CN104030895A - Method for preparing resveratrol and viniferin from waste grape vine branches and tendrils - Google Patents
Method for preparing resveratrol and viniferin from waste grape vine branches and tendrils Download PDFInfo
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- CN104030895A CN104030895A CN201410238415.2A CN201410238415A CN104030895A CN 104030895 A CN104030895 A CN 104030895A CN 201410238415 A CN201410238415 A CN 201410238415A CN 104030895 A CN104030895 A CN 104030895A
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- resveratrol
- tendrils
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- grape vine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/004—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D307/78—Benzo [b] furans; Hydrogenated benzo [b] furans
- C07D307/82—Benzo [b] furans; Hydrogenated benzo [b] furans with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to carbon atoms of the hetero ring
- C07D307/83—Oxygen atoms
Abstract
The invention discloses a method for preparing resveratrol and viniferin from waste grape vine branches and tendrils obtained through pruning in autumn. The method comprises the steps: with fresh grape branches and tendrils obtained through pruning as raw materials, storing in a shady, cool and dark place, detecting contents of resveratrol and viniferin on time, after a given period, performing ultrasonic-assisted extraction, and performing adsorption separation through macroreticular resin to respectively obtain resveratrol and viniferin products. The yield of the obtained resveratrol reaches 1.1 percent, the content of the resveratrol reaches above 22 percent, the yield of the viniferin reaches 1.0 percent, and the content of the viniferin reaches above 20 percent. The method is capable of remarkably increasing the contents of the resveratrol and the viniferin in grape vines, low in energy consumption, high in separation efficiency, free from using an organic solvent, capable of recycling waste materials so that the environment pollution is reduced, simple in process and suitable for industrialized product.
Description
Technical field
The present invention relates to a kind of method of preparing trans-resveratrol and grape element from useless grape vine branches and tendrils, especially relate to a kind of starting material pre-treatment processing technology and in conjunction with macroporous adsorbent resin isolation technique, from the useless branches and tendrils of fresh grape rattan, prepare the method for trans-resveratrol and grape element simultaneously.
Background technology
Trans-resveratrol is found to be present in each position of grapevine seedling in recent years, at aspects such as disease resistance of plant, human cardiovascular disease and cancer preventions, all shows excellent characteristic.The dipolymer grape element of trans-resveratrol, aspect anti-inflammatory, antibacterial, anticancer, anti-oxidant, preventing cardiovascular disease, is proved to be and has the activity similar to trans-resveratrol, even also high than the activity of trans-resveratrol.Because (leaf, really) trans-resveratrol and grape cellulose content in grapevine seedling are lower, the content of 5/1000000ths left and right only, cost of development is very high, and trans-resveratrol product is mainly derived from medicinal plant giant knotweed in the market.Owing to deriving from the Coexisting component that contains certain toxic side effect in the trans-resveratrol product of giant knotweed, the closeer trans-resveratrol product that derives from grape of looking at of European & American Market, the trans-resveratrol product price that derives from grape also wants high a lot.In viticulture process, in order to improve vintage, the grape vine branches and tendrils that need to prune away a large amount of in autumn and winter every year, the grape vine shearing off branches and tendrils are generally all to take the way of burning on the spot to process, and have caused the pollution of ecotope and the serious waste of resource.The useless branches and tendrils of grape vine that obtain after finding after deliberation to take suitable pre-treating process to beta pruning are processed, and can significantly improve the wherein content of trans-resveratrol and grape element, reach the needs of suitability for industrialized production.Ultrasonic wave auxiliary extraction has the advantages such as extraction efficiency is high, speed is fast, price is low, macroporous adsorbent resin, owing to having the features such as rate of adsorption is fast, selectivity good, manipulation of regeneration is convenient, life cycle is long, is applied and is more and more applied in the extraction separation of herbal medicine activeconstituents.
Present method is carried out pre-treatment processing to useless grape vine branches and tendrils, separated with macroporous adsorbent resin in conjunction with ultrasonic-assisted extraction, obtains trans-resveratrol and grape element product from beta pruning the useless grape branches and tendrils that obtain.Present method provides a kind of new material source for trans-resveratrol and grape element product, has set up the trans-resveratrol in a grape source and quick, efficient, the economic preparation method of grape element simultaneously.
