CN104496957A - Method for extracting procyanidine from grape skins - Google Patents
Method for extracting procyanidine from grape skins Download PDFInfo
- Publication number
- CN104496957A CN104496957A CN201410710766.9A CN201410710766A CN104496957A CN 104496957 A CN104496957 A CN 104496957A CN 201410710766 A CN201410710766 A CN 201410710766A CN 104496957 A CN104496957 A CN 104496957A
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- CN
- China
- Prior art keywords
- vitis viniferae
- pericarpium vitis
- pycnogenols
- solution
- procyanidine
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting procyanidine from grape skins. The method comprises the following steps: (1) adding 3-6 times of 30-70 percent of ethanol into the grape skins; (2) performing reflux extraction on the uniformly mixed raw materials for 1-5 times to obtain extracting solutions, wherein the extraction time is 1-4 hours each time; (3) merging the extracting solutions, and concentrating until the concentration of the mixed solution is 1.2-1.27g/ml; (4) treating the concentrated solution by using a D101 macroporous resin, adding clean water with a volume amount of 0.5-1 time that of the concentrated solution for washing, wherein methanol is used as eluent, performing ultraviolet monitoring, and collecting the eluent when an absorption peak occurs at 260-270nm; and (5) performing vacuum concentration on the collected eluent until the solution is dry, thereby obtaining the procyanidine. According to the method for extracting the procyanidine from the grape skins, disclosed by the invention, the extraction efficiency is high, the pertinence is high, and the procyanidine can be effectively extracted from grapes.
Description
Technical field
The present invention relates to a kind of grape deep process technology, particularly a kind of method extracting pycnogenols from Pericarpium Vitis viniferae, belongs to agricultural technology field.
Background technology
Grape, also known as grape, is a kind of delicious food and is rich in the fruit of nutritive ingredient.Grape is a kind of multi-functional fruit, is widely cultivated in worldwide.There are some researches show in Pericarpium Vitis viniferae and be rich in pycnogenols, and have people to extract from Pericarpium Vitis viniferae to obtain pycnogenols.
Pycnogenols, is called for short OPC, is a class Flavanol monomers and polymeric polyphenolic substance thereof, belongs to Vitamin P complex.Confirm through large quantity research, pycnogenols has very outstanding effect for aspects such as improving blood circulation, skin care, reduction cholesterol.
Studies have reported that and show to be rich in pycnogenols in Pericarpium Vitis viniferae, and grape itself being as a kind of daily fruit, from the product wherein extracting the anthocyanidin obtained and belong to food and medicine consangunity, is desirable healthcare products starting material.The extensive attention kept healthy for healthy diet along with people and pursuit, increase fast for pycnogenols demand.Need a kind of simple method can extracting pycnogenols from grape in a large number badly.
Summary of the invention
The object of the invention is to overcome in prior art and lack the extensive deficiency extracting pycnogenols processing method, a kind of method extracting pycnogenols from Pericarpium Vitis viniferae is provided.The pycnogenols in grape source, undoubtedly for market provides a kind of approach of a large amount of production pycnogenols, the present invention is directed to corresponding technological difficulties and carries out Improvement, provide a kind of pycnogenols production method of high-efficiency and low-pollution.
In order to realize foregoing invention object, the invention provides following technical scheme:
From Pericarpium Vitis viniferae, extract a method for pycnogenols, comprise the following steps:
(1) get Pericarpium Vitis viniferae, add the ethanol of 3-6 times of 30%-70%, the ethanol of preferred 30%-50%, preferably can be uniformly mixed and promote material uniformity coefficient.
(2) raw material will mixed, refluxing extraction 1-5 time, preferred 2-3 time, each 1-4 hour, preferred 1-2 hour.
(3) united extraction liquid, being concentrated into strength of solution is 1.2-1.27g/ml.
(4) by the solution D101 macroporous resin treatment after concentrated, the clear water adding 0.5-1 times of volume rinses, and then use methanol as eluent, ultraviolet monitor function effluent liquid, when absorption peak appears in 260-270nm, collects this elutriant.
(5) elutriant collected is evaporated to dry, obtains pycnogenols.
The feature that the present invention is directed to the complicated polyphenolic substance of pycnogenols adopts ethanol to extract, and extraction effect is good, can effectively be extracted from Pericarpium Vitis viniferae by pycnogenols.Then coordinate methyl alcohol to be separated with macroporous resin, after being rinsed by clear water, meoh eluate procyanidins purity is high, quality better, effectively by various extraction Impurity removal, can obtain the pycnogenols of high-quality.
Further, 30%-40% ethanolic soln is preferably used to extract.According to the feature of Pericarpium Vitis viniferae structural constituent and pycnogenols, select 30%-40% ethanolic soln to extract, selectivity in solution-treated process, better, be more conducive to follow-up purification process, obtain effective yield of final pycnogenols.
