CN101628859A - Extraction method of resveratrol - Google Patents
Extraction method of resveratrol Download PDFInfo
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- CN101628859A CN101628859A CN200910162072A CN200910162072A CN101628859A CN 101628859 A CN101628859 A CN 101628859A CN 200910162072 A CN200910162072 A CN 200910162072A CN 200910162072 A CN200910162072 A CN 200910162072A CN 101628859 A CN101628859 A CN 101628859A
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Abstract
The invention provides a preparation method of resveratrol, which relates to the field of medicament preparation and solves the problems of low preparation conversion rate, low yield and poor product quality of resveratrol in the prior art. The process comprises the following steps: pretreating giant knotweed used as raw material, washing away dust of the giant knotweed, cutting the giant knotweed into slices or preparing the giant knotweed into coarse powder, adding ethanol and heating to carry out reflux extraction, decompressing and distilling extract liquid to recover the ethanol, concentrating the ethanol into stiff paste, diluting the stiff paste by water for 10 times, adding enzymolysis liquid to carry out enzymolysis, heating and filtering the enzymatic enzymolysis liquid, decoloring the enzymolysis liquid by activated carbon, repeatedly recrystallizing the enzymolysis liquid by alcohol, and finally decompressing and drying the enzymolysis liquid to obtain a white resveratrol solid with purity of more than 98 percent. The extraction method of resveratrol greatly improves the production efficiency and the conversion rate, promotes active substances in the raw material to be converted into trans-resveratrol more, and further improves the quality of products with high purity, thereby being suitable for industrial production.
Description
Technical field
The present invention relates to the Chinese medicine extraction of effective components, be specifically related to from the Chinese medicine giant knotweed, extract the extracting method of trans-resveratrol.
Background technology
Trans-resveratrol, English name Resveratrol, molecular formula C
14H
12O
3, molecular weight 228.25.At occurring in nature, trans-resveratrol mainly is present in the plants such as grape, giant knotweed, peanut, Maackia amurensis Rupr et Maxim.Trans-resveratrol is a kind of natural antioxidant, but blood viscosity lowering suppresses thrombocyte and condenses and vasorelaxation, keep unobstructed blood, but the generation of preventing cancer and development has atherosclerosis and coronary heart disease, ischemic heart disease, the preventive and therapeutic effect of hyperlipidemia.Suppress tumour, anti-inflammatory, antianaphylactic effect in addition, also have estrogen-like effects, can be used for treating diseases such as mammary cancer.
Its existence form of trans-resveratrol mainly contains 4 kinds, is respectively cis-resveratrol, trans-resveratrol and cis-resveratrol glucosides, trans-resveratrol glucosides.Trans-resveratrol mainly exists with trans forms, and the physiologically active of trans-isomer(ide) is better than cis-isomeride, and monomer is better than glucosides.
In the prior art scheme, the extracting method of trans-resveratrol has multiple common methods such as solvent-extraction process, alkali extraction and acid precipitation, ultrasonic extraction, supercritical CO 2 extraction.All there are some defectives in this several method, but time-consuming longer, efficient is not high as solvent-extraction process, and output is very low.The polydatin that alkali extraction method obtains is more, and impurity is more, and Resveratrol content is low, and can produce a large amount of bucks.Ultrasonic extraction and supercritical CO 2 abstraction technique equipment requirements height, problems such as also some Technology Need is further perfect in the process of production in enormous quantities.Application number is 99115156.9 patent disclosure a kind ofly will add complex enzyme zymohydrolysis in the Powdered giant knotweed raw material, concentrates the half-finished extraction process that obtains to contain trans-resveratrol through extracting again.But this patent does not disclose any information of prozyme, does not provide other corresponding data that can compare reference yet.Application number be 200810004142.X patent disclosure a kind of from peanut root, stem, leaf through the method for enzymolysis and extraction trans-resveratrol.But this method is to extract trans-resveratrol from peanut root, stem, leaf, and the yet just low dose of of process using extracts, and yet do not meet need of industrial production.System meets also report not of employing enzymolysis process that industrialized producing technology requires extracts trans-resveratrol from the giant knotweed starting material method.
