CN1923831B - Preparation technology of grape seed polyphenols - Google Patents
Preparation technology of grape seed polyphenols Download PDFInfo
- Publication number
- CN1923831B CN1923831B CN2005100606031A CN200510060603A CN1923831B CN 1923831 B CN1923831 B CN 1923831B CN 2005100606031 A CN2005100606031 A CN 2005100606031A CN 200510060603 A CN200510060603 A CN 200510060603A CN 1923831 B CN1923831 B CN 1923831B
- Authority
- CN
- China
- Prior art keywords
- ethyl acetate
- concentrated solution
- water
- grape seed
- seed polyphenols
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a manufacturing technology of grape seed polyphenols from grape seed in the brewing industrial leftover bits and pieces, which comprises the following steps: extracting through water instead of alcohol; centrifuging; columning; condensing; extracting; spraying; drying; detecting; packing; adopting large-hole resin column to adsorb polyphenols selectily; extracting the condensed liquid through acetic ester.
Description
Technical field
The present invention relates to a kind of processing method of utilizing water as solvent from liquor industry tankage Semen Vitis viniferae, to extract grape seed polyphenols.
Background technology
Grape seed polyphenols is a kind of powerful antioxidant, and the title of " polyphenol king " is arranged, and its anti-oxidation efficacy is 20 times of VC, 50 times of VE.Its basal component is the polymkeric substance of the complexity that forms through biochemical reaction in plant materials of simple material such as catechin, l-Epicatechol.Extent of polymerization is low more, and product efficacy is strong more.Grape seed polyphenols uses as bulk drug, foodstuff additive, protective foods and cosmetics additive on American-European market.The medicine that is made into is to prevention and treat cardiovascular and cerebrovascular diseases, reducing blood-fat, blood pressure, and anti-cancer, anticancer etc. has remarkable efficacy.In recent years, grape seed polyphenols is constantly being opened up new purposes, for example: add in the grape wine as wine additive, with the mouthfeel of improving wine, the nourishing function that strengthens wine, improvement colours of wine.In the world, France is the country that produces the grape seed polyphenols product the earliest, but the price of this product is very expensive.China also had minority producer to begin to produce grape seed polyphenols in recent years, but production process is quite loaded down with trivial details.As divide 10 procedures:
1. lixiviate: with 5 times of 70% alcohol to the Semen Vitis viniferae raw material as solution, lixiviate below 65 ℃ 24 hours;
2. filter: screen filtration, impregnated Semen Vitis viniferae is discarded, vat liquor is standby;
3. concentrate A: temperature is lower than 60 ℃ of concentrating under reduced pressure, and the concentrated solution degree Beaume reaches 29 °;
4. depositing in water: add 6-7 water doubly after the concentrated solution cooling, the limit adds the waterside stirs, and normal temperature left standstill more than 8 hours in setting tank thereafter, and supernatant liquor takes out standby; Add 4-5 times of water in the throw out again and carry out secondary sedimentation, leave standstill more than 8 hours again, supernatant liquor takes out standby, and throw out discards; Merge supernatant liquor;
5. concentrate B: be lower than under 60 ℃ of temperature, concentrating under reduced pressure is to about 6 ° of degree Beaume;
6. cross post: concentrated solution advances macroporous resin column, carries out selective adsorption; Behind the washing pillar, wash, get two kinds of elutriants with 30%, 70% alcohol gradation;
7. concentrate C: two kinds of elutriants distill separately sloughs alcohol and portion water, and making degree Beaume is 8-10 °;
8. extraction: the elutriant that washes through spissated 70% alcohol with the ethyl acetate extraction of 5 times of volumes, 2 times of volumes each once, merging secondary acetic acid ethyl acetate extract, water layer discarded;
9. concentrate D: add water to ethyl acetate layer, boil off ethyl acetate, get degree Beaume 8-10 ° concentrated solution;
10. dry: as to merge 7., 9. two kinds of concentrated solutions of C, D of operation spraying drying under 200 ℃-210 ℃ of inlet temperatures, 91 ℃ of-125 ℃ of conditions of temperature out.
