.79kg, HPLC method detection level is 99.3%.
Claims (6)
1. technology of extracting purified resveratrol from giant knotweed is characterized in that: it is to be raw material to give birth to the giant knotweed medicinal material, soaks the biological enzyme that utilizes self and carries out enzymolysis, and it is heavy that alkali is proposed back acid, gained precipitation crystallization after decolouring is handled, and recrystallization is drying to obtain.
2. the technology of extracting purified resveratrol from giant knotweed according to claim 1 is characterized in that may further comprise the steps:
1) gets the raw medicinal herbs giant knotweed, pulverize, add water and under 10～50 ℃ of conditions, soaked enzymolysis 2～20 days;
2) gained enzymolysis soup adds the water of 3～10 times of raw material weights, adds alkali and regulates pH value to 8～10, is warming up to 30～60 ℃ and extracts 1～3h, filters, and collects extracting solution;
3) extracting solution adds acid for adjusting pH value to 1～4, collecting precipitation;
4) the gained precipitation is washed to neutral back dissolve with ethanol, crosses the decolorizing resin post, collects effluent liquid;
5) effluent liquid concentrates, and places crystallization, recrystallization, promptly.
3. the technology of extracting purified resveratrol from giant knotweed according to claim 2, it is characterized in that: in the step 1), the add-on of water is 0.6～1.2 times of raw material weight.
4. the technology of extracting purified resveratrol from giant knotweed according to claim 2 is characterized in that: step 2) in, described alkali is yellow soda ash, sodium bicarbonate, sodium hydroxide or calcium hydroxide.
5. the technology of extracting purified resveratrol from giant knotweed according to claim 2, it is characterized in that: in the step 3), described acid is hydrochloric acid or sulfuric acid.
6. the technology of extracting purified resveratrol from giant knotweed according to claim 2, it is characterized in that: in the step 4), described decolorizing resin post is macroporous resin column, neutral alumina resin column or activated carbon column.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948370A (en) * | 2010-09-16 | 2011-01-19 | 花垣恒远植物生化有限责任公司 | Method for extracting resveratrol from polygonum cuspidatum |
| CN102080108A (en) * | 2010-12-15 | 2011-06-01 | 云南弗蓝替生物工程有限公司 | Method for extracting emodin, polydatin and resveratrol from polygonum cuspidatum by using vacuum enzymolysis technology |
| CN102408999A (en) * | 2011-06-29 | 2012-04-11 | 林元山 | Method for converting polydatin to resveratrol by microbial enzyme method |
| CN102559642A (en) * | 2012-01-19 | 2012-07-11 | 杭州师范大学 | Beta-glucosidase, coding gene, carrier and application thereof |
| CN103571891A (en) * | 2013-11-01 | 2014-02-12 | 湖南科源生物制品有限公司 | Method for extracting resveratrol from polygonum cuspidatum |
| CN105777496A (en) * | 2016-03-08 | 2016-07-20 | 陈爱华 | Method for extracting resveratrol from rhizoma polygoni cuspidate and rhizoma polygoni cuspidate healthcare product |
| EP3577228A1 (en) * | 2017-01-31 | 2019-12-11 | Evolva SA | Process and composition |
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| CN1341587A (en) * | 2001-09-17 | 2002-03-27 | 上海汇谷生物技术有限公司 | Method for preparing resveratrol from giant knotweed rhizome |
| CN1384088A (en) * | 2002-05-21 | 2002-12-11 | 杨建文 | Extraction process of resveratrol from giant knotweed |
| CN1385535A (en) * | 2002-05-29 | 2002-12-18 | 深圳清华现代中医药科技有限公司 | Method for raising Resveratrol content in Chinese herb-giant knotweed rhizome |
| CN1760166A (en) * | 2005-11-11 | 2006-04-19 | 余淑娴 | New method for picking-up purified resveratrol from giant knotweed |
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2010
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948370A (en) * | 2010-09-16 | 2011-01-19 | 花垣恒远植物生化有限责任公司 | Method for extracting resveratrol from polygonum cuspidatum |
| CN101948370B (en) * | 2010-09-16 | 2013-04-24 | 花垣恒远植物生化有限责任公司 | Method for extracting resveratrol from polygonum cuspidatum |
| CN102080108A (en) * | 2010-12-15 | 2011-06-01 | 云南弗蓝替生物工程有限公司 | Method for extracting emodin, polydatin and resveratrol from polygonum cuspidatum by using vacuum enzymolysis technology |
| CN102408999B (en) * | 2011-06-29 | 2013-12-25 | 湖南农业大学 | Method for converting polydatin to resveratrol by microbial enzyme method |
| CN102408999A (en) * | 2011-06-29 | 2012-04-11 | 林元山 | Method for converting polydatin to resveratrol by microbial enzyme method |
| CN102559642A (en) * | 2012-01-19 | 2012-07-11 | 杭州师范大学 | Beta-glucosidase, coding gene, carrier and application thereof |
| CN102559642B (en) * | 2012-01-19 | 2013-04-24 | 杭州师范大学 | Beta-glucosidase, coding gene, carrier and application thereof |
| CN103571891A (en) * | 2013-11-01 | 2014-02-12 | 湖南科源生物制品有限公司 | Method for extracting resveratrol from polygonum cuspidatum |
| CN103571891B (en) * | 2013-11-01 | 2015-07-08 | 湖南科源生物制品有限公司 | Method for extracting resveratrol from polygonum cuspidatum |
| CN105777496A (en) * | 2016-03-08 | 2016-07-20 | 陈爱华 | Method for extracting resveratrol from rhizoma polygoni cuspidate and rhizoma polygoni cuspidate healthcare product |
| EP3577228A1 (en) * | 2017-01-31 | 2019-12-11 | Evolva SA | Process and composition |
| US20200039909A1 (en) * | 2017-01-31 | 2020-02-06 | Evolva Sa | Process and composition |
| US11136283B2 (en) | 2017-01-31 | 2021-10-05 | Evolva Sa | Recovering and purifying resveratrol produced by microbial fermentation |
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