Summary of the invention
An object of the present invention is to solving above-mentioned prior art extraction time long, transformation efficiency is low, problems such as technological operation complexity provide reliability, the product recovery rate height of a kind of simple operation, conversion, can reach the extracting method of the trans-resveratrol that suitability for industrialized production requires.
This method comprises the steps the giant knotweed starting material through pre-treatment, after dust is fallen in drip washing, cuts into slices or makes meal, adds alcohol heating reflux and extracts, and ethanol is reclaimed in the extracting solution underpressure distillation, and be concentrated into the thick paste shape, and dilute with water 5-15 doubly and adds the enzymolysis solution enzymolysis.Enzymolysis solution heating suction filtration with enzymolysis after good, and through activated carbon decolorizing with alcohol recrystallization repeatedly, can get purity at the white solid trans-resveratrol more than 98% behind the last drying under reduced pressure again.
A nearlyer step says that described technology is as follows:
After 1 part of raw material drip washing fallen dust, to be cut into thickness be the sheet of 0.5-3mm or make meal, stand-by; With starting material giant knotweed section or make meal refluxing extraction is more than 2 times in advance with the ethanol of 70-80%, amount of alcohol is respectively starting material more than 1 times, preferred 2-3 doubly, return time 1-2.5h, united extraction liquid is concentrated into amalgamation liquid the thick paste shape again; Add 5-15 times of water to heavy paste extract, and add 0.01-0.05 part enzyme, described enzyme is a cellulase, or prozyme, and described prozyme is any one or a multiple mixture in cellulase and distiller's yeast, amylase, proteolytic enzyme, lipase, the N,O-Diacetylmuramidase; Cellulase and distiller's yeast, amylase, proteolytic enzyme, lipase, N,O-Diacetylmuramidase are according to Mass Calculation, and ratio is 1: 0-2: 0-0.5: 0-1: 0-1: 0-0.5; Enzymolysis time is 2-24 hour, and hydrolysis temperature is 15-70 ℃
Purifying: enzymolysis solution is heated to 80 ℃ of suction filtrations while hot, and uses activated carbon decolorizing, get crude product; Recrystallization 2-5 time must elaboration repeatedly by ethanol with crude product; Get finished product behind the elaboration drying under reduced pressure.
In the described prozyme, cellulase and distiller's yeast, amylase, proteolytic enzyme, lipase, N,O-Diacetylmuramidase are according to Mass Calculation, and preferred proportion is 1: 1: 0.3-0.4: 0.5-0.6: 0.5-0.7: 0.2-0.3.
Described proteolytic enzyme is preferably aspartic protease.
Comprise cellulase and distiller's yeast in the described prozyme, the preferred mass ratio is 1: 1.
Comprise cellulase, amylase, three kinds of enzymes of aspartic protease in the described prozyme, the ratio of three kinds of enzymes preferred 1: 2: 3 or 2: 3: 5.
Describedly comprise cellulase, amylase, proteolytic enzyme, lipase and N,O-Diacetylmuramidase in compound, the ratio of five kinds of enzymes is preferably 3: 2: 2: 2: 1.
Described enzymolysis time 4-6 hour, hydrolysis temperature 40-50 ℃.
Beneficial effect of the present invention is:
The present invention through research improvement repeatedly, adopts enzymolysis process on the basis of the work of summing up forefathers and oneself exploration, extract purified resveratrol from giant knotweed.Whole leaching process all is to finish whole production processes in the alcohol-water system, and schedule of operation is easy, and solvent is safe in utilization, and production cost is low, and can really realize the purpose of industrialized production.
Greatly improve production efficiency and transformation efficiency by method of the present invention, impelled the active substance in the raw material more to be converted into trans-resveratrol, made quality product further improve, and the product purity height, be fit to suitability for industrialized production.
Embodiment
Further specify the present invention below in conjunction with embodiment, but not as a limitation of the invention.
Embodiment 1
Giant knotweed starting material 1kg, through pre-treatment, after dust is fallen in drip washing, section, the extraction using alcohol 2h that adds 800ml 80% again uses the alcohol reflux 1h of 500ml 80% again, concentrates, concentrated solution is added 100ml water dilution, join among the Xie Huachi of the enzymolysis solution that contains the 0.02kg cellulase and carry out enzymolysis 5h.Enzymolysis solution with enzymolysis after good changes extractor over to, heats 100 ℃ of 30min, and filtered while hot also adds activated carbon decolorizing, with alcohol recrystallization repeatedly, again behind drying under reduced pressure 98% finished product 9.2g.