Summary of the invention
The invention provides a kind of method of preparing trans-resveratrol and grape element from useless grape vine branches and tendrils.The method takes the grape vine branches and tendrils that pre-treatment working method obtains new beta pruning to carry out pre-treatment, significantly improve the content of activeconstituents trans-resveratrol and grape element in grape vine branches and tendrils, take ultrasonic wave auxiliary extraction technology to extract grape vine branches and tendrils, obtain trans-resveratrol and grape element crude extract, select again macroporous adsorbent resin to adsorb, with the ethanol of different concns, carry out wash-out, obtain respectively trans-resveratrol and grape element product.The method adopts pretreatment technology pre-treatment grape vine branches and tendrils, can significantly improve trans-resveratrol and grape cellulose content, and trans-resveratrol and grape element extraction and separation method are simple to operate, pollution-free.The rate of the trans-resveratrol that the method obtains and grape element product is high, and content is high.
The object of the invention is to be achieved through the following technical solutions.
It comprises the steps: the pre-treatment of (1) grape vine branches and tendrils: the useless branch of the grape vine under new beta pruning in autumn is positioned over to the indoor preservation 60-90 days of shady and cool dry, dark lucifuge, during in 10 days sampling and measuring grape vine branches and tendrils trans-resveratrol and grape cellulose content.When Resveratrol content surpasses 1.0%, grape vine branches and tendrils are shredded or to be ground into meal stand-by.(2) ultrasonic-assisted extraction: take a certain amount of grape vine branches and tendrils meal, the distilled water that adds 2-5 doubly to measure, after soaking, ultrasonic 30 minutes.Then add 5-10 times of edible ethanol, refluxing extraction 1-2h in multi-function extractor, filter-cloth filtering obtains extracting solution, and grape vine branches and tendrils residue repeats to extract 1 time, united extraction liquid, high speed centrifugation, gets supernatant liquor standby.(3) concentration and recovery solvent: vacuum-concentrcted reclaims ethanol, obtains grape vine branches and tendrils crude extract by medicinal extract vacuum-drying.(4) macroporous adsorbent resin is separated: select low-pole or nonpolar macroporous adsorption resin as D101, AB-8 etc., resin is carried out to pre-treatment, abundant swelling, removal be contained unpolymerized organic solvent wherein.Macroporous adsorbent resin is seated in glass column or stainless steel pillar, by grape vine branches and tendrils crude extract adding distil water heating for dissolving, wet method loading, thin-layer chromatography detects effluent liquid trans-resveratrol and grape cellulose content simultaneously, until adsorb saturated.The extracting solution not being adsorbed with 2 times of BV/h speed wash-outs with the distilled water of 1 times of bed volume (BV) adsorbing saturated macroporous adsorptive resins, then with 50% the ethanol of 3BV with 2BV/h speed wash-out, collect elutriant, and then with 70% the ethanol of 3BV with 2BV/h speed wash-out, collect elutriant.(5) the elutriant concentrating under reduced pressure 50% ethanol elution being obtained, reclaims ethanol, and the medicinal extract obtaining is carried out to vacuum-drying, obtain trans-resveratrol product, the elutriant concentrating under reduced pressure that 70% ethanol elution is obtained, reclaims ethanol, the medicinal extract obtaining is carried out to vacuum-drying, obtain grape element product.
The trans-resveratrol preparing through method of the present invention and grape element, trans-resveratrol yield is more than 1.1, and content can reach more than 25%, and grape element yield is 1.0, and content can reach more than 20%, and two kinds of product recovery rates all reach more than 85%.
In a word, advantage of the present invention is: can significantly improve trans-resveratrol and the content of grape element in grape vine branches and tendrils, and obtain trans-resveratrol and the grape element product in grape source simultaneously.Adopt pre-treatment processing to process fresh grape vine branches and tendrils, effectively raise the content of trans-resveratrol and grape element, the useless branch of grape vine that autumn and winter beta pruning is abandoned becomes the raw material that obtains trans-resveratrol and grape element product, turns waste into wealth, and has also reduced the pollution of environment simultaneously.The present invention adopts ultrasonic-assisted extraction and macroporous adsorbent resin isolation technique to prepare trans-resveratrol and grape element, and extraction efficiency is high, does not use noxious solvent, is the extraction process of environmental protection, and preparation technology is simple, and cost is low, and quality product is high.The present invention utilizes discarded resource to carry out the preparation of trans-resveratrol and grape element, both effectively utilized resource, opened up a kind of new material resources, saved resource and cost, the product simultaneously obtaining has more the market competitiveness with respect to traditional trans-resveratrol product obtaining from giant knotweed.
