CN102851114A - Method for extracting grape seed oil and proanthocyanidin - Google Patents
Method for extracting grape seed oil and proanthocyanidin Download PDFInfo
- Publication number
- CN102851114A CN102851114A CN 201210353608 CN201210353608A CN102851114A CN 102851114 A CN102851114 A CN 102851114A CN 201210353608 CN201210353608 CN 201210353608 CN 201210353608 A CN201210353608 A CN 201210353608A CN 102851114 A CN102851114 A CN 102851114A
- Authority
- CN
- China
- Prior art keywords
- extraction
- pycnogenols
- oil
- reagent
- grape seed
- 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.)
- Pending
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for efficiently and quickly extracting grape seed oil and proanthocyanidin, which comprises the following steps: 1) pulverizing grape seed, adding the pulverized grape seed into a subcritical extraction kettle, introducing a nonpolar organic reagent, dynamically extracting at 20-80 DEG C under the pressure of 0.3-5 MPa for 20-80 minutes, recycling the reagent from the extract, and adding atlapulgite and activated carbon for decolorization and deodorization, thereby obtaining the grape seed oil; and 2) introducing a polar organic reagent or water into the extraction residue, dynamically extracting at 20-150 DEG C under the pressure of 0.3-8 MPa for 30-90 minutes, recycling the reagent from the extract, adding into a macroporous resin column for adsorption, carrying out gradient elution with an ethanol solution, concentrating the eluate, and carrying out spray drying to obtain the proanthocyanidin. The method disclosed by the invention has the advantages of low energy consumption, low solvent volume and high product yield, and is suitable for industrialized popularization.
Description
Technical field
The present invention relates to the method for a kind of extraction of oil from grape seeds and pycnogenols, particularly a kind of method of utilizing subcritical fluid extraction grape seed oil and pycnogenols.
Background technology
Semen Vitis viniferae is the seed of grape, contains to enrich various greases, polyphenol, VITAMIN and mineral substance etc., has superpower antioxygenation, is widely used in beauty treatment, health care.Wherein research finds that linolenic acid can be resisted free radical in the raisin seed oil, and is anti-aging; help vitamins C and E, strengthen the elasticity of the recycle system, reduce ultraviolet injury; collagen protein in the protection skin improves venous engorgement and oedema, the prevention melanin deposition.Proanthocyanidins from Grape Seeds (OPC) is a kind of efficient free-radical scavengers.The oxidative function of its Green Tea Extract is 50 times, ascorbic 20 times of vitamin-E.Can remove poisonous free radical in the human body, the protection human cell tissue exempts to be prevented the diseases relevant with free radical of kind more than 80 such as allergy, cancer, aging by the oxidative damage of free radical.
Mostly oil and grease extracting is to adopt squeezing, normality lixiviate or supercritical CO from Semen Vitis viniferae
2Extraction.Antioxidant component destroys seriously in squeezing, the many Semen Vitis viniferaes of normality lixiviate, especially the pycnogenols in the Semen Vitis viniferae.And supercritical CO
2Extracting process is efficient, environmental protection, but equipment manufacturing cost is high, is difficult to realize large production.Seed extracting procyanidins method also is to adopt the Semen Vitis viniferae normality extraction processed grease, and extraction temperature is crossed and lowly caused easily that yield is low, the cycle is long, and the extraction temperature height easily causes the pycnogenols oxygenolysis.If employing supercritical CO
2Extraction also be to be difficult to large production, and the pycnogenols molecular weight in the Semen Vitis viniferae is larger, and polarity is stronger, also is to be difficult to extraction fully even add entrainment agent.The technique of extraction of oil from grape seeds and pycnogenols is less from Semen Vitis viniferae simultaneously.(application number: 200710191255.0) " a kind of from Semen Vitis viniferae single stage method extract the method for raisin seed oil and pycnogenols " disclosed method is that to adopt the Semen Vitis viniferae of pulverizing be raw material such as patent, with getting gently phase and heavy phase extracting solution after the mixed solvent lixiviate, light phase extracting solution gets the Semen Vitis viniferae crude oil behind desolventizing, the heavy phase extracting solution gets the pycnogenols finished product behind macroporous resin purification.This patent employing mixed dissolution extraction time is long, solvent load is larger, can cause production cost too high.(application number: 201110155971.X) " a kind of method of extracting raisin seed oil and pycnogenols " disclosed method is to soak the Semen Vitis viniferae of pulverizing with mixed solvent to get raisin seed oil extracting solution and pycnogenols extracting solution to patent for another example, with the raisin seed oil extracting solution with after the pycnogenols extracting solution separates, the pycnogenols extracting solution gets pycnogenols behind the ultra-filtration membrane purifying, the raisin seed oil extracting solution gets raisin seed oil behind the evaporation desolvation.This patent also adopts constant-pressure and high-temperature to extract, and solvent load is large, and it is poor that there is being selected in property in membrane filtration simultaneously, and product purity is low.