Embodiment 2
After dust was fallen in drip washing, to cut thickness be the sheet of 2mm or make meal, stand-by; With 10kg starting material giant knotweed section or make meal with 75% the alcohol reflux of using three parts of every part of 5000ml respectively 3 times, each return time 1.5h.United extraction liquid is concentrated into amalgamation liquid the thick paste shape again, is 1000ml; Heavy paste extract adds 10 times of water, adds the 0.3kg prozyme in wherein a part of water, is mixed with enzymolysis solution, carries out enzymolysis.Described prozyme is that 0.15kg cellulase and 0.15kg distiller's yeast mix; Enzymolysis time is 5 hours, and temperature is 50 ℃ enzymolysis solution is heated to 80 ℃ of suction filtrations while hot, and uses activated carbon decolorizing, crude product.With crude product by ethanol repeatedly recrystallization 3 times elaboration.Get finished product behind the elaboration drying under reduced pressure.
Embodiment 3
Described enzymolysis solution is cellulase, amylase, three kinds of prozymes of aspartic protease, and the ratio of three kinds of enzymes is 1: 2: 3, and all the other are with embodiment 2.
Embodiment 4
Described enzymolysis solution is cellulase, amylase, three kinds of prozymes of aspartic protease, and the ratio of three kinds of enzymes is 2: 3: 5, and all the other are with embodiment 2.
Embodiment 5
Described enzymolysis solution is the prozyme of cellulase, amylase, proteolytic enzyme, lipase and N,O-Diacetylmuramidase, and the ratio of five kinds of enzymes is 3: 2: 2: 2: 1.Enzymolysis time is 6 hours, and hydrolysis temperature is 40 ℃.
Embodiment 6-13
Described enzymolysis solution is the combination of the prozyme following table ratio of cellulase, amylase, proteolytic enzyme, lipase and N,O-Diacetylmuramidase; Hydrolysis temperature, enzymolysis time are also as shown in the table, and all the other are with embodiment 2.
| Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 | Embodiment 12 | Embodiment 13 | |
| Cellulase | ??1 | ??1 | ??1 | ??1 | ??1 | ??1 | ??1 | ??1 |
| Amylase | ??0.7 | ??0.5 | ??0 | ??0 | ??0.6 | ??0.3 | ??0.1 | ??0 |
| Proteolytic enzyme | ??0.7 | ??0.6 | ??0 | ??0 | ??0.5 | ??0.3 | ??0 | ??0 |
| Lipase | ??0.7 | ??0 | ??0.5 | ??0 | ??0.6 | ??0.2 | ??0 | ??0.1 |
| N,O-Diacetylmuramidase | ??0.3 | ??0 | ??0 | ??0.5 | ??0.2 | ??0 | ??0.4 | ??0 |
| Hydrolysis temperature ℃ | ??15 | ??30 | ??40 | ??45 | ??50 | ??70 | ??35 | ??60 |
| Enzymolysis time h | ??2 | ??24 | ??12 | ??3 | ??4 | ??5 | ??3.5 | ??4.5 |
Claims (8)
1. the extracting method of a trans-resveratrol, it is characterized in that: described technology is as follows:
The giant knotweed starting material are through pre-treatment, after dust is fallen in drip washing, cut into slices or make meal, add alcohol heating reflux and extract, and ethanol is reclaimed in the extracting solution underpressure distillation, and be concentrated into the thick paste shape, and dilute with water 5-15 doubly and adds the enzymolysis solution enzymolysis.Enzymolysis solution heating suction filtration with enzymolysis after good, and through activated carbon decolorizing with alcohol recrystallization repeatedly, can get purity at the white solid trans-resveratrol more than 98% behind the last drying under reduced pressure again.
