CN102517144A - Method for extracting oil and procyanidin from grape seeds - Google Patents
Method for extracting oil and procyanidin from grape seeds Download PDFInfo
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- CN102517144A CN102517144A CN2011103845171A CN201110384517A CN102517144A CN 102517144 A CN102517144 A CN 102517144A CN 2011103845171 A CN2011103845171 A CN 2011103845171A CN 201110384517 A CN201110384517 A CN 201110384517A CN 102517144 A CN102517144 A CN 102517144A
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Abstract
The invention relates to a technology for extracting effective components from a natural product and in particular relates to a method for extracting oil and procyanidin from grape seeds. The method comprises the following process steps: preparing grape seeds, grinding, performing ultrasonic extraction to obtain grape seed oil, and performing ultrasonic extraction to obtain procyanidin. The method integrates the characteristics of an ultrasonic extraction method and a double-solvent extraction method, has the characteristics of low solvent dosage, low extraction cost, high extraction efficiency, less influence on the environment and the like, and can be used for effectively avoiding the problem that in the extraction process of the prior art, the bioactivities of grape seed oil and procyanidin are damaged.
Description
Affiliated technical field
The present invention relates to a kind of from natural product the technology of extracting effective components, particularly a kind of method of from Semen Vitis viniferae, extracting grease and pycnogenols.
Background technology
Pycnogenols, English name are Oligomeric Proantho Cyanidins (OPC), are a kind of Vitamin P complexs that special molecular structure is arranged, and are the most effective natural antioxidantss of radical in the removing human body of generally acknowledging in the world at present.Be generally the reddish-brown powder, little, the puckery of gas, water-soluble and most organic solvent.Be generally Semen Vitis viniferae extract or French maritime pine bark extract.Pycnogenols is a kind of new and effective inhibitor, and the free-radical scavengers of imitating the most by force that is so far to be found has very strong activity in vivo.The Green Tea Extract oxidation capacity that experiment showed, OPC is 50 times of vitamin E, ascorbic 20 times, and absorb rapidly fully, can reach the highest haemoconcentration in oral 20 minutes, metabolic half life is for 7 hours.
At present about utilizing the method for Semen Vitis viniferae stripping oil or pycnogenols to mainly contain following several kinds: solvent-extraction process, supercritical CO
2Extraction method, microwave extraction method etc., the deficiency that these process for extracting mainly exist is: the defective that solvent-extraction process mainly exists is that organic solvent consumption is many, length consuming time; Production cost is high; The product that obtains more or less all exists the residual of solvent, and the solvent pollution on the environment that leaks, thereby brings production unit complicated; The investment operation expense is high, problems such as cost increase; Supercritical CO
2The weak point of extraction method mainly be cost high, to the requirement of operational condition than higher; The weak point that the microwave extraction method exists such as the selection of spe medium are bigger to the product components influence, cause the loss of part composition.And the pycnogenols high thermal resistance is poor, instability, the inactive that is prone to, and process for extracting is just had strict requirement, and just extracted a kind of material in the Semen Vitis viniferae in the above-mentioned existing method, like raisin seed oil or pycnogenols, is a kind of waste to resource.
Summary of the invention
The objective of the invention is to solve the defective that prior art exists; Provide a kind of ultrasonic extraction method and solvent pairs method utilized to combine; In same technology, can extract grease in the Semen Vitis viniferae; Can extract the pycnogenols in the Semen Vitis viniferae again, and extraction yield is high, power consumption is low and the method for from Semen Vitis viniferae, extracting grease and pycnogenols of easy purifying.
