CN1281857A - Microwave extraction method of protocyaidin-like substances from grape seed - Google Patents
Microwave extraction method of protocyaidin-like substances from grape seed Download PDFInfo
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- CN1281857A CN1281857A CN 00120353 CN00120353A CN1281857A CN 1281857 A CN1281857 A CN 1281857A CN 00120353 CN00120353 CN 00120353 CN 00120353 A CN00120353 A CN 00120353A CN 1281857 A CN1281857 A CN 1281857A
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Abstract
The present invention relates to a new method for extracting proanthocyanidine substance from grape seed by using microwave whose frequency is 2450 MHz or 915 MHz and power is 500-15000 W to treat grape seed in the solvent selected from water, C1-C3 alcohol, ethyl ether, propanone, ethyl acetate and toluene or their mixture. As compared with conventional chemical method it is simple in technological process, high in efficiency, quick in speed, low in cost and less in discharge of waste liquor.
Description
Present invention relates in general to separation, the extraction of material, more particularly, the present invention relates to from Semen Vitis viniferae, extract the method for pycnogenols class with microwave radiation.
The pycnogenols class that is present in the Semen Vitis viniferae is the material of the good antibiont interior free yl of a class, and its biological activity can reach ascorbic 30-50 doubly, and the 15-30 of vitamin-E doubly.Pycnogenols class material is mainly used in anti-cardiovascular disease, anti-ageing, antineoplastic health therapy.
At present, the method for extracting pycnogenols class material from Semen Vitis viniferae has two big classes basically, and the one, the traditional chemical solvent extraction method, another kind of is the supercritical extraction method.Yet this two classes extraction process all exists many defectives.
Particularly, the shortcoming of chemical solvents extraction has the energy, raw materials consumption amount big, and extraction efficiency is low, and the industrial pollution quantity discharged is big etc.In addition, though the supercritical extraction method is improved on extraction efficiency widely, the equipment that these class methods require is complicated, and the solvent range of choice is narrow, and product stability is poor, is unfavorable for scale operation.For example, CN1241623A discloses a kind of method of utilizing supercritical co extracting and separating raisin seed oil and pycnogenols class material from Semen Vitis viniferae.This method need be crushed to Semen Vitis viniferae the 20-40 order, and needs CO
2A series of equipment such as high-pressure pump, properties-correcting agent pump, preheater, extraction kettle, separator, refrigerator, and need under certain pressure (27 ± 2 MPa), to carry out.As seen, these class methods also exist certain defective.
Because microwave extracting can carry out the selectivity heating to the different components in the extraction system, and because microwave is to utilize molecular polarization or ionic conduction effect and directly material is heated, therefore can make that target components is easier dissociates out from extract, and the thermo-efficiency height has improved extraction efficiency.Yet up to this point, still nobody adopts microwave to extract pycnogenols class material.
The objective of the invention is to overcome the shortcoming that exists in the prior art,, provide the novel method of from Semen Vitis viniferae, extracting pycnogenols class material fast and efficiently by utilizing the characteristics of microwave extracting.That is, provide a kind of and can replace the simple and easy to do, efficient, quick of above-mentioned traditional solvent lixiviate and supercritical fluid extraction technology, cost is low, the novel method that the discharging of waste liquid amount is few.
The present invention is that to adopt frequency be that 2450MHz or 915MHz, power are that 500-15000 watt microwave is handled in solvent the Semen Vitis viniferae particle, extracts the novel method of pycnogenols class material from Semen Vitis viniferae.
Particularly, the present invention includes following aspect:
The invention provides a kind of extracting method of pycnogenols class material, this method comprises:
With frequency is that 2450MHz or 915MHz, power are that 500-15000 watt microwave is being selected from water, C to the Semen Vitis viniferae particle
1-C
3The solvent of alcohol, ether, acetone, ethyl acetate, the alkane of C6-C8 and composition thereof in the microwave treatment step handled.
In above-mentioned extracting method, also preferably include with the solvent that is selected from ethanol, acetone, ethyl acetate and composition thereof to microwave extraction after gained contain the step that water extracts once more, wherein saidly contain water and extract solvent for use once more and count 1 by volume: 1-3.
In above-mentioned extracting method, the amount of preferred described Semen Vitis viniferae particle and solvent counts 1 by weight: 2-8.
In above-mentioned extracting method, preferred described solvent contains the alkane of the C6-C8 of 10-20%.
