CN102228256A - Method for producing grape seed extract - Google Patents
Method for producing grape seed extract Download PDFInfo
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- CN102228256A CN102228256A CN 201110154827 CN201110154827A CN102228256A CN 102228256 A CN102228256 A CN 102228256A CN 201110154827 CN201110154827 CN 201110154827 CN 201110154827 A CN201110154827 A CN 201110154827A CN 102228256 A CN102228256 A CN 102228256A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 229940087603 grape seed extract Drugs 0.000 title claims abstract description 19
- 235000002532 grape seed extract Nutrition 0.000 title claims abstract description 19
- 239000001717 vitis vinifera seed extract Substances 0.000 title claims abstract description 19
- 241000219095 Vitis Species 0.000 claims abstract description 44
- 235000009754 Vitis X bourquina Nutrition 0.000 claims abstract description 44
- 235000012333 Vitis X labruscana Nutrition 0.000 claims abstract description 44
- 235000014787 Vitis vinifera Nutrition 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000000284 extract Substances 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 13
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- 238000000605 extraction Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
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- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 238000004587 chromatography analysis Methods 0.000 claims description 8
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- 235000013824 polyphenols Nutrition 0.000 abstract description 20
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- 150000001875 compounds Chemical class 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
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- 229930014669 anthocyanidin Natural products 0.000 description 4
- 150000001452 anthocyanidin derivatives Chemical class 0.000 description 4
- 235000008758 anthocyanidins Nutrition 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
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- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
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Images
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- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention provides a method for producing a grape seed extract, which comprises the following steps: (1) separation: immediately separating grape dregs, which are produced in a wine preparation process, grape juice production process or any other grape working process without fermentation, into grape skin, grape seed and scrap; and (2) extraction: A. extraction: extracting by using alcohol and water as an extraction solvent under the conditions of low oxygen content, low humidity and high pressure, wherein the ratio of water to alcohol is 30:70, and the ratio of grape seed to solvent is 1:10; B. concentration: concentrating the liquid part in a concentrator to eliminate the water phase; and C. drying: drying the concentrated eluate or any product from the concentrator. The invention has the following advantages: before any fermentation situation occurs, the seed and skin in the grapes can be directly separated; in the obtained extract, the content of polyphenols is high, and the content of monomeric substances is low; and by referring to the scrap extraction process, the grape seed can also be used for producing grape seed oil.
Description
Technical field
The present invention relates to a kind of method of producing grape seed extract, belong to food processing technology field.
Background technology
In food production, polyphenol is very useful as compound or additive, and plays an important role for high concentration, high-purity and production cheaply.About the influence of more raw-material factors and these factors, become the research object of a plurality of research projects, for example: stress induced (Cantos E, calendar year 2001 to polyphenol quality and quantity in the plant; Rivero R M, calendar year 2001), maturity (Lattanzio V, calendar year 2001; Gooding P S, calendar year 2001; Kennedy J A, 2000; Chevalier T, 1999; Murata M, 1997; Joy R W 4
Th, nineteen ninety-five) and cultivated form (Chang S, 2000; Sanoner P, 1999) etc. the influence of different factors.
Up to now, still lack the understanding that key factor is exerted an influence.Key factor has a lot, for example originally plays the raw material of centrifugation because fermentation produces alcohol (stack raw material or having that brew grape wine produces the alcohol waste residue under the situation of grape pip before processing raw material, all can cause fermentation)
Other factors of not verifying then are to constitute between the quality and quantity of polyphenol in organic the cultivating plants, and exist what kind of relevance.
In relatively lacking organic the cultivating plants of synthetic, there are maturity mentioned above, cultivated form sometimes simultaneously and from the pressure of pathogen aspect.In the special organic grape juice made that cultivates plants, the content of monomer polyphenol is lower, and especially catechol or epicatechol are two principal monomer compositions of grape pip.
Content of monomer is lower, and organic grape juice of making of cultivating plants is had than the better characteristics of other products (as containing green-tea extract) that are rich in monomer on the market, can avoid not wishing the side effect that occurs simultaneously.
Can find that all kinds of polyphenol in the phytobiocoenose exist with monomeric form, or exist, or exist with the condensate of HMW (HWMP) with the oligomer of low-molecular-weight (LWMP).All kinds of extracts all can influence the quality of end product largely.
For example, the polyphenol extract of plant-derived group, the influence (Garcia L A, 1985 years that are subjected to factors vary such as temperature, acid-base value; Molinelli A, 2002; Scalia S, 1999).The extracting method difference of using, quality and quantity also different (Saucier C, calendar year 2001 of extracting product; Wu T, 2002).