Not only operating process is consuming time reaches more than 50 hour for above operation, and with regard to 24 hours consuming time, secondary depositing in water 16 hours consuming time altogether influenced production output as the lixiviate operation.And enrichment process nearly 4 times, elongated man-hour, consumed a large amount of energy, repeatedly being heated descends quality product.
Relatively distinct issues are: 1. 70% edible ethanol with 5 times of raw materials obtains the Semen Vitis viniferae vat liquor as solvent, and the alcohol amount of expending is big especially, certainly will cause cost to improve like this.2. leave standstill depositing in water with screen filtration and secondary and remove fine particle and residue, working efficiency is extremely low.And because production process is scientific and reasonable inadequately, and labour intensity is big, and the product recovery rate is lower, quality is not ideal enough.
Summary of the invention
Technical problem to be solved by this invention is to remedy above-mentioned defective, adopt new production technique to simplify production process, shorten Production Flow Chart, reduce cost, improve recovery rate, improve quality product, disclose a kind of production technique of new preparation grape seed polyphenols to society.
Concrete operation of the present invention is:
1. lixiviate: the Semen Vitis viniferae raw material is added 5-9 doubly to the water of raw material weight, heats to 95 ℃, keep 95 ℃-98 ℃ 4 hours, get the juice time vat liquor of winning; Mend 3-6 times of water again, be warming up to 95 ℃ again, keep 95 ℃-98 ℃ 2 hours, obtain vat liquor for the second time, merge the secondary vat liquor;
2. centrifugal: as, to carry out centrifugally operated and remove fine particle, residue with 50 ℃-70 ℃ vat liquor;
3. cross post: with the centrifugate below 50 ℃, advance macroporous resin column, carry out the polyphenol selective adsorption, behind the washed resin, wash with concentration 40-60% alcohol again, get elutriant;
4. concentrate: elutriant at vacuum tightness 0.4-0.6Mpa, 60 ℃ of-70 ℃ of recovered alcohols of temperature, is concentrated elutriant, get concentrated solution;
5. dust: above-mentioned concentrated solution is pumped into spray-drying tower spraying, 215 ℃-225 ℃ of spray-drying tower inlet temperature, 105 ℃-107 ℃ of air outlet temperatures are dried to the grape seed polyphenols fine powder of good fluidity, detect qualified back and pack.
For obtaining product of high grade, need before dusting concentrated solution is implemented extraction: divide secondary to add the ethyl acetate extraction secondary of 2-3 times of concentrated solution volume, abandon water layer, after merging the secondary acetic acid ethyl acetate extract, the pure water or the deionized water that add concentrated solution volume before being equivalent to extract, ethyl acetate is reclaimed in distillation, gets the polyphenol concentrated solution.
In order to reduce cost, in raw materials quality generally speaking, when the raw material effective component content is low, the 1. the procedure lixiviate can be, in the Semen Vitis viniferae raw material, add 5 times to the water of raw material weight, heat to 95 ℃, keep 95 ℃-98 ℃ 4 hours, juice is emitted; Mend 3 times of water, be warming up to 95 ℃, keep 95 ℃-98 ℃ 2 hours, again juice is emitted; Thereafter add the washing slag of 1 times of raw material weight again, get washings, merge secondary juice and washings at last and get vat liquor.
Under the good situation of raw materials quality, can add 7 times or 9 times during lixiviate to the water of Semen Vitis viniferae weight, heat to 95 ℃, keep 95 ℃-98 ℃ 4 hours, get the juice time vat liquor of winning; Mend the water of 5 times or 6 times weight again, repeat previous step, keep getting vat liquor for the second time in 2 hours; Thereafter add the washing slag of 1 times of weight again, get washings, merge secondary vat liquor and washings at last and get vat liquor.
In order to guarantee the vat liquor quality, the temperature during the lixiviate heating remains in 98 ℃ and is optimum regime.