Technical scheme of the present invention is: a kind of method of from Semen Vitis viniferae, extracting grease and pycnogenols, and its process step is:
1) preparation of Semen Vitis viniferae: will reclaim the grape skin behind the wine liquid, through drying remove residual moisture to water ratio less than 2% after, Pericarpium Vitis viniferae is separated with Semen Vitis viniferae, Semen Vitis viniferae;
2) pulverize: be crushed to behind the 80-100 order Semen Vitis viniferae after air-dry for use;
3) ultrasonic extraction raisin seed oil: the Semen Vitis viniferae after will pulverizing is put into fat-soluble solvent, adopts ultrasonic extraction, and wherein Semen Vitis viniferae and fat-soluble solvent weight, volume ratio are 1: 5～10; Extract 50 ℃～70 ℃ of temperature, extraction time 10～20min is after extraction finishes; Extracting solution was carried out filtering filtrating and filter residue, and will filtrate concentrates and the recovery solvent, utilizes recovered solvent that filter residue is extracted once more; The extraction temperature and time is with extract phase is same for the first time; After extracting end, extracting solution is carried out filtering filtrating and filter residue, concentrated and reclaimed solvent to filtrating; After the liquid concentrator of extracted twice mixed, after the drying raisin seed oil;
4) ultrasonic extraction pycnogenols: the filter residue behind the said extracted raisin seed oil is put into water-soluble solvent, adopt ultrasonic extraction then; Wherein the weight of filter residue and water-soluble solvent, volume ratio are 1: 9～15, extract 30 ℃～50 ℃ of temperature, extraction time 8～10min; After extracting end, extracting solution is carried out filtering filtrating and filter residue, concentrated and reclaimed solvent to filtrating; Utilize recovered solvent that filter residue is extracted once more, extract temperature and time and extract phase for the first time with, extract finish after; Extracting solution is carried out filtering filtrating and filter residue, concentrated and reclaimed solvent to filtrating; After the liquid concentrator of extracted twice mixed, after the drying the pycnogenols meal, after purified the pycnogenols product.
Above-mentioned fat-soluble solvent is normal hexane, sherwood oil, tetracol phenixin.
The solvent that above-mentioned polarity is stronger is acetone, ethanol, methyl alcohol.
The above-mentioned dry vacuum-drying of adopting, drying temperature is 40-60 ℃.
The purifying of above-mentioned pycnogenols is to adopt macroporous resin to carry out Static Adsorption and wash-out, to remove partial impurities such as polysaccharide.
The characteristics of the present invention is integrated ultrasonic extraction and solvent pairs method formulation; Have following characteristics: 1, utilize special roles such as judder that UW produces, very high acceleration stresses, intensive cavitation effect, stirring can improve the impact velocity between the material molecule; Shorten action time, promoted raisin seed oil, pycnogenols, thereby can reduce the consumption of solvent to two kinds of dissolution raties of extracting in the solvent; Reduce extraction cost, improve extraction efficiency.Can find out through following table, technical scheme of the present invention compared with prior art, the raisin seed oil leaching process extracts temperature and has reduced by one times, extraction yield has improved 3 percentage points, purity is high more than 10 percentage points.The leaching process of pycnogenols extracts temperature and has reduced by 20 ℃, and extraction yield has improved nearly 10 percentage point, and purity is high more than 15 percentage points; 2, owing to poor, the instability of pycnogenols high thermal resistance in the Semen Vitis viniferae, be prone to inactivation, must under comparatively gentle condition, extract, and contain more hydroxyl in the structure of pycnogenols; Be easy to form hydrogen bond with polysaccharose substance and other phenolic cpds etc.; So the energy that utilizes hyperacoustic high-frequency vibration to produce replaces heating the energy that provides, the thermal motion of molecule is quickened; This has just determined that the condition of UW effect is relatively gentleer; Can extract at normal temperatures, avoid in the leaching process of prior art, the destruction of raisin seed oil and biological activity of procyanidine.
The raisin seed oil that the present invention and prior art are produced, the index of pycnogenols contrast like following table:
3, the present invention is the extraction process of environment-friendly type.With traditional technology Comparatively speaking lower because used solvent can recycle in leaching process, solvent load is little to the influence of environment, make the present invention have the characteristics of environmental protection.4, market outlook aspect: related data shows; The content of unsaturated fatty acids is up to 92% in the raisin seed oil; Also contain abundant linolic acid, it has the blood fat of keeping balance, reducing cholesterol, prevents thrombotic effect, also contains various trace elements and vitamin E; Pycnogenols has stronger antioxygenation, removes radical and active oxygen; The two all has good health-care effect, so raisin seed oil and pycnogenols product are very well sold and in short supply in the world market, is in great demand, and has very vast market prospect.