In above-mentioned extracting method, preferred used microwave frequency is 2450MHz, and microwave treatment time is 1-20 minute.
In above-mentioned extracting method, preferred described microwave treatment is divided and is carried out for 1-3 time, each 1-10 minute.
In above-mentioned extracting method, preferred described Semen Vitis viniferae particle grain size is smaller or equal to 5 millimeters.
In above-mentioned extracting method, preferred describedly extract once more that to adopt frequency be that 2450MHz or 915MHz power are that 500-15000 watt microwave carries out.
In above-mentioned extracting method, also comprise in the preferred described extraction step once more and use the gac that is equivalent to Semen Vitis viniferae weight 0.1-1%.
More particularly, a particularly preferred method of the present invention comprises the steps: the Semen Vitis viniferae pulverizing is not more than 5 millimeters particle for particle diameter, pack into then in the extraction vessel, in this container in solid: the ratio of liquid=1: 2-8 (weight ratio) adds extraction solvent, with frequency is that 2450MHz or 915MHz, power tentatively add extraction heat 1-30 minute at 500-15000 watt microwave apparatus, preferred 1-20 minute.
Above-mentioned microwave treatment step is preferably divided and is carried out for 1-3 time, each 1-10 minute.
The alkane that preferably comprises the C6-C8 of about 10-20% (volume) in the described extraction solvent is as hexane, hexanaphthene, heptane, octane etc.
After finishing the preliminary extraction of microwave, also preferably gained is contained water and further extract.This step extracts and can carry out according to a conventional method, also can adopt microwave extracting of the present invention, and the latter is preferred.
The Semen Vitis viniferae that the present invention is adopted has no particular limits, but preferably is crushed into tiny particle, and particle diameter is generally and is not more than 5 millimeters, and in general is more in small, broken bits good more.
It extraction container of the present invention is had no particular limits, as long as can be used for microwave heating.This container can be open, also can have lid.Its example has the extractor of glass beaker, extractor such as tetrafluoroethylene or ceramic inner walls etc.
The microwave frequency that the present invention adopts is 2450MHz or 915MHz.The frequency of most industrial or civilian microwave instrument is 2450MHz at present.The inventor thinks that another industrial microwave frequency 915MHz also can realize purpose of the present invention.This be because the wavelength of 915MHz microwave greater than the wavelength of 2450MHz microwave, its to the penetration coefficient of vegetable cell should microwave unlike 2450MHz a little less than, and the final output rating of two kinds of microwaves can be adjusted to certain value, therefore, as long as coordinate the microwave output parameter, 915MHz is suitable for equally and extracts.2450MHz is the preferred frequency of the present invention.The power of the used microwave apparatus of the present invention is 500-20000 watt or bigger, preferred 500-15000 watt.
In preliminary extraction step of the present invention, preferably contain alkane such as hexane, hexanaphthene, heptane and the toluene etc. of C6-C8 in the solvent for use, they can use separately, also can mix use.Its consumption is the 10-20% of extraction agent.The ratio of used Semen Vitis viniferae and extraction agent (abbreviates as solid: liquid)=1: 2-8.The microwave radiation processing time of this step is 1-30 minute, preferred 15-20 minute.This microwave is just put forward step and can be divided and carry out for 1-3 time, each microwave action 1-10 minute.
Wherein after just putting forward step, remove by filter residue and the oily upper strata of liquid phase is removed, must contain water.
The above-mentioned step of extracting (essence is carried) once more can be the traditional extraction step, also can be the microwave extracting step as the preliminary extraction step of microwave of the present invention, and the latter is preferred.
Extract in (essence is carried) step once more of the present invention, solvent for use is for being preferably ethyl acetate, acetone, ethanol etc., and they can use separately, also can mix use.The above-mentioned water that contains is concentrated, the enriched material and the essence of gained are carried extraction agent by 1: the mixed of 1-3 (volume ratio).
Carry out above-mentioned extract once more before, also preferably adopt charcoal absorption, cross polyamide resin column, the mode of centrifugal and washing, the above-mentioned impurity that contains aqueous phase is removed.The mode that wherein adopts charcoal absorption is preferred.The general gac that is equivalent to Semen Vitis viniferae weight 0.1-1% that adopts.
Above-mentioned essence is put forward step and can be repeated repeatedly, till upper organic phase becomes clarification.