Because relevant (National Library of Medicine (2000a) the chemical carcinogenesis research information system of consumption of some species with some mutagenesis risk, be positioned at Maryland State Bei Saisida, in July, 2000 search [recording mechanism: 1960,3256,6855,7097,7127]), thereby a key factor is exactly to extract the content that phase process is controlled some monomer at all.
Concern and development thereof to the polyphenol extract that is derived from grape pip are confirmed by several patents.People's such as Yokohama invention (U.S. Patent number is 4320200) discloses a kind of method that obtains the anthocyanidin colouring agent from natural prodcuts such as grape, that is: mix with sulphite at the following raw material of at least 85 ℃ of conditions.A kind of method that obtains polyphenol extract from Grape Skin is developed in people's such as Hilton invention (U.S. Patent number is 4320009), also promptly prepares a kind of water extract earlier, and elution is carried out in further absorption on ion exchange resin then again; In case of necessity, at last at paper or the enterprising step chromatography of thin layer silica gel.
Make the polyphenol concentration that obtains in this way lower.XiLi Ke Han top grade people's invention (U.S. Patent number is 4452822), a kind of method of extracting anthocyanidin from treaster or other sources is disclosed, that is: handle with enzyme after, extract with sulfur dioxide again, thereby remove the solid matter that exists in the extract.People's such as Crosby invention (U.S. Patent number is 4481223) has proved that tannic acid can be used for the fixed extraction thing.Lanace people's invention (U.S. Patent number is 4500556) such as pause relates to sulfurous acid (H
2SO
3) handle treaster, make a kind of compound, the removal process of this compound relates to nonionic sorbent treatment extract, to adsorb this compound.Use the water treatment adsorbent bed then, remove water-soluble substanceses such as carbohydrate, organic acid and solid particle.And then use through the organic solvent of acidifying elution compound from the adsorbent bed, make the anthocyanidin polymerization by elution at last.The solvent that uses in this method preferably carries out 100% alcohol of acidifying with small amounts of inorganic acid, to destroy compound, do not contain sulfurous acid (H in the anthocyanidin thereby make
2SO
3).
The invention of Ford (U.S. Patent number is 5141611), use a kind of polyamide, control its porous and surface, so that from extract, remove polyphenol substance, from grape pip, extract most flavones and need a kind of technology, especially when we need select some molecular groups, this technology can realize separating very accurately.
In these patents, the patent of Indena is best (by people's such as Fu Langji invention, U.S. Patent number is 5484594), and this patent can selected polyphenol extract, and removes and produce unnecessary most of monomer originally.This method uses multiple solvent to make concentrated type glucosidase procyanidins extract, and wherein employed solvent has: acetone and methyl alcohol (as primary solvent), ethyl acetate, carrene and dichloroethanes.The major defect that this method exists is as follows: 1) use all kinds of solvents, cause extracting the OPC of multiple beneficial; 2) the required step of this method is more, as filtration and hatching, and the length that therefore expends time in, and also workload is big; 3) use carcinogenic chlorinated solvents, can cause all kinds of pollution problems and industrial hygiene problem; 4) do not forming under the situation of azeotropic mixture, it is impossible thoroughly removing acetone, methyl alcohol or acetate; 5) all extract flow process all from containing the treaster of skin and seed, and these flow processs are all passed through the alcohol device, and the latter can remove alcohol by all substrates; The refuse that this method produces is delivered to drier and is carried out the drying processing, humidity is reduced to about 4%, on separation filter screen or seed singulator, skin and seed are separated then, when removing alcohol, also extracted polyphenol, and owing to cause content of monomer to increase through drier; 7) under normal conditions, last treatment step carries out under hot conditions, and the duration is short, is intended to the production time is reduced to the shortest, and reduces cost.Because the grape pip that uses in these flow processs is with low quality, therefore these grape pips are used as the burning things which may cause a fire disaster of drier usually, or owing to unsaturated oils content height in the grape pip is used to produce grape-kernel oil, up to now, form practical method as yet, from grape pip, to extract polyphenol selectively and to reduce the content of monomer polyphenol.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, a kind of method of producing grape seed extract is provided.
The method of production grape seed extract of the present invention comprises the following steps:
1) separating step: the treaster with producing in grape wine preparation, grape juice production or any other the grape process that need not to ferment is separated into Grape Skin, grape pip and waste material immediately;
2) extraction step:
A, extraction: use alcohol and water as extractant, water and alcohol ratio are 30:70, and the ratio of grape pip and solvent is 1:10, extracts under the environment of low oxygen content, low humidity and high pressure;
B. concentrate: in inspissator, liquid is partly concentrated, to eliminate water;
C. dry: that eluate that concentrates or the spawn that is derived from inspissator are carried out drying.
Preferably, step 1) and step 2) between also comprise the dry treatment step of grape pip, the moisture after the processing is 2-3%.
