CN101602652A - A kind of method of from moraceae plants, extracting trans-resveratrol - Google Patents
A kind of method of from moraceae plants, extracting trans-resveratrol Download PDFInfo
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- CN101602652A CN101602652A CNA2009101005247A CN200910100524A CN101602652A CN 101602652 A CN101602652 A CN 101602652A CN A2009101005247 A CNA2009101005247 A CN A2009101005247A CN 200910100524 A CN200910100524 A CN 200910100524A CN 101602652 A CN101602652 A CN 101602652A
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- resveratrol
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Abstract
The present invention relates to the extracting method of trans-resveratrol, aim to provide a kind of method of from moraceae plants, extracting trans-resveratrol.Comprise: raw material chooses, broken, alcohol solvent extracts and purifying, and purifying is with polar macroporous adsorption resin chromatography column absorption on the extracting solution, with collecting elutriant behind the alcohol solvent wash-out, carries out vacuum concentration, drying then, obtains the trans-resveratrol product.The chemical reagent that uses in present method preparation process is simple, only is ethanol; Because the material that uses in the leaching process is also very simple, therefore avoided risk because of using number of chemical reagent to bring.As adopt the method for two kinds of macroporous adsorbent resin couplings, and can significantly reduce the link of technological process, simple to operate and be convenient to control.As will further improving the Resveratrol content of sample, can reach 98% resveratrol recrystallized product just can obtain content by suitable concentrating and placing.
Description
Technical field
The present invention relates to the extracting method of trans-resveratrol, be specifically related to a kind of method of from moraceae plants, extracting trans-resveratrol.
Background technology
Trans-resveratrol is as a kind of natural polyphenol compounds, demonstrate multiple biological activity, be a kind of natural material, be widely used in fields such as medicines and health protection with functions such as antitumor, anti-cardiovascular disease, anti-mutation, antibiotic, anti-inflammatory, anti-oxidant, cell death inducing and estrogen regulating.
Trans-resveratrol is main at present to be passed through from some Chinese medicinal materials, as extracting in the giant knotweed.Extract trans-resveratrol at present from giant knotweed, most organic solvents that adopt as extractions such as acetone, ethyl acetate, are used silica gel purification, again by methods such as recrystallizations, obtain the higher trans-resveratrol product of purity with this.The method that has is also added zymin and alkaline reagents.But these method complex process, cycle are long, need in the process to add number of chemical and biological reagent, and operation is too much, have increased production cost and to the occupancy of equipment.
Therefore, excavate other Biological resources and to study its extraction process significant.Discover that trans-resveratrol also has existence in Sang Ziyuan.China is the relatively abundanter country of Sang Ziyuan, therefore extracts trans-resveratrol from moraceae plants, and is all significant from utilization of resources angle and economic aspect.
Summary of the invention
Problem to be solved by this invention is to overcome deficiency of the prior art exactly, and a kind of method of extracting trans-resveratrol from moraceae plants is provided.
For realizing goal of the invention, technical scheme provided by the invention may further comprise the steps:
(1) raw material is chosen: select to contain the moraceae plants of trans-resveratrol for extracting raw material;
(2) fragmentation: with the raw material Mechanical Crushing;
(3) extract: the raw material after the fragmentation is added 15～25Kg/L alcohol solvent doubly, extract 60～120 minutes after-filtration under little condition of boiling, getting filtrate is extracting solution;
(4) purifying: with polar macroporous adsorption resin chromatography column absorption on the extracting solution,, carry out vacuum concentration, drying then, obtain the trans-resveratrol product with collecting elutriant behind the alcohol solvent wash-out.
As a kind of improvement, described step (4) comprises utilizes polar macroporous adsorption resin to carry out the process of twice absorption and wash-out: the elutriant after the absorption is gone up second kind of polar macroporous adsorption resin absorption more for the first time, secondary elutriant carries out vacuum concentration, drying, obtains the trans-resveratrol product; In two kinds of macroporous adsorbent resins, first kind of macroporous adsorbent resin is low-pole or nonpolar resin, and second kind of macroporous adsorbent resin is Semi-polarity or polar resin.By this step, can obtain purity and reach trans-resveratrol product more than 92%.