The present invention also randomly has been included in after the said extracted, with isolated refining liquid through concentrating, obtaining target product after the drying.
From as can be seen above-mentioned, method technology of the present invention is simple, saves time, and economizes energy, and the discharging of waste liquid amount is few, is a kind of environment-friendly type technique.
In the mode of embodiment, the present invention is done more detailed description below.
Embodiment 1:
Semen Vitis viniferae particle 100g is pulverized, pack in 1 liter the glass beaker, add methyl alcohol: ether: the solvent of water=0.6: 0.1: 0.3 (volume ratio), Gu: liquid (weight ratio)=1: 8, with power is microwave oven (the National K577 WFS that 900 watts of frequencies are 2540MHz, 1300W, 6A) heating was extracted 10 minutes, after the filtration, through concentrating under reduced pressure, reclaim first extract 180g, again with 50% ethyl acetate 500ml routinely extraction process extracted 1.0 hours and with 1/3 volume washing three times, through separation, concentrating under reduced pressure in room temperature is smart, and, get product 3.2g in-20 ℃ of dryings.The content of surveying pycnogenols class material with high efficiency liquid chromatography is 94%.
Wherein the parameter of used high efficiency liquid chromatography is as follows:
Chromatographic column: C18,
Eluent: A:4% aqueous formic acid, B:10% acetonitrile solution
Elution rate: 1.2ml/min
Wavelength: 280 nanometers
Embodiment 2:
Semen Vitis viniferae 1kg in small, broken bits is packed in the extractor, add ethanol: ethyl acetate: the solvent of water=0.5: 0.2: 0.3, Gu: liquid=1: 5 is the extracting through microwave heating 30 minutes of 2540MHz for the 1200W frequency with power, separate through filtration under diminished pressure, reclaim first extract 800ml.Use 50% acetone extraction again, wherein earlier with the microwave action identical with power 5 minutes, again through stirring with just putting forward the used frequency of step, extracted 2 hours, and separated after filtration, contain water and partly use 50% ethyl acetate extraction 3 times, through separating, with organic phase concentrating under reduced pressure, the dry product 29g that gets.Wherein the content with high efficiency liquid chromatography survey pycnogenols class material is 95%.Condition determination is with embodiment 1.
Embodiment 3
Semen Vitis viniferae particle 100g is pulverized, pack in 1 liter the glass beaker, add methyl alcohol: hexane: the solvent of water=0.6: 0.15: 0.25 (volume ratio), Gu: liquid (weight ratio)=1: 6, with power is that the microwave oven heating that 1000 watts of frequencies are 2540MHz was extracted 10 minutes, isolated for disposal liquid phase upper strata grease, filter rear filtrate through concentrating under reduced pressure, reclaim the first about 180g of extract, use 50% ethyl acetate 500ml again and be equivalent to Semen Vitis viniferae to weigh 0.5% gac, stir, add 1/3 volume washing three times, extraction process extracted 1.5 hours in room temperature is smart routinely, through separating, concentrating under reduced pressure, and, getting product 2.8g in-20 ℃ of dryings, the content of pycnogenols class material is 96%.
Comparative example
Adopt Semen Vitis viniferae 100 grams, experimentize with method and the common extraction process of embodiment 1.Difference of these two experiments only is that common extraction process is to replace the microwave among the embodiment 1 just to carry in 30 minutes with 1000 watts electric furnace heating and refluxing extraction.As a result, adopt microwave extraction to obtain end product 3.1g, the content 95% of pycnogenols class material; Adopt the electric furnace heating and refluxing extraction, get product 7.9g, the content 37% of pycnogenols class material.
From as can be seen above-mentioned, the inventive method step is easy, easy handling, and products obtained therefrom purity can reach 90-96%, and its energy consumption and solvent-oil ratio only are the 10-25% of conventional chemical method.The discharging of waste liquid amount reduces about 75-90%, belongs to typical clean environment production technique.
Claims (9)
1. the extracting method of a pycnogenols class material, this method comprises:
With frequency is that 2450MHz or 915MHz, power are that 500-15000 watt microwave is being selected from water, C to the Semen Vitis viniferae particle
1-C
3The solvent of alcohol, ether, acetone, ethyl acetate, the alkane of C6-C8 and composition thereof in the microwave treatment step handled.