Resin was to the selective adsorption capacity of polyphenol when strengthening post, and it is good adopting the resin of PN100, PN400, CAD40, YWD04B2 or PN700 model.The alcohol that is used for wash-out can be that 50% concentration is advisable.
In order in the concentrated solution of elutriant after recovery wine is clear, to extract the grape seed polyphenols effective ingredient more, can be earlier with 3 times of ethyl acetate extractions, use 2 times ethyl acetate extraction again, after merging the secondary ethyl acetate layer, the pure water or the deionized water that in the ethyl acetate solution of polyphenol, add polyphenol concentrated solution volume before 1 times of extraction, ethyl acetate is reclaimed in distillation, must change water-soluble high purity grape seed polyphenols solution.Distillation recovery ethyl acetate can be carried out in still kettle, and ethyl acetate through the condensation recovery, promptly stays the high purity grape seed polyphenols solution that changes water-soluble through the outlet of still kettle top in the still, for the usefulness of the drying process that dusts.
Advantage of the present invention is: reasonable in design, the science of a. operation sequence, technology, parameter, improved recovery rate and quality product.The polyphenol content of product can reach more than 95.47%, moisture content≤1.0%, ash≤0.48%.B. immerse in the water heating with Semen Vitis viniferae and obtain vat liquor, replace 70% alcohol to obtain vat liquor in 24 hours 65 ℃ of following lixiviates, saved a large amount of edible ethanols, the consumption of product and alcohol is than being reduced to 1: 2 by 1: 8.C. simplified operation sequence, alleviated labour intensity, reduced steam economy, two of b, c have reduced production cost.D. remove residue with centrifugally operated and replace screen filtration and secondary depositing in water, not only operating effect is good, and weak point consuming time, foreshortens to 16 hours from 53 hours during the chief engineer.
Embodiment
Raw material is selected from winery's system tankage-Semen Vitis viniferae after drinking in Xinjiang and Shandong.
Embodiment 1:
1, lixiviate: get fair Semen Vitis viniferae raw material, be incorporated in the water of 5 times of raw material weights, heat to 95 ℃, keep 95 ℃-98 ℃ 4 hours, get win time vat liquor of juice; Mend 3 times of water again, be warming up to 95 ℃, keep 95 ℃-98 ℃ 2 hours, obtain vat liquor for the second time, merge the secondary vat liquor.
2, centrifugal: as will to be cooled to 50 ℃-70 ℃ vat liquor, and to use the whizzer centrifugally operated, and remove fine particle, residue.
3, cross post: the centrifugate below 50 ℃ is pumped into the pillar that is filled with macroporous resin, adopt PN100 model resin to carry out the polyphenol selective adsorption, non-adsorbable impurity flows out pillar with water.Centrifugate is all flowed through behind the resin column, pumps into the deionized water rinsing macroporous resin, and the alcohol with 50% concentration washes again, elutriant.
4, concentrate: elutriant with 0.4-0.6Mpa, 60 ℃ of-70 ℃ of recovered alcohols, is concentrated to degree Beaume 14-16 ° with elutriant, gets concentrated solution.
5, extraction: divide secondary to add the ethyl acetate extraction secondary of 2-3 times of concentrated solution volume, after merging extraction fluid, ethyl acetate is reclaimed in the deionized water distillation that adds 1 times of concentrated solution volume, reclaims ethyl acetate and can carry out in still kettle, gets the spissated highly purified polyphenol aqueous solution.
6, dust: above-mentioned polyphenol concentrated solution is pumped into spray-drying tower spraying, 220 ℃ of spray-drying tower inlet temperature, 105 ℃-107 ℃ of air outlet temperatures are dried to the grape seed polyphenols fine powder of good fluidity, detect qualified packing.
Embodiment 2:
1, lixiviate: select the first-class Semen Vitis viniferae raw material of quality, be incorporated in the water of 7 times of raw material weights, heat to 95 ℃, keep 98 ℃ 4 hours, get win time vat liquor of juice; Mend 5 times of water again, be warming up to 95 ℃, keep 98 ℃ 2 hours, get juice and get vat liquor for the second time, add the washing slag of 1 times of raw material weight thereafter again, get washings, merge secondary juice and washings at last and get vat liquor.
