CN101397242A - Technique for extracting and purifying resveratrol from fresh giant knotweed rhizome - Google Patents
Technique for extracting and purifying resveratrol from fresh giant knotweed rhizome Download PDFInfo
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- CN101397242A CN101397242A CNA2007100306017A CN200710030601A CN101397242A CN 101397242 A CN101397242 A CN 101397242A CN A2007100306017 A CNA2007100306017 A CN A2007100306017A CN 200710030601 A CN200710030601 A CN 200710030601A CN 101397242 A CN101397242 A CN 101397242A
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- giant knotweed
- resveratrol
- ethanol
- silica gel
- thick paste
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process method for extracting and purifying resveratrol from fresh giant knotweed rhizome, the process method is characterized in that the process method comprises the following steps: the collected fresh giant knotweed rhizome is cleaned, air-dried, cut into slices and weighed; ethanol with the weight which is 4 to 8 times of the weight of the giant knotweed rhizome and the concentration of 60 percent to 85 percent is added, the soaking and the extraction are carried out for 24 hours at 30 DEG C to 60 DEG C, extract liquid is collected and filtered; the secondary extraction is carried out by using the same method, filtrate is combined, the pressure is reduced as far as possible and a thick paste is obtained by evaporation, 4 times of inactivated silica gel with 70 to 140 meshes is added and evenly stirred with the thick paste, the blow drying by cold air is carried out, the chromatography is carried out by 6 times of the sample amount of the silica gel with 70 to 140 meshes, ethanol-ethyl acetate-petroleum ether is used for elution at the temperature of 60 to 90 DEG C, the part containing the resveratrol is guided to merge by using the thin layer chromatography result, the pressure is reduced, the solvent is recycled, a crude solid is obtained, and a pure resveratrol needle-like crystal is obtained by recrystallization in ethanol. The process method has simple manufacturing process, easy realization, low production cost and high product purity.
Description
Technical field
The present invention relates to a kind of extraction, purification process of chemical composition of Chinese materia medica, particularly a kind ofly from fresh giant knotweed, extract, the processing method of purified resveratrol.
Background technology
Trans-resveratrol has blood fat reducing, anticoagulant, antitumor, anti-ageing, protection cardiovascular systems, the effectively effect of preventing cancer, and its medical value and health care are worth and have obtained globally generally acknowledging.
Facts have proved that trans-resveratrol many forms with glycosides in the Chinese medicinal materials giant knotweed exist, and the small-amount free trans-resveratrol is arranged and deposit, is the important activity composition of giant knotweed, need pass through certain processing method but want to extract highly purified trans-resveratrol from giant knotweed.Through looking into new discovery, China Patent No. is: 200610031850,3 disclose " the microbial transformation giant knotweed materials extracts the technology of high-purity trans-resveratrol ", its characteristics are: microorganisms such as its elder generation's employing yeast carry out bio-transformation to giant knotweed materials, make the giant knotweed resveratrol analogs be converted into trans-resveratrol, add a certain proportion of ethanol and hydrocarbon alcohol again, utilize microwave low temperature to extract, concentrate after filtration trans-resveratrol.
More than disclosed patent be that to adopt drying giant knotweed be raw material, need carry out bio-transformation to giant knotweed materials with microorganism, and with method assisted extraction such as ultra-sonic oscillation, microwave treatment, this class methods technological operation is complicated, the cycle is long, trans-resveratrol purity that extracted is not high.
Summary of the invention
The objective of the invention is to solve the prior art deficiency, provide a kind of production cost processing method low, extraction, purification of high-purity trans-resveratrol in fresh giant knotweed.
Technical scheme of the present invention is achieved in that and a kind ofly extracts from fresh giant knotweed, the processing method of purified resveratrol may further comprise the steps:
(1), fresh giant knotweed is cleaned, dries, is thinly sliced, weighing gathering;
(2), add suitable giant knotweed weight 4-8 60%-85% ethanol doubly, soak down at 30 ℃-60 ℃ and extracted 24 hours, collect extracting solution, and filter;
(3), extract once more once with above-mentioned same procedure, merging filtrate, decompression is steamed to thick paste as far as possible;
(4), the gained thick paste is carried out silica gel column chromatography, to separate and purified resveratrol: mix thoroughly with 4 times of 70-140 order inactivation silica gel and thick paste, cold wind dries up, 70-140 order silica gel with 6 times of sample sizes carry out chromatography, with ethanol-ethyl acetate-sherwood oil wash-out under 60-90 ℃ temperature, instruct merging to contain trans-resveratrol part, decompression and solvent recovery with the tlc analysis result, get thick solid, ethyl alcohol recrystallization gets pure white veratryl alcohol needle-like crystal.
The optimum concn of alcoholic acid is 80% in the step of the present invention (2), extracts 5h down at 60 ℃.