Further, described Pericarpium Vitis viniferae is that area is less than 5-10mm
2pericarpium Vitis viniferae.If the Pericarpium Vitis viniferae that surface-area is larger, then pulverized or cutting process, obtained the Pericarpium Vitis viniferae raw material that specific surface area is larger.The size of Pericarpium Vitis viniferae can affect the boiling flowing of pycnogenols solution in reflux course, the entirety that the Pericarpium Vitis viniferae that area is less can realize extracting solution is boiling, and corresponding solution usage is minimum in this case, is very advantageous in the extraction of the pycnogenols in Pericarpium Vitis viniferae.
Further, Pericarpium Vitis viniferae raw material 300-400W microwave device microwave treatment 0.5-2 hour, and then carry out refluxing extraction with ethanol.Pericarpium Vitis viniferae belongs to the epidermis of grape fruit, and structure is closely knit, can well destroy the core of wherein compact structure with lower powered microwave device pre-treatment, improves the efficiency extracted.
compared with prior art, beneficial effect of the present invention:
Pericarpium Vitis viniferae of the present invention extracts the method for pycnogenols, and extraction efficiency height is with strong points, effectively can extract from grape and obtain pycnogenols.The solution that extracting method of the present invention uses is ethanol or methanol solution, cheap, and comparatively friendly to environment, can effectively reduce the cost of Pericarpium Vitis viniferae deep processing, improves product competitive power commercially.
Embodiment
In the present invention, described ethanolic soln is the aqueous ethanolic solution of volume percent, as the mixing solutions that 30% ethanolic soln is made up of the second alcohol and water of 70:30 volume ratio.In case of no particular description, all the solution used in the present invention should be explained according to usual understanding and above explanation, must not be conflicted mutually with routine techniques or above-mentioned explanation.
The grape that the present invention uses can choose commercially available Pericarpium Vitis viniferae raw material, also can be prepared the Pericarpium Vitis viniferae raw material obtained in accordance with the following methods.Grape berry separation method, comprises the following steps:
(1) with extrusion equipment by grape fruit pressure break, extrusion equipment compression gap is greater than the 1.2-2 of the size of Semen Vitis viniferae doubly, and during extrusion equipment extruding grape, between compressive plane, spacing/gap size is 1.2-2 times of Semen Vitis viniferae, ensure that grape berry can by sufficient pressure break, and Semen Vitis viniferae is not damaged.Described extrusion equipment mainly can realize the equipment that grape fruit tentatively destroys, and can select the commercially available extrusion equipment meeting the demand.
(2) slope cutting unit sent into by the grape through extrusion process, described slope cutting equipment includes tilted plate and is arranged on the projection on tilted plate, grape slides along inclined plate surface on the slope, be subject to the projection cutting action on tilted plate surface, Pericarpium Vitis viniferae and pulp and Semen Vitis viniferae are separated from each other out.Preferred projection can be sharp keen projection, also can be obtuse projection.Projection is the outstanding, not of uniform size of mixing shape, pointed by the Pericarpium Vitis viniferae of different sizes with pulp to partly destroying.
(3) rear of slope cutting unit is provided with collection mesh screen, it is the first collection container below mesh screen, mesh screen has flushing mechanism near the side on slope, flushing mechanism is to the surface bath of collection mesh screen, make slope is slipped to grape berry on screen cloth and Pericarpium Vitis viniferae washes away, and Semen Vitis viniferae is also in scour process, fall into the first collection container below mesh screen through the hole on mesh screen.Collect the object that mesh screen mainly realizes Semen Vitis viniferae to be separated, in the process that Semen Vitis viniferae is separated, still have part pulp and/or Pericarpium Vitis viniferae to fall into the first collection container of below, therefore need further process.
The mixture of the Semen Vitis viniferae that (4) first collection containers obtain and grape berry, after thin up, stirs miscible pulp, filters, and is separated and obtains Semen Vitis viniferae and grape berry slurries.
(5) pulp on mesh screen and Pericarpium Vitis viniferae are flushed in the second collection container of mesh screen side by water.Add water to the material in the second collection container, stir miscible pulp, filter, be separated and obtain Pericarpium Vitis viniferae and grape berry slurries.
Below in conjunction with test example and embodiment, the present invention is described in further detail.But this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on content of the present invention all belong to scope of the present invention.Per-cent not specified in the present invention is all weight percentage.
Embodiment 1
From Pericarpium Vitis viniferae, extract pycnogenols: get Pericarpium Vitis viniferae 80kg, add the ethanol of 200 liter 70%, be uniformly mixed, refluxing extraction 3 times, each 2 hours.United extraction liquid, being concentrated into strength of solution is 1.24g/ml.By the solution D101 macroporous resin treatment after concentrated, add 10 liters of clear water and rinse, then use methanol as eluent, ultraviolet monitor function effluent liquid, when absorption peak appears in 260-270nm, collects this elutriant.The elutriant collected is evaporated to dry, obtains pycnogenols 47g.