Embodiment
Embodiment 1
The indoor preservation 60-90 days that the useless branch of grape vine under new beta pruning in autumn is positioned over to shady and cool dry, dark lucifuge, then shreds or is ground into meal by grape vine branches and tendrils.Take 500g grape vine branches and tendrils meal, add the distilled water of 2L, after soaking, ultrasonic 30 minutes.Then transfer them in the refluxing extraction tank of 20L, in extractor, add 5L edible ethanol, heating and refluxing extraction 2h, slightly cooling rear filter-cloth filtering obtains extracting solution, and grape vine branches and tendrils residue repeats to extract 1 time, united extraction liquid, high speed centrifugation, gets supernatant liquor.Supernatant liquor is transferred to vacuum-concentrcted in concentrating under reduced pressure instrument and reclaims ethanol, until obtain medicinal extract, medicinal extract is put in to the dry grape vine branches and tendrils crude extract that obtains in vacuum drier.Select D101 macroporous adsorbent resin 2L, resin is carried out to pre-treatment, abundant swelling, removal be contained unpolymerized organic solvent wherein.Adopt wet method dress post that D101 is seated in glass column or stainless steel pillar, grape vine branches and tendrils crude extract is added to 1L distilled water heating for dissolving, with the speed loading of 2 times of BV/h, adopt tlc to detect trans-resveratrol and grape cellulose content in effluent liquid, until adsorb saturated simultaneously.To adsorbing the extracting solution not first being adsorbed with 2 times of BV/h speed wash-outs with the distilled water of 1 BV for saturated macroporous adsorptive resins, then with 50% the ethanol of 3BV with 2BV/h speed wash-out, collect elutriant, and then with 70% the ethanol of 3BV with 2BV/h speed wash-out, collect elutriant.The elutriant concentrating under reduced pressure that 50% ethanol elution is obtained, reclaim ethanol, the medicinal extract obtaining is carried out to vacuum-drying, obtain trans-resveratrol product, Resveratrol content is 25%, the elutriant concentrating under reduced pressure that 70% ethanol elution is obtained, reclaim ethanol, the medicinal extract obtaining is carried out to vacuum-drying, obtain grape element product, trans-resveratrol output content is 21%.
Embodiment 2
The indoor preservation 60-90 days that the useless branch training of grape vine under new beta pruning in autumn is positioned over to shady and cool dry, dark lucifuge, then shreds or is ground into meal by grape vine branches and tendrils.Take 10kg grape vine branches and tendrils meal, add the distilled water of 20L, after soaking, ultrasonic 30 minutes.Then transfer them in multi-function extractor, in extractor, add 100L edible ethanol, heating and refluxing extraction 2h in multi-function extractor, slightly cooling rear filter-cloth filtering obtains extracting solution, and grape vine branches and tendrils residue repeats to extract 1 time, united extraction liquid, high speed centrifugation, gets supernatant liquor.Supernatant liquor is transferred to vacuum-concentrcted in concentrating under reduced pressure instrument and reclaims ethanol, until obtain medicinal extract, medicinal extract is put in to the dry grape vine branches and tendrils crude extract that obtains in vacuum drier.Select D101 macroporous adsorbent resin 20L, resin is carried out to pre-treatment, abundant swelling, removal be contained unpolymerized organic solvent wherein.Adopt wet method dress post that D101 is seated in stainless steel pillar, grape vine branches and tendrils crude extract is added to 10L distilled water heating for dissolving, with the speed loading of 2 times of BV/h, adopt tlc to detect trans-resveratrol and grape cellulose content in effluent liquid, until adsorb saturated simultaneously.To adsorbing the extracting solution not first being adsorbed with 2 times of BV/h speed wash-outs with the distilled water of 1 BV for saturated macroporous adsorptive resins, then with 50% the ethanol of 3BV with 2BV/h speed wash-out, collect elutriant, and then with 70% the ethanol of 3BV with 2BV/h speed wash-out, collect elutriant.The elutriant concentrating under reduced pressure that 50% ethanol elution is obtained, reclaim ethanol, the medicinal extract obtaining is carried out to vacuum-drying, obtain trans-resveratrol product, Resveratrol content is 22.5%, the elutriant concentrating under reduced pressure that 70% ethanol elution is obtained, reclaim ethanol, the medicinal extract obtaining is carried out to vacuum-drying, obtain grape element product, trans-resveratrol output content is 20%.