Summary of the invention
The objective of the invention is to solve shortcomings and deficiencies of the prior art, a kind of method of utilizing subcritical fluid extraction raisin seed oil and pycnogenols is provided.
To achieve these goals, the present invention is by the following technical solutions:
The method of a kind of extraction of oil from grape seeds and pycnogenols is characterized in that following steps:
1) Semen Vitis viniferae is pulverized, and drops into the subcritical abstraction still, passes into nonpolar organic reagent, under 20 ~ 80 ℃ of temperature, pressure 0.3 ~ 5MPa condition, dynamic extraction 20-80min, the gained extract reclaims reagent, add again atlapulgite and activated carbon decolorizing deodorization, namely get raisin seed oil;
2) pass into polarity organic reagent or water in the above-mentioned extraction residue under 20 ~ 150 ℃ of temperature, pressure 0.3 ~ 8MPa condition, dynamic extraction 30-90min, the gained extract reclaims reagent, add in the macroporous resin column and adsorb, the ethanolic soln gradient elution, elutriant is concentrated, and spraying drying namely gets pycnogenols.
A kind of in the optional propane of nonpolar organic reagent, butane, dme and the sherwood oil described in the step 1).
Step 2) a kind of in the optional ethyl acetate of polarity organic reagent, acetone, ethanol and the methyl alcohol described in.
Step 2) a kind of among the optional HZ818 of macroporous resin model, the NK-II described in and the ADS-21.
Step 2) ethanol gradient elution described in is 3-5 column volume 10-50% ethanolic soln wash-out impurity, uses 4-7 column volume 60-80% ethanol elution effective constituent again.
Positively effect of the present invention is: adopt subcritical fluid extraction, extract with the normal pressure organic reagent and compare, have advantage with short production cycle, that efficient is high, energy consumption is low, and the solvent capacity is few, the extraction process product is oxygenolysis not; With overcritical and extraction phase ratio, have industrialization degree height, advantage that production cost is low.Whole technique is extracted continuously, obtains simultaneously two kinds of products, has reduced production cost, has improved raw material availability.
Embodiment
Embodiment 1:
Get Semen Vitis viniferae 1kg, pulverize, drop into the subcritical abstraction still, pass into propane, under 40 ℃ of temperature, pressure 4MPa condition, dynamic extraction 30min, the gained extract reclaims reagent, adds 10g atlapulgite and activated carbon decolorizing deodorization again, gets raisin seed oil 120g.In residue, pass into water, under 140 ℃ of temperature, pressure 0.5MPa condition, dynamic extraction 40min, the gained extract is chilled in the normal temperature adding HZ818 macroporous resin column and adsorbs, 3 column volumes, 50% ethanolic soln wash-out impurity, use 4 column volumes, 80% ethanol elution effective constituent, elutriant is concentrated again, and spraying drying namely gets pycnogenols 40g.Content 95%.
Embodiment 2:
Get Semen Vitis viniferae 1kg, pulverize, drop into the subcritical abstraction still, pass into butane, under temperature 60 C, pressure 4MPa condition, dynamic extraction 50min, the gained extract reclaims reagent, adds 20g atlapulgite and activated carbon decolorizing deodorization again, gets raisin seed oil 109g.In residue, pass into 70% ethanol, under 120 ℃ of temperature, pressure 1MPa condition, dynamic extraction 40min, the gained extract reclaims reagent, add in the NK-II macroporous resin column and adsorb, ethanol gradient elution is 4 column volumes, 30% ethanolic soln wash-out impurity, uses 5 column volumes, 70% ethanol elution effective constituent again, elutriant is concentrated, and spraying drying namely gets pycnogenols 36g.Content 98%.
Embodiment 3:
Get Semen Vitis viniferae 1kg, pulverize, drop into the subcritical abstraction still, pass into dme, under temperature 50 C, pressure 2MPa condition, dynamic extraction 30min, the gained extract reclaims reagent, adds 15g atlapulgite and activated carbon decolorizing deodorization again, gets raisin seed oil 112g.In residue, pass into ethyl acetate, under 90 ℃ of temperature, pressure 0.3MPa condition, dynamic extraction 40min, the gained extract reclaims reagent, and the suitable quantity of water dilution adds in the ADS-21 macroporous resin column and adsorbs, 4 column volumes, 20% ethanolic soln wash-out impurity, use 4 column volumes, 75% ethanol elution effective constituent, elutriant is concentrated again, and spraying drying namely gets pycnogenols 34g.Content 92%.