Described dry processing is under 30-120 ℃ condition, adopts hot-air drier to carry out.
Comprise that also chromatography purifies before the concentrating step 2), said chromatography is to carry out chromatography to purify on polystyrene resins such as XAD-16, XAD-4 and CIAION HP-20.
Used separating tool is single-stage or multistage oscillating separator or seed seperator in the step 1).
Whether no matter the method for production grape seed extract of the present invention ferment the treaster that produces in grape wine preparation, grape juice production or any other grape process, all is separated into Grape Skin, grape pip and waste material; Used separating tool is single-stage or multistage oscillating separator or seed seperator; After processing, should separate immediately, to avoid or to stop fermentation, because fermentation may reduce the concentration of polyphenol.Make in this way, can save all and remove the alcohol process, or preventative dry the processing, therefore this method has tangible economic advantages, and obviously, the grape pip to separate need not to separate again.The Grape Skin of having processed can also be as other purposes.If necessary, with removing the alcohol device Grape Skin is removed the alcohol processing.The grape pip that has separated can carry out drying with drier to be handled, and hot-air drier is very useful, because the burning bonnet of these hot-air driers can be avoided discharging, thereby avoids polluting hydrocarbon or other organic or inorganics source.Dry processing should be carried out under 30-120 ℃ of condition, humidity up to raw material reaches the value that 2-30% maybe can avoid bacterium, saccharomycete or any other microbial growth, because these bacteriums, saccharomycete or any other microorganism can cause product fermentation or other any type of qualities to worsen.
If the grape pip that separates is extracted immediately, can omit dry the processing, the grape pip of gained can be used as any other purposes, comprises the production of grape-kernel oil or without the production that separates grape seed extract.For content of monomer low the production of extract, should be can from phytobiocoenose, extracting relevant any solvent as extracting raw material, in the case, preferably water and alcohol are mixed (mixed proportion is 30:70), wherein the ratio of grape pip and liquid is 1:10, up to the maximum extracted ability that obtains solvent.
Extract and handle and can carry out under the condition of low oxygen content, low humidity and high pressure, isolate useless grape pip then from liquid, the latter can be used for other any purposes, comprises the production grape-kernel oil.
Then liquid is concentrated, remove nonaqueous phase, thereby can use polystyrene resins such as XAD-16, XAD-4 or DIAION HP-20 pair and resulting product to carry out chromatography purifies, as need not to purify, then should concentrate, so that reclaim eluate or product is concentrated to eluate or from the product of inspissator, other any technologies of using spray-drying maybe can obtain particulate are then proceeded dry the processing, products therefrom, the polyphenol content height, content of monomer is low.
The nutritional labeling that extract of the present invention can be used for preparing additive or is used as Foods or drinks can also be mixed with green-tea extract, and formation is rich in monomer but is not had any genotoxic mixture.
The method of production grape seed extract of the present invention has following technique effect:
1) before any fermentation appearance takes place, seed and skin in the processing grape directly can be separated;
2) polyphenol content height in the extract that obtains of the present invention, monomeric substance content are low;
3) the present invention utilizes grape pip can produce grape-kernel oil also with reference to the refuse extraction process.
Description of drawings
Fig. 1 is the HPLC-TV chromatogram of grape seed extract of the present invention;
Fig. 2 is the method flow diagram of grape seed extract of the present invention.
The specific embodiment
Embodiment 1 produces grape seed extract
The method of the production grape seed extract of present embodiment may further comprise the steps:
1) uses two-sided separator, the filter press gained treaster that is used to produce biological red grape juice is separated, continue 72 hours;
2) be not higher than under 60 ℃ of conditions, with the dry gained grape pip of thermal current drier about 4 hours, reaching 7% up to the humidity of grape pip;
3) the gained grape pip is handled under 40-50 ℃ of condition with the mixture (70:30) of alcohol and water, divided four cycles, weekly 1 hour phase, the ratio of its Chinese traditional medicine and solvent is 1:3, use filter screen to reclaim residual grape pip, concentrate liquid phase, to remove alcohol; The alcohol that reclaims can be used for other leaching process once more;
4) water that will contain main extract places spray dryer, is no more than 35% primary product to obtain the polyphenol total content, also can use the HP-20 chromatogram to purify, and uses 70% alcohol to carry out extracting then.
