CN105153096A - Method for extracting procyanidins (OPC) from grape seeds - Google Patents
Method for extracting procyanidins (OPC) from grape seeds Download PDFInfo
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- CN105153096A CN105153096A CN201510667523.6A CN201510667523A CN105153096A CN 105153096 A CN105153096 A CN 105153096A CN 201510667523 A CN201510667523 A CN 201510667523A CN 105153096 A CN105153096 A CN 105153096A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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Abstract
The invention provides a method for extracting procyanidins (OPC) from grape seeds. The OPC is extracted by using the grape seeds as the main raw materials and combining an enzymic preparation with a solvent. The preparation method comprises the following steps: material preparation, buffer solution preparation, enzyme liquid preparation, feeding, enzymolysis, extraction and finished product preparation. The OPC prepared by utilizing the method has good product safety and quality and small amount of the enzymic preparation and has an extraction rate 30-40% higher than that in ethanol extraction methods. The method is simple in process, is convenient to operate, has high efficiency and is suitable for industrial production.
Description
Technical field
The invention belongs to natural product processing scientific domain, particularly a kind of method extracting pycnogenols from Semen Vitis viniferae.
Background technology
Be otherwise known as pycnogenols (Procyanidins is called for short OPC) oligomeric flavanone, is a kind of new and effective antioxidant, is the most potent found so far free-radical scavengers, has very strong activity in vivo.Experiment proves, the Green Tea Extract oxidation capacity of OPC is 50 times of vitamin-E, ascorbic 20 times, and absorbs rapidly completely, and within oral 20 minutes, can reach the highest haemoconcentration, metabolic half life is for 7 hours.
Pycnogenols is kind the abundantest in nature phenolic compound, and pycnogenols produces coloured anthocyanidin because there is typical oxidation DeR under acid medium and gains the name.In all kinds of pycnogenols, dimer is the class pycnogenols that is the widest, most study that distributes.Report both at home and abroad a lot about the pharmacotoxicological effect of pycnogenols, the functions such as such as scavenging free radicals, strong anti-oxidation, antitumor and arteriosclerosis; Pycnogenols has also been used for the complication after preventing Operation of Cataract in Diabetics; In addition pycnogenols also serves vital role in plant defense predator and microbial mechanism.So act on widely in view of pycnogenols has, its extracting method also receives the very big concern of domestic and international researchist.Tradition is extracted pycnogenols and is mainly adopted the methods such as organic solvent lixiviate, ultra filtering reverse osmosis separation and resin absorption.Representative extracts pycnogenols with boiling water as US3435407 discloses from Korean pine bark, and ethyl acetate extracts crude extract at low temperatures, and trichloromethane precipitation obtains the method for product; 200510013084.3 disclose the method for the oligomeric procyanidolics in a kind of membrane ultrafiltration process purification Semen Vitis viniferae; 02144709.8 discloses a kind of method that resin method extracts Proanthocyanidins from Grape Seeds.But these method ubiquities complex process, with an organic solvent, the problem such as the low and unstable product quality of separation efficiency.
The extracting method of above-mentioned pycnogenols does not all adopt zymin, affects the extraction yield of pycnogenols.
Summary of the invention
The object of the invention is the deficiency overcoming existing extracting method, propose a kind of zymin that utilizes in conjunction with the method for solvent from extracting proanthocyanidin from grape seeds.The pycnogenols product that this method obtains can be used for the industry such as medicines and health protection and makeup.
A kind of method extracting pycnogenols from Semen Vitis viniferae of the present invention, raw material is Semen Vitis viniferae, and reagent has polygalacturonase (30000IU), cellulase (15000IU), 95% ethanol (food grade), citric acid (food grade), Sodium phosphate dibasic (food grade).