As a kind of improvement, described step (4) comprises utilizes polar macroporous adsorption resin to carry out the process of twice absorption and wash-out: the elutriant after the absorption is gone up second kind of polar macroporous adsorption resin absorption more for the first time, secondary elutriant concentrates and low temperature is placed crystallization, obtains the resveratrol recrystallized product; In two kinds of macroporous adsorbent resins, first kind of macroporous adsorbent resin is low-pole or nonpolar resin, and second kind of macroporous adsorbent resin is Semi-polarity or polar resin.By this step, can obtain purity and reach resveratrol recrystallized product more than 98%.
As a kind of improvement, be in Ramulus Mori, mulberry leaf, Fructus Mori juice or the sorosis skin any one as the moraceae plants that extracts raw material.
As a kind of improvement, the machinery that is used for raw material crushing is that hammer is pulverized or the chip crusher.
As a kind of improvement, described alcohol solvent is the alcoholic acid aqueous solution, and its concentration is 60～80%.
As a kind of improvement, described spissated method is to add that normal temperature and pressure concentrates or heating vacuum concentrates.
As a kind of improvement, described exsiccant method is a kind of in heat drying, heating vacuum drying, lyophilize or the seasoning.
As a kind of improvement, described crystalline method is crystallizing at room temperature or low temperature crystallization.
Beneficial effect of the present invention is:
The chemical reagent that uses in present method preparation process is simple, only is ethanol; Because the material that uses in the leaching process is also very simple, therefore avoided risk because of using number of chemical reagent to bring.
As adopt the method for two kinds of macroporous adsorbent resin couplings, and can significantly reduce the link of technological process, simple to operate and be convenient to control.As will further improving the Resveratrol content of sample, can reach 98% resveratrol recrystallized product just can obtain content by suitable concentrating and placing.
Embodiment
Macroporous resin (macroporous resin) claim full porous resin again, polymer absorbant, it be a class to be adsorbed as characteristics, organism is had high molecular polymer concentrated, centrifugation.Macroporous resin is to be prepared from through polyreaction by additives such as polymerization single polymerization monomer and linking agent, pore-creating agent, dispersion agents.Behind the polymer formation, pore-creating agent is removed, and has stayed hole big and small, different, that interpenetrate in resin.Therefore macroporous resin its inside under drying regime has higher porosity, and the aperture is bigger, between 100-1000nm, so be called macroporous adsorbent resin.Macroporous adsorbent resin is different with selected monomer molecule structure by its polarity size, can be divided into nonpolar, Semi-polarity and polarity three classes.General absorption with macroporous adsorbent resin meets following rule: apolar substance is adsorbed by non-polar adsorbent in polarizable medium (water), polar material is adsorbed by polar adsorbent in nonpolar medium, can good adsorption of polar compounds in non-polar solvent with the sorbent material of strong polar group.
Macroporous adsorbent resin is for absorption and screen the parting material that principle combines.Its adsorptivity is because the result of Van der Waals force or generation hydrogen bond.The screening principle is because itself cellular structure determines.Because absorption and screening principle, organic compound separates through certain solvent elution on macroporous absorption fat according to the difference of adsorptive power and the size of molecular weight.This make organic compound especially the purification of water-soluble cpds simplified greatly.
Trans-resveratrol contains 3 hydroxyls, it is a kind of polyphenolic compound, has stronger polarity, it is soluble in the strong solvent of polarity, it has bigger solubleness in concentration is 60～80% ethanolic soln, therefore, can extract trans-resveratrol in the moraceae plants raw material with 60～80% ethanol to greatest extent as solvent.