Description of drawings
Accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
The process flow sheet that from Semen Vitis viniferae, extracts grease and pycnogenols shown in accompanying drawing 1, embodiment is following.
Embodiment 1:
1) preparation of Semen Vitis viniferae: will reclaim the grape skin behind the wine liquid, through drying remove residual moisture to water ratio less than 2% after, Pericarpium Vitis viniferae is separated with Semen Vitis viniferae, Semen Vitis viniferae;
2) pulverize: be crushed to behind 80 orders Semen Vitis viniferae after air-dry for use.
3) ultrasonic extraction raisin seed oil: different at first extraction of solvability according to raisin seed oil and pycnogenols gets raisin seed oil in the Semen Vitis viniferae, take by weighing and pulverize back 80 purpose Semen Vitis viniferae powder 2g, adds the sherwood oil 14ml of volume(tric)fraction >=99.5%; Place the supersound extraction device to extract, extracting temperature is 60 ℃, extraction time 15min; After extracting end, extracting solution was carried out filtering filtrating and filter residue, will filtrate concentrates and reclaims solvent; Utilize recovered solvent that filter residue is extracted once more, extract temperature and time and extract phase for the first time with, extract finish after; Extracting solution is carried out filtering filtrating and filter residue, concentrated and reclaimed solvent to filtrating; After the liquid concentrator of extracted twice mixed, place after 60 ℃ the vacuum drying oven drying raisin seed oil, calculating extraction yield is 15.7%.
4) ultrasonic extraction pycnogenols: take by weighing the filter residue 2g behind the said extracted raisin seed oil, add the 18ml volume(tric)fraction and be 70% acetone soln, place the supersound extraction device to extract; Extract 40 ℃ of temperature, extraction time 9min is after extraction finishes; Extracting solution was carried out filtering filtrating and filter residue, and will filtrate concentrates and the recovery solvent, utilizes recovered solvent that filter residue is extracted once more; Extract temperature and time and extract phase for the first time with, extract finish after, extracting solution was carried out filtering filtrating and filter residue; Concentrate and reclaim solvent to filtrating, so circulation is extracted three times continuously; The liquid concentrator that extracts for three times merged to be placed on carry out drying in the vacuum drying oven, 40 ℃ of drying temperatures, dry back gained pycnogenols meal, the extraction yield that calculates pycnogenols is 25.09%.
5) purifying of pycnogenols: take by weighing the good AB-8 type macroporous resin 1g of pre-treatment in the tool plug Erlenmeyer flask of 50ml; And the pycnogenols meal 0.5g that takes by weighing dry gained to be dissolved in the 10ml volume(tric)fraction be in 50% the ethanolic soln; Join to place on the shaking table in the tool plug Erlenmeyer flask and vibrate, the vibration temperature is 50 ℃, adsorption time 15min; After absorption finishes; Saturated polymeric adsorbent elder generation water is carried out wash-out, and till elutriant was water white transparency, purpose was to remove impurity such as inorganic salt, polysaccharide, protein; Using volume(tric)fraction again is that 50% ethanolic soln carries out wash-out once more, and elution time is 45 ℃ of 15min, eluting temperatures.Elutriant is collected, reclaimed solvent, concentrates the small amount of liquid that obtains containing pycnogenols, and place 40 ℃ vacuum drying oven drying to obtain the pure article of pycnogenols, purity is 95.6%.