2, centrifugal: with among the embodiment 12.
3, cross post: the centrifugate below 50 ℃ is pumped into macroporous resin column, adopt PN700 model resin to the polyphenol selective adsorption, non-adsorbable impurity flows out pillar with water, centrifugate is all flowed through behind the resin, pump into the deionized water rinsing macroporous resin, carry out wash-out with the 50% concentration alcohol that is equivalent to raw material weight again, get elutriant.
4, concentrate: with among the embodiment 14.
5, extraction: with the ethyl acetate extraction of 3 times of concentrated solution volumes, with the ethyl acetate extraction of 2 times of concentrated solution volumes, during extraction, heat while stirring for the second time for the first time, leave standstill after the mixing, natural layering, polyphenol enter in the ethyl acetate on upper strata; Impurity is stayed in the following water layer, discards with water.Thereafter in the ethyl acetate that is dissolved with polyphenol that merges, add the deionized water of concentrated solution volume before being equivalent to extract, in still kettle, reclaim ethyl acetate.
6, dust: with among the embodiment 16.
Get the grape seed polyphenols product of content more than 90%.
Embodiment 3:
1, lixiviate: selected high-quality Semen Vitis viniferae raw material, be incorporated in the water of 9 times of raw material weights, heat to 95 ℃, keep 98 ℃ 4 hours, get win time vat liquor of juice; Mend 6 times of water again, be warming up to 95 ℃, keep 98 ℃ 2 hours, get juice and get vat liquor for the second time; Thereafter add the washing slag of 1 times of raw material weight again, get washings, merge secondary juice and washings at last and get vat liquor.
The 2-6 operation is with 2-6 among the embodiment 2.Obtain the high-quality grape seed polyphenols product of content more than 95%.
Embodiment 4:
If wish to get the grape seed polyphenols of content 80-85%, embodiment 1 can be omitted extraction process, the concentrated solution behind the recovered alcohol in the 4th procedure is directly entered spray-dired operation get final product.
Claims (4)
1. a preparation technology of grape seed polyphenols is characterized in that, its concrete operation is as follows:
1. lixiviate: the Semen Vitis viniferae raw material is added 5-9 doubly to raw material weight water, heats to 95 ℃, keep 95 ℃-98 ℃ 4 hours, get the juice time leach liquor of winning; Mend 3-6 times of water again, be warming up to 95 ℃ again, keep 95 ℃-98 ℃ 2 hours, obtain leach liquor for the second time, merge the secondary leach liquor and get vat liquor;
2. centrifugal: as, to carry out centrifugally operated and remove fine particle, residue with 50 ℃-70 ℃ vat liquor;
3. cross post: with the centrifugate below 50 ℃, advance macroporous resin column, carry out the polyphenol selective adsorption, behind the washed resin, wash with concentration 40-60% alcohol again, get elutriant;
4. concentrate: elutriant at vacuum tightness 0.4-0.6Mpa, 60 ℃ of-70 ℃ of recovered alcohols, is further concentrated, get concentrated solution; Perhaps:
Concentrate: elutriant at vacuum tightness 0.4-0.6Mpa, 60 ℃ of-70 ℃ of recovered alcohols, is further concentrated, get concentrated solution;
Again this concentrated solution is implemented extraction process: divide secondary to add the ethyl acetate extraction secondary of 2-3 times of concentrated solution volume, abandon water layer, behind the merging secondary acetic acid ethyl acetate extract, add the pure water or the deionized water of the concentrated solution volume before being equivalent to extract, ethyl acetate is reclaimed in distillation, gets the polyphenol concentrated solution;
5. dust: above-mentioned concentrated solution or polyphenol concentrated solution are pumped into the spray-drying tower spraying, 215 ℃-225 ℃ of spray-drying tower inlet temperature, 105 ℃-107 ℃ of air outlet temperatures are dried to the grape seed polyphenols fine powder of good fluidity, detect qualified back and pack.