Embodiment 4:
Get Semen Vitis viniferae 1kg, pulverize, drop into the subcritical abstraction still, pass into dme, under temperature 50 C, pressure 2MPa condition, dynamic extraction 30min, the gained extract reclaims reagent, adds 15g atlapulgite and activated carbon decolorizing deodorization again, gets raisin seed oil 112g.In residue, pass into 80% acetone soln, under 110 ℃ of temperature, pressure 0.5MPa condition, dynamic extraction 30min, the gained extract reclaims reagent, and the suitable quantity of water dilution adds in the NK-II macroporous resin column and adsorbs, 3 column volumes, 30% ethanolic soln wash-out impurity, use 4 column volumes, 80% ethanol elution effective constituent, elutriant is concentrated again, and spraying drying namely gets pycnogenols 37g.Content 90%.
Claims (5)
1. the method for an extraction of oil from grape seeds and pycnogenols is characterized in that following steps:
1) Semen Vitis viniferae is pulverized, and drops into the subcritical abstraction still, passes into nonpolar organic reagent, under 20 ~ 80 ℃ of temperature, pressure 0.3 ~ 5MPa condition, dynamic extraction 20-80min, the gained extract reclaims reagent, add again atlapulgite and activated carbon decolorizing deodorization, namely get raisin seed oil;
2) pass into polarity organic reagent or water in the above-mentioned extraction residue under 20 ~ 150 ℃ of temperature, pressure 0.3 ~ 8MPa condition, dynamic extraction 30-90min, the gained extract reclaims reagent, add in the macroporous resin column and adsorb, the ethanolic soln gradient elution, elutriant is concentrated, and spraying drying namely gets pycnogenols.
2. the method for extraction of oil from grape seeds according to claim 1 and pycnogenols is characterized in that a kind of in the optional propane of nonpolar organic reagent, butane, dme and the sherwood oil described in the step 1).
3. the method for extraction of oil from grape seeds according to claim 1 and pycnogenols is characterized in that step 2) described in the optional ethyl acetate of polarity organic reagent, acetone, ethanol and methyl alcohol in a kind of.
4. the method for extraction of oil from grape seeds according to claim 1 and pycnogenols is characterized in that step 2) described in the optional HZ818 of macroporous resin model, NK-II and ADS-21 in a kind of.
5. the method for extraction of oil from grape seeds according to claim 1 and pycnogenols, it is characterized in that step 2) described in ethanol gradient elution for 3-5 column volume 10-50% ethanolic soln wash-out impurity, use again 4-7 column volume 60-80% ethanol elution effective constituent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210353608 CN102851114A (en) | 2012-09-21 | 2012-09-21 | Method for extracting grape seed oil and proanthocyanidin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210353608 CN102851114A (en) | 2012-09-21 | 2012-09-21 | Method for extracting grape seed oil and proanthocyanidin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102851114A true CN102851114A (en) | 2013-01-02 |
Family
ID=47398096
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210353608 Pending CN102851114A (en) | 2012-09-21 | 2012-09-21 | Method for extracting grape seed oil and proanthocyanidin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102851114A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173275A (en) * | 2013-03-06 | 2013-06-26 | 曹庸 | Pressing-low-temperature continuous phase-change castor oil extraction method |
| CN103173280A (en) * | 2013-03-06 | 2013-06-26 | 曹庸 | Continuous-phase-change soy sauce residue oil extraction method |
| CN103740460A (en) * | 2014-01-15 | 2014-04-23 | 甘肃农业大学 | Method for extracting and purifying grape seed oil from grape seeds |
| CN103834470A (en) * | 2014-03-04 | 2014-06-04 | 秦广雍 | Method for extracting macadamia nut oil by adopting subcritical extraction technology |
| CN105130941A (en) * | 2015-08-31 | 2015-12-09 | 桂林茗兴生物科技有限公司 | Preparation method of grape seed extract |
| CN105368625A (en) * | 2015-09-18 | 2016-03-02 | 洛阳古草生物科技有限公司 | Flavored wild grape wine and making method thereof |
| CN105675768A (en) * | 2016-04-25 | 2016-06-15 | 广西壮族自治区梧州食品药品检验所 | Method for measuring solvent residues by rapid extraction and ultra-performance liquid chromatography |