The invention has the advantages that: 1, with fresh giant knotweed as raw material, the trans-resveratrol of the unbound state in the giant knotweed and glycoside are not destroyed, improve the extraction yield of trans-resveratrol; 2, owing in fresh giant knotweed, add dissolve with ethanol, can effectively isolate trans-resveratrol and resveratrol analogs, this technological operation is simple, at the bottom of the extraction cost; 3, adopt silica gel column chromatography,, promptly get purity greater than 95% trans-resveratrol product, its separation, purification effect ideal with ethanol-ethyl acetate-sherwood oil wash-out.
Specific implementation method
Clean gathering fresh giant knotweed, dry, thinly slice, take by weighing 500g, adding 3000g concentration is 80% ethanol, under 60 ℃ temperature, soak and extracted 5 hours, collect extracting solution, filter, extract once more once with identical method again, merging filtrate steams the filtrate after merging to thick paste, mixes thoroughly with 4 times of 70-140 order inactivation silica gel and thick paste, cold wind dries up, 70-140 order silica gel with 6 times of sample sizes carry out chromatography, with ethanol-ethyl acetate-sherwood oil wash-out under 75 ℃ temperature, separate out white, needle-shaped crystals, filtration obtains crystallization, instruct merging to contain the trans-resveratrol part with the tlc analysis result, decompression and solvent recovery gets thick solid, ethyl alcohol recrystallization gets pure white veratryl alcohol needle-like crystal, promptly gets purity greater than 95% trans-resveratrol product.
Claims (2)
- One kind from fresh giant knotweed, extract, the processing method of purified resveratrol, it is characterized in that may further comprise the steps:(1), fresh giant knotweed is cleaned, dries, is thinly sliced, weighing gathering;(2), add suitable giant knotweed weight 4-8 60%-85% ethanol doubly, soak down at 30 ℃-60 ℃ and extracted 24 hours, collect extracting solution, and filter;(3), extract once more once with above-mentioned same procedure, merging filtrate, decompression is steamed to thick paste as far as possible;(4), the gained thick paste is carried out silica gel column chromatography, to separate and purified resveratrol.Mix thoroughly with 4 times of 70-140 order inactivation silica gel and thick paste, cold wind dries up, 70-140 order silica gel with 6 times of sample sizes carry out chromatography, with ethanol-ethyl acetate-sherwood oil wash-out under 60-90 ℃ temperature, instruct merging to contain the trans-resveratrol part with the tlc analysis result, decompression and solvent recovery gets thick solid, and ethyl alcohol recrystallization gets pure white veratryl alcohol needle-like crystal.
- 2. according to claim 1ly from fresh giant knotweed, extract, the processing method of purified resveratrol, it is characterized in that it is 80% ethanol that step (2) adds 4-8 times of concentration of suitable giant knotweed weight, extracts 5h down at 60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100306017A CN101397242A (en) | 2007-09-28 | 2007-09-28 | Technique for extracting and purifying resveratrol from fresh giant knotweed rhizome |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100306017A CN101397242A (en) | 2007-09-28 | 2007-09-28 | Technique for extracting and purifying resveratrol from fresh giant knotweed rhizome |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101397242A true CN101397242A (en) | 2009-04-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007100306017A Pending CN101397242A (en) | 2007-09-28 | 2007-09-28 | Technique for extracting and purifying resveratrol from fresh giant knotweed rhizome |
Country Status (1)
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| CN (1) | CN101397242A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102925497A (en) * | 2012-11-01 | 2013-02-13 | 恩施清江生物工程有限公司 | Method for preparing high-purity resveratrol from polygonum cuspidatum |
| CN104026159A (en) * | 2014-07-08 | 2014-09-10 | 山东农业大学 | Preparing method for botanical pesticides |
| CN108383691A (en) * | 2018-01-23 | 2018-08-10 | 湖北未来家园高科技农业股份有限公司 | A method of extracting resveratrol from giant knotweed |
-
2007
- 2007-09-28 CN CNA2007100306017A patent/CN101397242A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102925497A (en) * | 2012-11-01 | 2013-02-13 | 恩施清江生物工程有限公司 | Method for preparing high-purity resveratrol from polygonum cuspidatum |
| CN104026159A (en) * | 2014-07-08 | 2014-09-10 | 山东农业大学 | Preparing method for botanical pesticides |
| CN104026159B (en) * | 2014-07-08 | 2016-03-30 | 山东农业大学 | A kind of preparation method of plant insecticide |
| CN108383691A (en) * | 2018-01-23 | 2018-08-10 | 湖北未来家园高科技农业股份有限公司 | A method of extracting resveratrol from giant knotweed |
| CN108383691B (en) * | 2018-01-23 | 2021-03-02 | 湖北未来家园高科技农业股份有限公司 | Method for extracting resveratrol from giant knotweed rhizome |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090401 |