A kind of method extracting pycnogenols from Semen Vitis viniferae of the present invention, is made up of following steps:
(1) get the raw materials ready: Semen Vitis viniferae is carried out constant temperature drying under reduced pressure, pulverize after weighing, 40 orders sieve, and obtain raw material dry powder for subsequent use;
(2) buffered soln is prepared: mixed with the volume ratio of 0.2mol/L disodium phosphate soln by 1:1.5 ~ 2 by 0.1mol/L citric acid solution, then thin up 2 times, be mixed with buffered soln:
(3) prepare enzyme liquid: mixing buffered soln, polygalacturonase and cellulase, and fully stirring makes it dissolve completely, thus form uniform enzyme liquid; The consumption of buffered soln is in raw material dry powder weight (kg): the ratio calculating polygalacturonase of volume of buffer solution (L)=1:15 ~ 30 and the consumption of cellulase are that the buffered soln of every L adds 0.1 ~ 0:3g polygalacturonase and 0.1 ~ 0.3g cellulase;
(4) feed intake: in raw material dry powder weight (kg): the ratio of volume of buffer solution (L)=1:15 ~ 30, raw material dry powder is added in enzyme liquid;
(5) enzymolysis: after raw material dry powder and enzyme liquid are stirred, lucifuge insulation in the thermostat water bath of 50 ~ 55 DEG C, every 30min stirs once, enzymolysis 3-4h, generates the mixture of enzymolysis solution and residue;
(6) extract: 75 ~ 95% ethanol are added in above-mentioned enzymolysis solution and residue mixture by the method adding 75 ~ 95% ethanol of 15 ~ 30L by every kg raw material dry powder, under 60 ~ 65 DEG C of conditions, extract 2 ~ 3h, after filtration, obtain extracting solution;
(7) finished product: putting extracting solution in the baking oven of 60 ~ 70 DEG C dries to constant weight, and obtains pycnogenols.
A kind of method extracting pycnogenols from Semen Vitis viniferae of the present invention, take Semen Vitis viniferae as main raw material, adopt zymin in conjunction with solvent extraction pycnogenols, its advantage is that former blue and white plain Product Safety is good, quality is good, and former blue and white plain extraction yield comparatively alcohol extracting is followed the example of high by 30 ~ 40%, and the consumption of zymin is few, and technique is simple, easy to operate, efficiency is high, is applicable to suitability for industrialized production.The pectin substance using polygalacturonase and cellulase can destroy cell wall structure based on Mierocrystalline cellulose in plant material and iuntercellular thereof to be connected, makes extraction resistance to mass transfer reduce, makes the former blue and white plain composition of content be easy to stripping.Ethanolic soln is as the Extraction solvent of the former blue and white element of alcohol dissolubility.Citric acid phosphoric acid buffered soln plays the effect of regulator solution pH value.By the buffered soln that method of the present invention is prepared, its pH=6 after testing, can ensure the best effect of zymin effect.
Embodiment:
Specific embodiment: in order to fully disclose a kind of method extracting pycnogenols from Semen Vitis viniferae of the present invention, be illustrated below in conjunction with embodiment.
Embodiment: a kind of method extracting pycnogenols from Semen Vitis viniferae
The Semen Vitis viniferae getting collection period is raw material, and extracting method comprises the following steps:
L () puts fresh Semen Vitis viniferae dries in 65 DEG C of baking ovens, pulverizes, within 40th, sieve, obtain raw material dry powder for subsequent use with high-speed tissue mashing machine.
(2) get 0.1mol/L citric acid solution 160ml, 0.2mol/L disodium phosphate soln 320ml, mix and dilute and be settled to 1000ml, be mixed with buffered soln.
(3) get the buffered soln of 250ml, add 0.05g polygalacturonase and 0.075g cellulase, stir and make it dissolve completely, form uniform enzyme liquid.
(4) in above-mentioned enzyme liquid, add the raw material dry powder of 10g.
(5) lucifuge insulation in the thermostat water bath of 50 DEG C after stirring, every 30min stirs once, enzymolysis 3h, generates the mixture of enzymolysis solution and residue.
(6) in the mixture of enzymolysis solution and residue, add 250m195% ethanol, under 60 DEG C of conditions, extract 2h, after filtration extracting solution.
(7) putting extracting solution in the baking oven of 65 DEG C dries to constant weight, and obtains pycnogenols.