2. preparation technology of grape seed polyphenols as claimed in claim 1 is characterized in that, the 1. the temperature of the heating Semen Vitis viniferae described in the procedure and water keep 98 ℃.
3. preparation technology of grape seed polyphenols as claimed in claim 1, it is characterized in that, described extraction is earlier with 3 times of ethyl acetate extractions to the concentrated solution volume, use 2 times of ethyl acetate extractions again to the concentrated solution volume, after merging the secondary ethyl acetate layer, the pure water or the deionized water that add 1 times of polyphenol concentrated solution volume before the extraction in the ethyl acetate solution of polyphenol, ethyl acetate is reclaimed in distillation, must change water-soluble high purity grape seed polyphenols solution.
4. as claim 1 or 3 described preparation technology of grape seed polyphenols, it is characterized in that described distillation recovery ethyl acetate is carried out in common still kettle, ethyl acetate exports through still kettle top and reclaims through condensation, promptly stay the grape seed polyphenols that changes water-soluble in the still, enter the operation of dusting thereafter.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2005100606031A CN1923831B (en) | 2005-09-01 | 2005-09-01 | Preparation technology of grape seed polyphenols |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2005100606031A CN1923831B (en) | 2005-09-01 | 2005-09-01 | Preparation technology of grape seed polyphenols |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1923831A CN1923831A (en) | 2007-03-07 |
CN1923831B true CN1923831B (en) | 2011-07-06 |
Family
ID=37816671
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN2005100606031A Expired - Fee Related CN1923831B (en) | 2005-09-01 | 2005-09-01 | Preparation technology of grape seed polyphenols |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN1923831B (en) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102228256A (en) * | 2011-06-10 | 2011-11-02 | 江苏国银投资有限公司 | Method for producing grape seed extract |
CN102628227A (en) * | 2012-03-29 | 2012-08-08 | 江南大学 | Grape-seed-based ecological preparation method for ultravioresistant woolen and silk textiles |
CN103435661A (en) * | 2013-08-13 | 2013-12-11 | 新疆西部牧业股份有限公司 | Extraction method for grape seed polyphenols |
CN105669780A (en) * | 2016-01-14 | 2016-06-15 | 张敬明 | Method for raising polyphenol content and water-solubility of grape seed extract |
CN110960459A (en) * | 2019-12-18 | 2020-04-07 | 宁波杰顺生物科技有限公司 | Grape seed extract and preparation method thereof |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0348781A2 (en) * | 1988-06-28 | 1990-01-03 | TECNOFARMACI S.p.A. | Procyanidol oligomeric fractions, the processes for the preparation thereof and pharmaceutical compositions containing them |
US5484594A (en) * | 1988-06-28 | 1996-01-16 | Tecnofarmaci S.P.A. | Process for preparing grapeseed extracts enriched in procyanidol oligomers |
US5912363A (en) * | 1997-08-29 | 1999-06-15 | Interhealth Nutraceuticals | Method for extraction of proanthocyanidins from plant material |
US6479081B2 (en) * | 1997-12-30 | 2002-11-12 | Ferco | Method for obtaining grape tannin, resulting tannin and uses |
US6544581B1 (en) * | 1999-06-22 | 2003-04-08 | Canandaigua Wine Company, Inc. | Process for extraction, purification and enrichment of polyphenolic substances from whole grapes, grape seeds and grape pomace |
-
2005
- 2005-09-01 CN CN2005100606031A patent/CN1923831B/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0348781A2 (en) * | 1988-06-28 | 1990-01-03 | TECNOFARMACI S.p.A. | Procyanidol oligomeric fractions, the processes for the preparation thereof and pharmaceutical compositions containing them |