Embodiment 2-3:
The extraction of raisin seed oil: on the basis of case study on implementation 1; Change to extract solvent volume(tric)fraction, extract temperature (℃), the processing parameters such as particle size of extraction time (min), extraction time, solid-liquid ratio (g/ml), Semen Vitis viniferae raw material, the practical implementation parameter is as shown in the table:
In the foregoing description 2-3; Utilize extracting the parameter that filter residue behind the raisin seed oil extracts pycnogenols is: extract solvent volume(tric)fraction, extract temperature (℃), extraction time (min), extraction time, solid-liquid ratio (g/ml), the practical implementation parameter is as shown in the table:
The purifying of pycnogenols is identical with case 1.
Embodiment 4-5:
The extraction of raisin seed oil: on the basis of case study on implementation 2-3, other extraction conditions immobilize, and only change the volume(tric)fraction of extraction solvent and the particle size of Semen Vitis viniferae raw material, practical implementation parameter such as following table:
The extraction of pycnogenols: on the basis of case study on implementation 2-3, other extraction conditions immobilize, and only change the volume(tric)fraction of extraction solvent and the particle size of Semen Vitis viniferae raw material, practical implementation parameter such as following table:
The purifying of pycnogenols is identical with embodiment 1.
In the above-described embodiments, the purifying of pycnogenols can adopt existing technology to carry out.
Claims (5)
1. method of from Semen Vitis viniferae, extracting grease and pycnogenols, its process step is:
1) preparation of Semen Vitis viniferae: will reclaim the grape skin behind the wine liquid, through drying remove residual moisture to water ratio less than 2% after, Pericarpium Vitis viniferae is separated with Semen Vitis viniferae, Semen Vitis viniferae;
2) pulverize: be crushed to behind 80-100 orders Semen Vitis viniferae after air-dry for use;
3) ultrasonic extraction raisin seed oil: the Semen Vitis viniferae after will pulverizing is put into fat-soluble solvent, adopts ultrasonic extraction, and wherein Semen Vitis viniferae and fat-soluble solvent weight, volume ratio are 1:5～10; Extract 50 ℃～70 ℃ of temperature, extraction time 10～20min is after extraction finishes; Extracting solution was carried out filtering filtrating and filter residue, and will filtrate concentrates and the recovery solvent, utilizes recovered solvent that filter residue is extracted once more; The extraction temperature and time is with extract phase is same for the first time; After extracting end, extracting solution is carried out filtering filtrating and filter residue, concentrated and reclaimed solvent to filtrating; After the liquid concentrator of extracted twice mixed, after the drying raisin seed oil;
4) ultrasonic extraction pycnogenols: the filter residue behind the said extracted raisin seed oil is put into water-soluble solvent, adopt ultrasonic extraction then; Wherein the weight of filter residue and water-soluble solvent, volume ratio are 1:9～15, extract 30 ℃～50 ℃ of temperature, extraction time 8～10min; After extracting end, extracting solution is carried out filtering filtrating and filter residue, concentrated and reclaimed solvent to filtrating; Utilize recovered solvent that filter residue is extracted once more, extract temperature and time and extract phase for the first time with, extract finish after; Extracting solution is carried out filtering filtrating and filter residue, concentrated and reclaimed solvent to filtrating; After the liquid concentrator of extracted twice mixed, after the drying the pycnogenols meal, after purified the pycnogenols product.
2. the method for from Semen Vitis viniferae, extracting grease and pycnogenols according to claim 1 is characterized in that above-mentioned fat-soluble solvent is normal hexane, sherwood oil, tetracol phenixin.
3. the method for from Semen Vitis viniferae, extracting grease and pycnogenols according to claim 2 is characterized in that the stronger solvent of above-mentioned polarity is acetone, ethanol, methyl alcohol.
4. according to the described method of from Semen Vitis viniferae, extracting grease and pycnogenols of above-mentioned any claim, it is characterized in that the above-mentioned dry vacuum-drying of adopting, drying temperature is 40-60 ℃.
5. the method for from Semen Vitis viniferae, extracting grease and pycnogenols according to claim 4, the purifying that it is characterized in that above-mentioned pycnogenols are that the employing macroporous resin carries out Static Adsorption and wash-out, to remove partial impurities such as polysaccharide.