Embodiment 2
From Pericarpium Vitis viniferae, extract pycnogenols: get Pericarpium Vitis viniferae 100kg, add the ethanol of 320 liter 40%, refluxing extraction 4 times, each 1 hour.United extraction liquid, being concentrated into strength of solution is 1.26g/ml.By the solution D101 macroporous resin treatment after concentrated, add 17 liters of clear water and rinse, then use methanol as eluent, ultraviolet monitor function effluent liquid, when absorption peak appears in 260-270nm, collects this elutriant.The elutriant collected is evaporated to dry, obtains pycnogenols 87g.
Embodiment 3
From Pericarpium Vitis viniferae, extract pycnogenols: get Pericarpium Vitis viniferae 100kg, be chopped into and be less than 10mm
2pericarpium Vitis viniferae, add the ethanol of 370 liter 40%, be uniformly mixed, refluxing extraction 2 times, each 2 hours.United extraction liquid, being concentrated into strength of solution is 1.26g/ml.By the solution D101 macroporous resin treatment after concentrated, add 22 liters of clear water and rinse, then use methanol as eluent, ultraviolet monitor function effluent liquid, when absorption peak appears in 260-270nm, collects this elutriant.The elutriant collected is evaporated to dry, obtains pycnogenols 93g.
Embodiment 4
From Pericarpium Vitis viniferae, extract pycnogenols: get Pericarpium Vitis viniferae 100kg, by 400W microwave device microwave treatment 2 hours, then add the ethanol of 320 liter 40%, be uniformly mixed, refluxing extraction 4 times, each 1 hour.United extraction liquid, being concentrated into strength of solution is 1.26g/ml.By the solution D101 macroporous resin treatment after concentrated, add 17 liters of clear water and rinse, then use methanol as eluent, ultraviolet monitor function effluent liquid, when absorption peak appears in 260-270nm, collects this elutriant.The elutriant collected is evaporated to dry, obtains pycnogenols 112g.
Claims (4)
1. from Pericarpium Vitis viniferae, extract a method for pycnogenols, comprise the following steps:
(1) get Pericarpium Vitis viniferae, add the ethanol of 3-6 times of 30%-70%;
(2) raw material will mixed, refluxing extraction 1-5 time, each 1-4 hour;
(3) united extraction liquid, being concentrated into strength of solution is 1.2-1.27g/ml;
(4) by the solution D101 macroporous resin treatment after concentrated, the clear water adding 0.5-1 times of volume rinses, and then use methanol as eluent, ultraviolet monitor function effluent liquid, when absorption peak appears in 260-270nm, collects this elutriant;
(5) elutriant collected is evaporated to dry, obtains pycnogenols.
2. the method extracting pycnogenols from Pericarpium Vitis viniferae according to claim 1, is characterized in that, uses 30%-40% ethanolic soln to extract.
3. the method extracting pycnogenols from Pericarpium Vitis viniferae according to claim 1, is characterized in that, described Pericarpium Vitis viniferae is that area is less than 5-10mm
2pericarpium Vitis viniferae.
4. the method extracting pycnogenols from Pericarpium Vitis viniferae according to claim 1, is characterized in that, Pericarpium Vitis viniferae raw material 300-400W microwave device microwave treatment 0.5-2 hour, and then carries out refluxing extraction with ethanol.
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| CN201410710766.9A CN104496957A (en) | 2014-12-01 | 2014-12-01 | Method for extracting procyanidine from grape skins |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503980A (en) * | 2015-12-01 | 2016-04-20 | 大兴安岭林格贝寒带生物科技股份有限公司 | Extraction method of anthocyanin of grape skin |
| CN105732239A (en) * | 2016-05-17 | 2016-07-06 | 许祚员 | Efficient biological organic fertilizer suitable for cherry and preparation method thereof |
| CN106008084A (en) * | 2016-05-17 | 2016-10-12 | 许祚员 | Efficient bio-organic fertilizer for litchis and preparation method of fertilizer |
| CN111303110A (en) * | 2020-04-14 | 2020-06-19 | 宁夏医科大学 | Method for extracting procyanidine from grape skin residues |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503980A (en) * | 2015-12-01 | 2016-04-20 | 大兴安岭林格贝寒带生物科技股份有限公司 | Extraction method of anthocyanin of grape skin |
| CN105732239A (en) * | 2016-05-17 | 2016-07-06 | 许祚员 | Efficient biological organic fertilizer suitable for cherry and preparation method thereof |
| CN106008084A (en) * | 2016-05-17 | 2016-10-12 | 许祚员 | Efficient bio-organic fertilizer for litchis and preparation method of fertilizer |
| CN111303110A (en) * | 2020-04-14 | 2020-06-19 | 宁夏医科大学 | Method for extracting procyanidine from grape skin residues |
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