CN1923831A - Preparation technology of grape seed polyphenols - Google Patents
Preparation technology of grape seed polyphenols Download PDFInfo
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- CN1923831A CN1923831A CN 200510060603 CN200510060603A CN1923831A CN 1923831 A CN1923831 A CN 1923831A CN 200510060603 CN200510060603 CN 200510060603 CN 200510060603 A CN200510060603 A CN 200510060603A CN 1923831 A CN1923831 A CN 1923831A
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- water
- grape seed
- ethyl acetate
- vat liquor
- seed polyphenols
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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 after drinking--the Semen Vitis viniferae 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 (8)
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 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, is further concentrated, 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.
2. preparation technology of grape seed polyphenols as claimed in claim 1, it is characterized in that, 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 secondary acetate acetic acid extraction liquid, the pure water or the deionized water that add the concentrated solution volume before being equivalent to extract, ethyl acetate is reclaimed in distillation, gets the polyphenol concentrated solution.
3. preparation technology of grape seed polyphenols as claimed in claim 1 is characterized in that, when 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.
4. preparation technology of grape seed polyphenols as claimed in claim 3, it is characterized in that, the 1. the procedure lixiviate can be in high-quality Semen Vitis viniferae raw material, to add 7 times or 9 times to the water of Semen Vitis viniferae weight, heat to 95 ℃, keep 95 ℃-98 ℃ 4 hours, get win time vat liquor of juice; 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 raw material weight again, get washings, merge secondary vat liquor and washings at last and get vat liquor.
5. as the described preparation technology of grape seed polyphenols of arbitrary claim in the claim 1 to 4, it is characterized in that, the 1. the optimum temps of the heating Semen Vitis viniferae described in the procedure and water keep 98 ℃.
6. preparation technology of grape seed polyphenols as claimed in claim 1, it is characterized in that, 3. the macroporous resin column of advancing described in the procedure carry out the polyphenol selective adsorption, its resin model can be PN100, PN400, CAD40, YWD04B2 or PN700, and the alcohol that obtains elutriant can be 50% concentration.
7. preparation technology of grape seed polyphenols as claimed in claim 2, it is characterized in that, described extraction can be earlier with 3 times of ethyl acetate extractions, use 2 times of ethyl acetate extractions again, 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.
8. as claim 2 or 7 described preparation technology of grape seed polyphenols, it is characterized in that described distillation recovery ethyl acetate can be 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.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005100606031A CN1923831B (en) | 2005-09-01 | 2005-09-01 | Preparation technology of grape seed polyphenols |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2005100606031A CN1923831B (en) | 2005-09-01 | 2005-09-01 | Preparation technology of grape seed polyphenols |
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| CN1923831A true CN1923831A (en) | 2007-03-07 |
| CN1923831B CN1923831B (en) | 2011-07-06 |
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Cited By (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 |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5484594A (en) * | 1988-06-28 | 1996-01-16 | Tecnofarmaci S.P.A. | Process for preparing grapeseed extracts enriched in procyanidol oligomers |
| IT1219732B (en) * | 1988-06-28 | 1990-05-24 | Tecnofarmaci Spa | PROCYANIDOLIC OLIGOMERIC FRACTIONS, THEIR PREPARATION PROCEDURE AND PHARMACEUTICAL COMPOSITIONS CONTAINING THEM |
| US5912363A (en) * | 1997-08-29 | 1999-06-15 | Interhealth Nutraceuticals | Method for extraction of proanthocyanidins from plant material |
| FR2773150B1 (en) * | 1997-12-30 | 2000-03-31 | Ferco | PROCESS FOR OBTAINING GRAPE TANNIN, TANNIN OBTAINED 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
Cited By (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 |
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| CN1923831B (en) | 2011-07-06 |
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