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816637A (en) * | 2012-08-27 | 2012-12-12 | 安徽农业大学 | Combined extraction method of Paeonia ostii seed oil and Paeonia ostii seed total flavonoids |
| CN103571608A (en) * | 2013-10-29 | 2014-02-12 | 张丽娜 | Method for extracting grape seed oil by utilizing cellulase |
| CN103833718A (en) * | 2013-04-24 | 2014-06-04 | 新乡医学院 | Preparation method and application of proanthocyanidin derivative |
| CN104886268A (en) * | 2014-03-06 | 2015-09-09 | 洛阳春魁农业开发有限公司 | Grape seed oil-containing peony seed blend oil and preparation method thereof |
| CN104997109A (en) * | 2015-08-06 | 2015-10-28 | 贵州三农楮桃产业开发有限公司 | Broussonetia papyrifera pulp rich in proanthocyanidins as well as preparation method and application of broussonetia papyrifera pulp |
| CN106118877A (en) * | 2016-07-14 | 2016-11-16 | 山东巧妻食品科技有限公司 | A kind of Oleum Gossypii semen antioxidant |
| CN106581318A (en) * | 2016-12-20 | 2017-04-26 | 大连赛姆生物工程技术有限公司 | Method for improving dissolution rate of grape seed extract flavones in press-shear assisted interaction mode |
| CN106632206A (en) * | 2016-12-20 | 2017-05-10 | 大连赛姆生物工程技术有限公司 | Method for improving dissolubility of proanthocyanidins of grape seed extract in press-shear assisted interaction manner |
| CN106699915A (en) * | 2016-12-20 | 2017-05-24 | 大连赛姆生物工程技术有限公司 | Method for improving dissolution rate of polysaccharide of grapeseed extract through pressure-shear induced chemical transition |
| CN106728480A (en) * | 2016-12-20 | 2017-05-31 | 大连赛姆生物工程技术有限公司 | It is a kind of to cut the method for helping interaction mode to improve grape seed extract polyphenol dissolution rate using micro- |
| CN106728481A (en) * | 2016-12-20 | 2017-05-31 | 大连赛姆生物工程技术有限公司 | It is a kind of to cut the method for helping interaction mode to improve grape seed extract saponin(e dissolution rate using micro- |
| CN106883927A (en) * | 2017-03-09 | 2017-06-23 | 管天球 | A kind of preparation method of grape-kernel oil |
| CN107307420A (en) * | 2017-07-04 | 2017-11-03 | 浙江绍兴东灵保健食品有限公司 | A kind of grape pip extract powder production technology |
| CN108934805A (en) * | 2018-04-23 | 2018-12-07 | 安徽省宗正农业科技开发有限公司 | A kind of high-quality Cortex Eucommiae implantation methods |
| 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 |
| CN109181356A (en) * | 2018-11-14 | 2019-01-11 | 罗莱生活科技股份有限公司 | A kind of technique extracted pigment from grape pip and prepare dyestuff |
| CN111205260A (en) * | 2020-02-12 | 2020-05-29 | 佛山市鼎科科技发展有限公司 | Method for extracting grape seed extract with high procyanidine content |
| CN114015082A (en) * | 2021-11-29 | 2022-02-08 | 齐鲁工业大学 | Method for preparing functional grape seed nano-sphere particles by utilizing grape seeds and product thereof |
| CN114010573A (en) * | 2021-11-25 | 2022-02-08 | 南京高光时刻生物科技有限公司 | Cell regeneration and repair essence for medical cosmetology and preparation method thereof |
Citations (1)
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| CN101177648A (en) * | 2007-12-12 | 2008-05-14 | 国家粮食储备局无锡科学研究设计院 | Method for extracting grape seed oil and procyanidine from grape seeds by one-step process |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177648A (en) * | 2007-12-12 | 2008-05-14 | 国家粮食储备局无锡科学研究设计院 | Method for extracting grape seed oil and procyanidine from grape seeds by one-step process |