| CN107721966A (en) * | 2017-10-30 | 2018-02-23 | 潍坊友容实业有限公司 | A kind of Suaeda salsa anthocyanidin and biogenic salt combined extraction method |
| 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 |
| CN114836258A (en) * | 2022-04-20 | 2022-08-02 | 宁夏松海盛华农林科技开发有限公司 | Method for extracting grape seed oil by using grape seeds after brewing |
-
2012
- 2012-09-21 CN CN 201210353608 patent/CN102851114A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173275A (en) * | 2013-03-06 | 2013-06-26 | 曹庸 | Pressing-low-temperature continuous phase-change castor oil extraction method |
| CN103173280A (en) * | 2013-03-06 | 2013-06-26 | 曹庸 | Continuous-phase-change soy sauce residue oil extraction method |
| CN103173280B (en) * | 2013-03-06 | 2015-03-18 | 曹庸 | Continuous-phase-change soy sauce residue oil extraction method |
| CN103740460A (en) * | 2014-01-15 | 2014-04-23 | 甘肃农业大学 | Method for extracting and purifying grape seed oil from grape seeds |
| CN103740460B (en) * | 2014-01-15 | 2015-06-10 | 甘肃农业大学 | Method for extracting and purifying grape seed oil from grape seeds |
| CN103834470A (en) * | 2014-03-04 | 2014-06-04 | 秦广雍 | Method for extracting macadamia nut oil by adopting subcritical extraction technology |
| CN105130941A (en) * | 2015-08-31 | 2015-12-09 | 桂林茗兴生物科技有限公司 | Preparation method of grape seed extract |
| CN105368625A (en) * | 2015-09-18 | 2016-03-02 | 洛阳古草生物科技有限公司 | Flavored wild grape wine and making method thereof |
| CN105675768A (en) * | 2016-04-25 | 2016-06-15 | 广西壮族自治区梧州食品药品检验所 | Method for measuring solvent residues by rapid extraction and ultra-performance liquid chromatography |
| CN107721966A (en) * | 2017-10-30 | 2018-02-23 | 潍坊友容实业有限公司 | A kind of Suaeda salsa anthocyanidin and biogenic salt combined extraction method |
| 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 |
| CN114836258A (en) * | 2022-04-20 | 2022-08-02 | 宁夏松海盛华农林科技开发有限公司 | Method for extracting grape seed oil by using grape seeds after brewing |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102851114A (en) | Method for extracting grape seed oil and proanthocyanidin | |
| Tan et al. | Extraction and purification of anthocyanins: A review | |
| CN101912480B (en) | Method for preparing procyanidin extract of lycium ruthenicum murr | |
| CN102746415B (en) | Method for simultaneously extracting tea polysaccharide and tea polyphenol with subcritical water | |
| CN103570664B (en) | Method of extracting procyanidine from huckleberries | |
| CN101744886B (en) | Method for extracting high-purity schisandra total lignan | |
| CN103420970A (en) | Method for extracting and purifying anthocyanidin | |
| CN104817527A (en) | Method for extracting anthocyanidin from pitaya peel | |
| CN106810904B (en) | Method for extracting anthocyanin components | |
| CN106632205A (en) | Method for extracting proanthocyanidins from Yunnan pine bark | |
| CN101392008A (en) | Extraction technique of high-purity phlorizin | |
| CN102993154A (en) | Method for extracting purple sweet potato anthocyanin | |
| CN105777698A (en) | Method for purifying pitaya peel anthocyanin | |
| CN103772339B (en) | A kind of method extracting NVP-XAA 723 from tealeaves tankage | |
| CN101386615A (en) | Method for extracting procyanidine from sea-buckthorn seed | |
| CN103483302A (en) | Method for separating and purifying oligomeric proanthocyanidins | |
| CN104095889B (en) | A kind of preparation method of ginkgo biloba p.e | |
| CN103992299B (en) | The method of multiple bioactive ingredients in separation and purification sea-buckthorn seed cake while of a kind of | |
| CN105859674A (en) | Method for extracting dragon fruit peel anthocyanin | |
| CN103012351A (en) | Technology for purifying natural vitamin E | |
| CN102533446B (en) | Method for removing furocoumarins from citrus essential oil | |
| CN101390975A (en) | Extraction method of citrus active ingredient | |
| CN102643261A (en) | Method for extracting cyanidin from blueberry wine residues | |
| CN112480053B (en) | Method for extracting and separating baicalin and baicalein | |
| CN103601713A (en) | Extraction and detection method for oligoprocyanidins in grape seeds |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130102 |