Present method is selected polar macroporous adsorption resin for use, helps adsorbing the more intense trans-resveratrol of polarity, uses the stronger ethanol of same polarity easily as eluent then, helps the wash-out of trans-resveratrol.Present method is by the gradient concentration elution method, collect the elutriant of 60% and 80% alcohol concn, can obtain content and reach 50%, in order to obtain the trans-resveratrol of greater concn, present method has adopted the method for 2 kinds of resin couplings, promptly behind a kind of macroporous adsorbent resin, and the another kind of macroporous adsorbent resin of having connected, by the purifying of these 2 kinds of macroporous adsorbent resins, obtain content at once and be not less than 92% trans-resveratrol sample.
Example 1:
Get the dried Ramulus Mori of 1000g, be chopped into 1 * 0.5cm with machinery
2Fragment places the stainless steel extractor, adds 80% aqueous ethanolic solution 15L, heats and boils to little, keeps little little stirring of boiling to extract 1h.After extraction is finished, filter with 200 order filter clothes, after filtrate suitably concentrates, with macroporous adsorbent resin (D101 or AB-8 etc.) column chromatography purification, treat that the whole upper props of solution finish after, keep leaving standstill 20 to 30min, use eluent (60% aqueous ethanolic solution) wash-out then, collect elutriant, concentrate drying just can obtain content and be 50% trans-resveratrol sample.
Example 2:
Get the dried mulberry leaf of 1000g, be broken into 1 * 1cm with pulverizer
2Fragment places the stainless steel extractor, adds 60% aqueous ethanolic solution 20L, heats and boils to little, keeps little little stirring of boiling to extract 1.5h.After extraction is finished, filter with 200 order filter clothes, after filtrate suitably concentrates, cross the 1st macroporous adsorbent resin (AB-8 or D101 etc.) chromatography column earlier, after treating that the whole upper props of solution finish, keep leaving standstill 20 to 30min, use eluent (70% aqueous ethanolic solution) wash-out then, collect elutriant, this elutriant is crossed the 2nd macroporous adsorbent resin (DM130 or HPD-500 etc.) chromatography column, treat that the whole upper props of solution finish after, keep leaving standstill 20 to 30min, use eluent (70% aqueous ethanolic solution) wash-out then, collect elutriant, behind the concentrate drying, just can obtain the trans-resveratrol of higher degree, measure through HPLC, its content reaches 92%.
Example 3:
Get the dried sorosis skin of 1000g, place the stainless steel extractor, add 75% aqueous ethanolic solution 25L, heat and boil, keep little little stirring of boiling to extract 2h to little.After extraction is finished, filter with 200 order filter clothes, after filtrate suitably concentrates, cross earlier the 1st macroporous adsorbent resin (AB-8 or D101 etc.) chromatography column, treat that the whole upper props of solution finish after, keep leaving standstill 20 to 30min, use eluent (80% aqueous ethanolic solution) wash-out then, collect elutriant, this elutriant is crossed the 2nd macroporous adsorbent resin (DM130 or HPD-500 etc.) chromatography column, treat that the whole upper props of solution finish after, keep leaving standstill 20 to 30min, use eluent (80% aqueous ethanolic solution) wash-out then, collect elutriant, after concentrating, placement is spent the night, just can obtain resveratrol recrystallized, detect through HPLC, its Resveratrol content is 98%.
Claims (9)
1, a kind of method of extracting trans-resveratrol from moraceae plants may further comprise the steps:
(1) raw material is chosen: select to contain the moraceae plants of trans-resveratrol for extracting raw material;
(2) fragmentation: with the raw material Mechanical Crushing;
(3) extract: the raw material after the fragmentation is added 15～25 Kg/L alcohol solvent doubly, extract 60～120 minutes after-filtration under little condition of boiling, getting filtrate is extracting solution;
(4) purifying: with polar macroporous adsorption resin chromatography column absorption on the extracting solution,, carry out vacuum concentration, drying then, obtain the trans-resveratrol product with collecting elutriant behind the alcohol solvent wash-out.