5) gained liquid is concentrated, be placed on spray dryer then, be higher than 70% purified product to obtain the polyphenol total content.
The component of the grape seed extract of producing of present embodiment and content are shown in the HPLC-TV chromatogram of Fig. 1.
Claims (5)
1. a method of producing grape seed extract is characterized in that, comprises the following steps:
1) separating step: the treaster with producing in grape wine preparation, grape juice production or any other the grape process that need not to ferment is separated into Grape Skin, grape pip and waste material immediately;
2) extraction step:
A, extraction: use alcohol and water as extractant, water and alcohol ratio are 30:70, and the ratio of grape pip and solvent is 1:10, extracts under the environment of low oxygen content, low humidity and high pressure;
B. concentrate: in inspissator, liquid is partly concentrated, to eliminate water;
C. dry: that eluate that concentrates or the spawn that is derived from inspissator are carried out drying.
2. production grape seed extract method according to claim 1 is characterized in that step 1) and step 2) between also comprise the dry treatment step of grape pip, the moisture after the processing is 2-3%.
3. the method for production grape seed extract according to claim 2 is characterized in that, described dry processing is under 30-120 ℃ condition, adopts hot-air drier to carry out.
4. production grape seed extract method according to claim 1 is characterized in that step 2) concentrate before comprise that also chromatography purifies, said chromatography is to carry out chromatography to purify on polystyrene resins such as XAD-16, XAD-4 and CIAION HP-20.
5. according to any described production grape seed extract of claim method among the claim 1-4, it is characterized in that used separating tool is single-stage or multistage oscillating separator or seed seperator in the step 1).
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|---|---|---|---|
| CN 201110154827 CN102228256A (en) | 2011-06-10 | 2011-06-10 | Method for producing grape seed extract |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110154827 CN102228256A (en) | 2011-06-10 | 2011-06-10 | Method for producing grape seed extract |
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| CN102228256A true CN102228256A (en) | 2011-11-02 |
Family
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| CN 201110154827 Pending CN102228256A (en) | 2011-06-10 | 2011-06-10 | Method for producing grape seed extract |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104706834A (en) * | 2013-12-13 | 2015-06-17 | 中国农业科学院农产品加工研究所 | Polyphenol preparation method and beverage production method |
| CN105533857A (en) * | 2016-01-18 | 2016-05-04 | 广西大学 | Antibacterial and breathable composition for anti-haze mask |
| CN105661215A (en) * | 2015-10-12 | 2016-06-15 | 华中农业大学 | Whole kiwi fruit juice and processing method thereof |
| CN109952110A (en) * | 2016-05-24 | 2019-06-28 | 莱里达大学 | Method for obtaining tannin extract isolated from grapes, obtained tannin extract and use thereof |
| CN118026981A (en) * | 2024-01-29 | 2024-05-14 | 宁波天鼎生物科技有限公司 | Preparation method of grape seed extract with low folpet residues |
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| CN1506362A (en) * | 2002-12-06 | 2004-06-23 | 沈阳中科药业公司 | Resin process of extracting proanthocyanidin from graup seed |
| CN1923831A (en) * | 2005-09-01 | 2007-03-07 | 浙江瑞康生物技术有限公司 | Preparation technology of grape seed polyphenols |
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| CN1506362A (en) * | 2002-12-06 | 2004-06-23 | 沈阳中科药业公司 | Resin process of extracting proanthocyanidin from graup seed |
| CN1923831A (en) * | 2005-09-01 | 2007-03-07 | 浙江瑞康生物技术有限公司 | Preparation technology of grape seed polyphenols |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104706834A (en) * | 2013-12-13 | 2015-06-17 | 中国农业科学院农产品加工研究所 | Polyphenol preparation method and beverage production method |
| CN105661215A (en) * | 2015-10-12 | 2016-06-15 | 华中农业大学 | Whole kiwi fruit juice and processing method thereof |
| CN105533857A (en) * | 2016-01-18 | 2016-05-04 | 广西大学 | Antibacterial and breathable composition for anti-haze mask |
| CN109952110A (en) * | 2016-05-24 | 2019-06-28 | 莱里达大学 | Method for obtaining tannin extract isolated from grapes, obtained tannin extract and use thereof |
| CN109952110B (en) * | 2016-05-24 | 2022-03-18 | 莱里达大学 | Method for obtaining tannin extract isolated from grapes, tannin extract obtained and use thereof |
| CN118026981A (en) * | 2024-01-29 | 2024-05-14 | 宁波天鼎生物科技有限公司 | Preparation method of grape seed extract with low folpet residues |
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