Claims (2)
1. extract a method for pycnogenols from Semen Vitis viniferae, it is characterized in that being made up of following steps:
(1) get the raw materials ready: Semen Vitis viniferae is carried out constant temperature drying under reduced pressure, pulverize after weighing, 40 orders sieve, and obtain raw material dry powder for subsequent use;
(2) buffered soln is prepared: mixed with the volume ratio of 0.2mol/L disodium phosphate soln by 1:1.5 ~ 2 by 0.1mol/L citric acid solution, then thin up 2 times, be mixed with buffered soln;
(3) prepare enzyme liquid: mixing buffered soln, polygalacturonase and cellulase, and fully stirring makes it dissolve completely, thus form uniform enzyme liquid; The consumption of buffered soln is in raw material dry powder weight (kg): the ratio calculating polygalacturonase of volume of buffer solution (L)=1:15 ~ 30 and the consumption of cellulase are that the buffered soln of every L adds 0.1 ~ 0:3g polygalacturonase and 0.1 ~ 0.3g cellulase;
(4) feed intake: in raw material dry powder weight (kg): the ratio of volume of buffer solution (L)=1:15 ~ 30, raw material dry powder is added in enzyme liquid;
(5) enzymolysis: after raw material dry powder and enzyme liquid are stirred, lucifuge insulation in the thermostat water bath of 50 ~ 55 DEG C, every 30min stirs once, enzymolysis 3-4h, generates the mixture of enzymolysis solution and residue;
(6) extract: 75 ~ 95% ethanol are added in above-mentioned enzymolysis solution and residue mixture by the method adding 75 ~ 95% ethanol of 15 ~ 30L by every kg raw material dry powder, under 60 ~ 65 DEG C of conditions, extract 2 ~ 3h, after filtration, obtain extracting solution;
(7) finished product: putting extracting solution in the baking oven of 60 ~ 70 DEG C dries to constant weight.
2. a kind of method extracting pycnogenols from Semen Vitis viniferae according to claim 1, is characterized in that by following steps group
Become:
(1) put fresh Semen Vitis viniferae to dry in 65 DEG C of baking ovens, pulverize with high-speed tissue mashing machine, 40 orders sieve, and obtain raw material dry powder for subsequent use;
(2) get 0.lmol/L citric acid solution 160ml, 0.2mol/L disodium phosphate soln 320m1, mix and dilute and be settled to 1000ml, be mixed with buffered soln;
(3) get the buffered soln of 250ml, add 0.05g polygalacturonase and 0.075g cellulase, stir and make it dissolve completely, form uniform enzyme liquid;
(4) in above-mentioned enzyme liquid, add the raw material dry powder of 10g;
(5) lucifuge insulation in the thermostat water bath of 50 DEG C after stirring, every 30min stirs once, enzymolysis 3h, generates the mixture of enzymolysis solution and residue;
(6) in the mixture of enzymolysis solution and residue, add 250m195% ethanol, under 60 DEG C of conditions, extract 2h, after filtration extracting solution;
(7) putting extracting solution in the baking oven of 65 DEG C dries to constant weight.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106955250A (en) * | 2017-04-17 | 2017-07-18 | 安徽工程大学 | A kind of facial mask that a kind of utilization grape vinasse prepares the method for facial mask and obtained according to the method |
| CN107556279A (en) * | 2016-07-01 | 2018-01-09 | 广州市博仕奥水产饲料科技有限公司 | The method that enzymatic isolation method extracts grape pip procyanidin |
| CN110878075A (en) * | 2019-12-06 | 2020-03-13 | 怀化学院 | Method for extracting procyanidine from grape seeds and procyanidine |
-
2015
- 2015-10-16 CN CN201510667523.6A patent/CN105153096A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107556279A (en) * | 2016-07-01 | 2018-01-09 | 广州市博仕奥水产饲料科技有限公司 | The method that enzymatic isolation method extracts grape pip procyanidin |
| CN106955250A (en) * | 2017-04-17 | 2017-07-18 | 安徽工程大学 | A kind of facial mask that a kind of utilization grape vinasse prepares the method for facial mask and obtained according to the method |
| CN106955250B (en) * | 2017-04-17 | 2020-06-23 | 安徽工程大学 | Method for preparing facial mask by using grape vinasse and facial mask obtained by method |
| CN110878075A (en) * | 2019-12-06 | 2020-03-13 | 怀化学院 | Method for extracting procyanidine from grape seeds and procyanidine |
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