2, the method for from moraceae plants, extracting trans-resveratrol according to claim 1, it is characterized in that, described step (4) comprises utilizes polar macroporous adsorption resin to carry out the process of twice absorption and wash-out: the elutriant after the absorption is gone up second kind of polar macroporous adsorption resin absorption more for the first time, secondary elutriant carries out vacuum concentration, drying, obtains the trans-resveratrol product; In two kinds of macroporous adsorbent resins, first kind of macroporous adsorbent resin is low-pole or nonpolar resin, and second kind of macroporous adsorbent resin is Semi-polarity or polar resin.
3, the method for from moraceae plants, extracting trans-resveratrol according to claim 1, it is characterized in that, described step (4) comprises utilizes polar macroporous adsorption resin to carry out the process of twice absorption and wash-out: the elutriant after the absorption is gone up second kind of polar macroporous adsorption resin absorption more for the first time, secondary elutriant concentrates and low temperature is placed crystallization, obtains the resveratrol recrystallized product; In two kinds of macroporous adsorbent resins, first kind of macroporous adsorbent resin is low-pole or nonpolar resin, and second kind of macroporous adsorbent resin is Semi-polarity or polar resin.
4, extracting the method for trans-resveratrol according to described any one of claim 1 to 3 from moraceae plants, it is characterized in that, is in Ramulus Mori, mulberry leaf, Fructus Mori juice or the sorosis skin any one as the moraceae plants that extracts raw material.
5, extract the method for trans-resveratrol according to described any one of claim 1 to 3 from moraceae plants, it is characterized in that, the machinery that is used for raw material crushing is that hammer is pulverized or the chip crusher.
6, extract the method for trans-resveratrol according to described any one of claim 1 to 3 from moraceae plants, it is characterized in that described alcohol solvent is an aqueous ethanolic solution, its concentration is 60～80%.
7, extract the method for trans-resveratrol according to described any one of claim 1 to 3 from moraceae plants, it is characterized in that, described spissated method is to add that normal temperature and pressure concentrates or heating vacuum concentrates.
8, extract the method for trans-resveratrol according to described any one of claim 1 to 3 from moraceae plants, it is characterized in that, described exsiccant method is a kind of in heat drying, heating vacuum drying, lyophilize or the seasoning.
9, the method for extracting trans-resveratrol from moraceae plants according to claim 3 is characterized in that described crystalline method is crystallizing at room temperature or low temperature crystallization.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2009101005247A CN101602652A (en) | 2009-07-09 | 2009-07-09 | A kind of method of from moraceae plants, extracting trans-resveratrol |
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| CNA2009101005247A CN101602652A (en) | 2009-07-09 | 2009-07-09 | A kind of method of from moraceae plants, extracting trans-resveratrol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408893A (en) * | 2011-09-21 | 2012-04-11 | 浙江大学 | Preparation method of mulberry twig antioxidant |
| CN104163754A (en) * | 2014-07-18 | 2014-11-26 | 苏州市职业大学 | Method for extraction and separating of high purity resveratrol from peanut root |
| CN105754002A (en) * | 2016-04-29 | 2016-07-13 | 江苏耐雀生物工程技术有限公司 | Preparation method of high-content tremella polysaccharide |
-
2009
- 2009-07-09 CN CNA2009101005247A patent/CN101602652A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 占鹏飞 等: "桑树各部位中白藜芦醇的提取与测定", 《桑蚕通报》 * |
| 姜瑞清等: "白藜芦醇分离纯化及检测技术研究进展", 《中药材》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408893A (en) * | 2011-09-21 | 2012-04-11 | 浙江大学 | Preparation method of mulberry twig antioxidant |
| CN104163754A (en) * | 2014-07-18 | 2014-11-26 | 苏州市职业大学 | Method for extraction and separating of high purity resveratrol from peanut root |
| CN105754002A (en) * | 2016-04-29 | 2016-07-13 | 江苏耐雀生物工程技术有限公司 | Preparation method of high-content tremella polysaccharide |
| CN105754002B (en) * | 2016-04-29 | 2018-06-12 | 江苏耐雀生物工程技术有限公司 | A kind of preparation method of high content silver fungus polysaccharides |
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Application publication date: 20091216 |