Claims (5)
1. a method of preparing trans-resveratrol and grape element from useless grape vine branches and tendrils is characterized in that: comprise the following steps the dry of (I) grape vine branches and tendrils: the grape vine branches and tendrils that beta pruning in autumn is obtained are collected and are positioned over the indoor of shady and cool dry lucifuge, allows its seasoning 30-60 days; (II) ultrasonic assisted extraction: adopt ultrasonic Assisted Ethanol refluxing extraction grape vine extract; (III) macroporous adsorbent resin is separated, selects low-pole or middle polarity macroporous adsorbent resin to carry out separation to extract, adopts the ethanol of different concns to carry out wash-out, and fraction collection obtains respectively trans-resveratrol and grape element.
2. from useless grape vine branches and tendrils, prepare a method for trans-resveratrol and grape element, it is characterized in that step (I), grape vine branches and tendrils dry, grape vine branches and tendrils prunes and are positioned over the dry lucifuge place's seasoning in indoor cool place 30-60 days to closely doing under fresh and alive state.
3. from useless grape vine branches and tendrils, prepare a method for trans-resveratrol and grape element, it is characterized in that step (II) and (III) comprising the steps: (1) ultrasonic wave Assisted Ethanol refluxing extraction grape vine extract; (2) the separated trans-resveratrol of macroporous adsorbent resin and grape element.
4. a kind of method of preparing trans-resveratrol and grape element from useless grape vine branches and tendrils according to claim 3, it is characterized in that, ultrasonic wave Assisted Ethanol refluxing extraction grape vine extract is: dried grape vine branches and tendrils are pulverized, the water soaking that adds 2 times of quality, ultrasonic 30 minutes of normal temperature, then add doubly 95% alcohol reflux 1-2h of 8-10, after filtration, obtain filtrate, filter residue adds doubly 95% alcohol reflux 1-2h of 5-8 again, after filtration, merging filtrate, ethanol is reclaimed in pressurization, obtain medicinal extract, vacuum-drying obtains grape vine extract.
5. a kind of method of preparing trans-resveratrol and grape element from useless grape vine branches and tendrils according to claim 3, it is characterized in that, the separated trans-resveratrol of macroporous adsorbent resin and grape element: grape vine extract is added to water heating for dissolving, with macroporous adsorbent resin, adsorb, different concentration ethanol is carried out wash-out, liquid chromatography tracking monitor trans-resveratrol and grape cellulose content, the trans-resveratrol of collecting and grape element section elutriant are merged respectively, and concentration and recovery ethanol, and vacuum-drying obtains respectively trans-resveratrol and the grape element product in grape source.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410238415.2A CN104030895A (en) | 2014-06-03 | 2014-06-03 | Method for preparing resveratrol and viniferin from waste grape vine branches and tendrils |
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| CN201410238415.2A CN104030895A (en) | 2014-06-03 | 2014-06-03 | Method for preparing resveratrol and viniferin from waste grape vine branches and tendrils |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829434A (en) * | 2015-05-08 | 2015-08-12 | 上海紫石生物科技有限公司 | Method for increasing content of stilbene compounds and preparation method of stilbene compounds |
| CN114539034A (en) * | 2022-04-06 | 2022-05-27 | 西夫拉姆酒业集团有限公司 | Purification process for extracting resveratrol from grape skin |
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2014
- 2014-06-03 CN CN201410238415.2A patent/CN104030895A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829434A (en) * | 2015-05-08 | 2015-08-12 | 上海紫石生物科技有限公司 | Method for increasing content of stilbene compounds and preparation method of stilbene compounds |
| CN114539034A (en) * | 2022-04-06 | 2022-05-27 | 西夫拉姆酒业集团有限公司 | Purification process for extracting resveratrol from grape skin |
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Application publication date: 20140910 |