2. the described extracting method of claim 1, also comprise with the solvent that is selected from ethanol, acetone, ethyl acetate and composition thereof to microwave extraction after gained contain the step that water extracts once more, wherein saidly contain water and extract solvent for use once more and count 1 by volume: 1-3.
3. the described extracting method of claim 1, the amount of wherein said Semen Vitis viniferae particle and solvent counts 1 by weight: 2-8.
4. the described extracting method of claim 3 contains the alkane of the C6-C8 of 10-20% in the wherein said solvent.
5. the described extracting method of claim 1, wherein used microwave frequency is 2450MHz, microwave treatment time is 1-20 minute.
6. each described extracting method among the claim 1-5, wherein said microwave treatment divide and carry out each 1-10 minute for 1-3 time.
7. each described extracting method among the claim 1-5, wherein said Semen Vitis viniferae particle grain size is smaller or equal to 5 millimeters.
8. the described extracting method of claim 2 describedly extracts once more that to adopt frequency be that 2450MHz or 915MHz power are that 500-15000 watt microwave carries out.
9. the described extracting method of claim 8 also comprises in the wherein said extraction step once more and uses the gac that is equivalent to Semen Vitis viniferae weight 0.1-1%.
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| CN00120353A CN1102589C (en) | 2000-07-08 | 2000-07-08 | Microwave extraction method of protocyaidin-like substances from grape seed |
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| CN00120353A CN1102589C (en) | 2000-07-08 | 2000-07-08 | Microwave extraction method of protocyaidin-like substances from grape seed |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102323378A (en) * | 2011-08-29 | 2012-01-18 | 湖南科技大学 | Method for rapidly detecting proanthocyanidin in plant |
| CN102351830A (en) * | 2011-08-16 | 2012-02-15 | 天津艾赛博生物技术有限公司 | Method for microwave extraction of anthocyanin, resveratrol and piceid from grape cell |
| CN103833718A (en) * | 2013-04-24 | 2014-06-04 | 新乡医学院 | Preparation method and application of proanthocyanidin derivative |
| CN104496957A (en) * | 2014-12-01 | 2015-04-08 | 成都红柿子科技有限公司 | Method for extracting procyanidine from grape skins |
| CN108634181A (en) * | 2018-05-04 | 2018-10-12 | 安徽燕之坊食品有限公司 | A kind of grape seed extract flour additive and preparation method thereof |
| CN109134415A (en) * | 2018-10-16 | 2019-01-04 | 宾川县华侨庄园农业科技开发有限公司 | A kind of extracting method of grape pip procyanidin |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100384832C (en) * | 2005-07-18 | 2008-04-30 | 天津大学 | Method of extracting proto anthocyanidin by supercritical extraction grape seed oil and resin absorption |
| EP2575844B1 (en) | 2010-05-28 | 2016-11-23 | Finzelberg GmbH & Co. KG | Method for producing an enriched extract from vine plants |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2205207T3 (en) * | 1996-09-20 | 2004-05-01 | The Howard Foundation | FOOD SUPPLEMENTS CONTAINING FLAVONOLES. |
-
2000
- 2000-07-08 CN CN00120353A patent/CN1102589C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351830A (en) * | 2011-08-16 | 2012-02-15 | 天津艾赛博生物技术有限公司 | Method for microwave extraction of anthocyanin, resveratrol and piceid from grape cell |
| CN102351830B (en) * | 2011-08-16 | 2013-09-04 | 天津艾赛博生物技术有限公司 | Method for microwave extraction of anthocyanin, resveratrol and piceid from grape cell |
| CN102323378A (en) * | 2011-08-29 | 2012-01-18 | 湖南科技大学 | Method for rapidly detecting proanthocyanidin in plant |
| CN103833718A (en) * | 2013-04-24 | 2014-06-04 | 新乡医学院 | Preparation method and application of proanthocyanidin derivative |
| CN104496957A (en) * | 2014-12-01 | 2015-04-08 | 成都红柿子科技有限公司 | Method for extracting procyanidine from grape skins |
| CN108634181A (en) * | 2018-05-04 | 2018-10-12 | 安徽燕之坊食品有限公司 | A kind of grape seed extract flour additive and preparation method thereof |
| CN109134415A (en) * | 2018-10-16 | 2019-01-04 | 宾川县华侨庄园农业科技开发有限公司 | A kind of extracting method of grape pip procyanidin |
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| CN1102589C (en) | 2003-03-05 |
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