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816637A (en) * | 2012-08-27 | 2012-12-12 | 安徽农业大学 | Combined extraction method of Paeonia ostii seed oil and Paeonia ostii seed total flavonoids |
| CN102816637B (en) * | 2012-08-27 | 2014-07-09 | 安徽农业大学 | Combined extraction method of Paeonia ostii seed oil and Paeonia ostii seed total flavonoids |
| CN103833718A (en) * | 2013-04-24 | 2014-06-04 | 新乡医学院 | Preparation method and application of proanthocyanidin derivative |
| CN103571608A (en) * | 2013-10-29 | 2014-02-12 | 张丽娜 | Method for extracting grape seed oil by utilizing cellulase |
| CN104886268A (en) * | 2014-03-06 | 2015-09-09 | 洛阳春魁农业开发有限公司 | Grape seed oil-containing peony seed blend oil and preparation method thereof |
| CN104997109A (en) * | 2015-08-06 | 2015-10-28 | 贵州三农楮桃产业开发有限公司 | Broussonetia papyrifera pulp rich in proanthocyanidins as well as preparation method and application of broussonetia papyrifera pulp |
| CN106118877A (en) * | 2016-07-14 | 2016-11-16 | 山东巧妻食品科技有限公司 | A kind of Oleum Gossypii semen antioxidant |
| CN106728480A (en) * | 2016-12-20 | 2017-05-31 | 大连赛姆生物工程技术有限公司 | It is a kind of to cut the method for helping interaction mode to improve grape seed extract polyphenol dissolution rate using micro- |
| CN106632206A (en) * | 2016-12-20 | 2017-05-10 | 大连赛姆生物工程技术有限公司 | Method for improving dissolubility of proanthocyanidins of grape seed extract in press-shear assisted interaction manner |
| CN106699915A (en) * | 2016-12-20 | 2017-05-24 | 大连赛姆生物工程技术有限公司 | Method for improving dissolution rate of polysaccharide of grapeseed extract through pressure-shear induced chemical transition |
| CN106581318A (en) * | 2016-12-20 | 2017-04-26 | 大连赛姆生物工程技术有限公司 | Method for improving dissolution rate of grape seed extract flavones in press-shear assisted interaction mode |
| CN106728481A (en) * | 2016-12-20 | 2017-05-31 | 大连赛姆生物工程技术有限公司 | It is a kind of to cut the method for helping interaction mode to improve grape seed extract saponin(e dissolution rate using micro- |
| CN106883927A (en) * | 2017-03-09 | 2017-06-23 | 管天球 | A kind of preparation method of grape-kernel oil |
| CN107307420A (en) * | 2017-07-04 | 2017-11-03 | 浙江绍兴东灵保健食品有限公司 | A kind of grape pip extract powder production technology |
| CN108934805A (en) * | 2018-04-23 | 2018-12-07 | 安徽省宗正农业科技开发有限公司 | A kind of high-quality Cortex Eucommiae implantation methods |
| 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 |
| CN109181356A (en) * | 2018-11-14 | 2019-01-11 | 罗莱生活科技股份有限公司 | A kind of technique extracted pigment from grape pip and prepare dyestuff |
| CN111205260A (en) * | 2020-02-12 | 2020-05-29 | 佛山市鼎科科技发展有限公司 | Method for extracting grape seed extract with high procyanidine content |
| CN114010573A (en) * | 2021-11-25 | 2022-02-08 | 南京高光时刻生物科技有限公司 | Cell regeneration and repair essence for medical cosmetology and preparation method thereof |
| CN114015082A (en) * | 2021-11-29 | 2022-02-08 | 齐鲁工业大学 | Method for preparing functional grape seed nano-sphere particles by utilizing grape seeds and product thereof |
| CN114015082B (en) * | 2021-11-29 | 2023-04-18 | 齐鲁工业大学 | Method for preparing functional grape seed nano-sphere particles by utilizing grape seeds and product thereof |
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