2. the extracting method of a kind of trans-resveratrol as claimed in claim 1, it is characterized in that: described technology is as follows:
After 1 part of raw material drip washing fallen dust, to be cut into thickness be the sheet of 0.5-3mm or make meal, stand-by; With starting material giant knotweed section or make meal refluxing extraction is more than 2 times in advance with the ethanol of 70-80%, amount of alcohol is respectively starting material more than 1 times, preferred 2-3 doubly, return time 1-2.5h, united extraction liquid is concentrated into amalgamation liquid the thick paste shape again; Add 5-15 times of water to heavy paste extract, and add 0.01-0.05 part enzyme, described enzyme is a cellulase, or prozyme, and described prozyme is any one or a multiple mixture in cellulase and distiller's yeast, amylase, proteolytic enzyme, lipase, the N,O-Diacetylmuramidase; Cellulase and distiller's yeast, amylase, proteolytic enzyme, lipase, N,O-Diacetylmuramidase are according to Mass Calculation, and ratio is 1: 0-2: 0-0.5: 0-1: 0-1: 0-0.5; Enzymolysis time is 2-24 hour, and hydrolysis temperature is 15-70 ℃;
Purifying: enzymolysis solution is heated to 80 ℃ of suction filtrations while hot, and uses activated carbon decolorizing, get crude product; Recrystallization 2-5 time must elaboration repeatedly by ethanol with crude product; Get finished product behind the elaboration drying under reduced pressure.
3. the extracting method of a kind of trans-resveratrol as claimed in claim 2, it is characterized in that: in the described prozyme, cellulase and distiller's yeast, amylase, proteolytic enzyme, lipase, N,O-Diacetylmuramidase are according to Mass Calculation, and ratio is 1: 1: 0.3-0.4: 0.5-0.6: 0.5-0.7: 0.2-0.3.
4. the extracting method of a kind of trans-resveratrol as claimed in claim 2, it is characterized in that: described proteolytic enzyme is aspartic protease.
5. the extracting method of a kind of trans-resveratrol as claimed in claim 2, it is characterized in that: comprise cellulase and distiller's yeast in the described prozyme, mass ratio is 1: 1.
6. the extracting method of a kind of trans-resveratrol as claimed in claim 2, it is characterized in that: comprise cellulase, amylase, three kinds of enzymes of aspartic protease in the described prozyme, the ratio of three kinds of enzymes is 1: 2: 3 or 2: 3: 5.
7. the extracting method of a kind of trans-resveratrol as claimed in claim 2 is characterized in that: describedly comprise cellulase, amylase, proteolytic enzyme, lipase and N,O-Diacetylmuramidase in compound, the ratio of five kinds of enzymes is 3: 2: 2: 2: 1.
8. the extracting method of a kind of trans-resveratrol as claimed in claim 2 is characterized in that: described enzymolysis time 4-6 hour, and hydrolysis temperature 40-50 ℃.
Priority Applications (1)
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| CN200910162072A CN101628859A (en) | 2009-08-11 | 2009-08-11 | Extraction method of resveratrol |
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| CN200910162072A CN101628859A (en) | 2009-08-11 | 2009-08-11 | Extraction method of resveratrol |
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Cited By (3)
| 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 |
| 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 |
| CN107721825A (en) * | 2017-10-18 | 2018-02-23 | 洋县秦龙药业有限公司 | A kind of method that resveratrol and Polydatin are extracted from giant knotweed |
Citations (3)
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| CN1251361A (en) * | 1999-09-24 | 2000-04-26 | 四川省凉山州生物研究所 | Process for extracting resveratrol from Chinese medicine giant knotweed root |
| CN1566349A (en) * | 2003-06-26 | 2005-01-19 | 中国医药研究开发中心有限公司 | Method for preparing resveratrol from giant knotweed |
| 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 |
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2009
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1251361A (en) * | 1999-09-24 | 2000-04-26 | 四川省凉山州生物研究所 | Process for extracting resveratrol from Chinese medicine giant knotweed root |
| CN1566349A (en) * | 2003-06-26 | 2005-01-19 | 中国医药研究开发中心有限公司 | Method for preparing resveratrol from giant knotweed |
| 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 |
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| 兰天路: "虎杖中白藜芦醇提取工艺研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
| 向海艳: "虎杖中白藜芦醇的分离纯化研究", 《中国优秀博硕士学位论文全文数据库(博士)工程科技I辑》 * |
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Cited By (4)
| 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 |
| 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 |
| CN107721825A (en) * | 2017-10-18 | 2018-02-23 | 洋县秦龙药业有限公司 | A kind of method that resveratrol and Polydatin are extracted from giant knotweed |
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