US5484594A (en) * | 1988-06-28 | 1996-01-16 | Tecnofarmaci S.P.A. | Process for preparing grapeseed extracts enriched in procyanidol oligomers |
US5912363A (en) * | 1997-08-29 | 1999-06-15 | Interhealth Nutraceuticals | Method for extraction of proanthocyanidins from plant material |
US6479081B2 (en) * | 1997-12-30 | 2002-11-12 | Ferco | Method for obtaining grape tannin, resulting tannin and uses |
US6544581B1 (en) * | 1999-06-22 | 2003-04-08 | Canandaigua Wine Company, Inc. | Process for extraction, purification and enrichment of polyphenolic substances from whole grapes, grape seeds and grape pomace |
Non-Patent Citations (6)
Title |
---|
何钊,任其龙.层析法分离葡萄籽中原花青素的研究.食品科学25 8.2004,25(8),70-73. |
何钊,任其龙.层析法分离葡萄籽中原花青素的研究.食品科学25 8.2004,25(8),70-73. * |
孙芸,谷文英.大孔吸附树脂对葡萄籽原花青素的吸附研究.离子交换与吸附19 6.2003,19(6),561-566. |
孙芸,谷文英.大孔吸附树脂对葡萄籽原花青素的吸附研究.离子交换与吸附19 6.2003,19(6),561-566. * |
李润丰,吕晓玲,王青华, 刘海燕.葡萄籽中原花色素提取和分离的初步研究.粮油加工与食品机械 6.2003,(6),67-69. |
李润丰,吕晓玲,王青华, 刘海燕.葡萄籽中原花色素提取和分离的初步研究.粮油加工与食品机械 6.2003,(6),67-69. * |
Also Published As
Publication number | Publication date |
---|---|
CN1923831A (en) | 2007-03-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN100564373C (en) | From tea tree, extract the complete processing of tea-polyphenol | |
CN101648980B (en) | Method for combined preparation of pineapple polyphenol and juice by taking pineapple peel as main material and application thereof | |
CN103265520B (en) | Method for preparing oligomeric proanthocyanidins and tannin pigment from grape seeds after winemaking | |
CN104086614B (en) | A kind of preparation method being applicable to industrial Fructus Monordicae extract | |
CN107397103A (en) | A kind of preparation method of Momordica grosvenori decolouring flavor inspissated juice | |
CN103468020A (en) | Blueberry pigment extraction method | |
CN1923831B (en) | Preparation technology of grape seed polyphenols | |
CN101423538A (en) | Production process for extracting high-purity birutan from flos sophora | |
CN101829210B (en) | Method for preparing apple polyphenol | |
CN101467576A (en) | Method for processing instant green tea powder | |
CN102106877B (en) | Production process of gingko leaf extract | |
CN104059163A (en) | Novel method for preparing Qinghai Qaidam lycium barbarum polysaccharide in extraction and separation manner | |
CN1923830B (en) | Preparation process of pine bark proanthocyanidin | |
CN106491458A (en) | A kind of preparation method and applications of tea polyphenols condensed cream | |
CN104098633B (en) | Method for extracting anthocyanin from huckleberry | |
CN102093748A (en) | Method for preparing radish red pigment homopolymer and radish proanthocyanidin from red-core radishes | |
CN105693678A (en) | Method for extracting procyanidine from grape seeds | |
CN105055563A (en) | Method for extracting jujube pit flavone on basis of steam explosion | |
CN101433322B (en) | Functional food rich in anthocyanidin and preparation method thereof | |
CN103254321A (en) | Method for extracting and purifying Phellinus vaninii polysaccharides of medicinal fungus Phellinus vaninii | |
CN105362346A (en) | Method for preparing high-purity cortex magnoliae officinalis total phenols from cortex magnoliae officinalis peel | |
CN107151259B (en) | The method that solid residue after a kind of pair of citrus pectin extraction is comprehensively utilized | |
CN104983778A (en) | Method for continuously and comprehensively extracting liquorice ingredient with high pressure | |
CN109293728A (en) | A kind of green low cost preparation method of high-purity tea saponin | |
CN106045959B (en) | A kind of method that glucosidase procyanidins are prepared using grape seed extract |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110706 Termination date: 20140901 |
|
EXPY | Termination of patent right or utility model |