CN101759727B - Nano-scale pine bark extract and preparation method thereof - Google Patents
Nano-scale pine bark extract and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a method for extracting nano-scale proanthocyanidin oligomers from pink bark. The production technical process of the method comprises: raw material treatment, filtrate extraction treatment, concentration treatment, high-efficiency countercurrent extraction treatment, dilution treatment, water dissolution treatment, liquid phase intercalation treatment, nano crushing treatment, drying and depolymerization treatment, purification treatment and sterilization and packing treatment. In the method, water is used as an extraction solvent, ethyl acetate is used as an extraction solvent, and after weakly acidic electrolyzed distilled water is mixed, a nanocrystallization process is used to prepare a finished product. The countercurrent electrolysis extraction method has high extraction rate and low cost, effectively separates the proanthocyanidin oligomers from proanthocyanidin polymers, greatly improves product extraction yield and quality, improves OPC active ingredient content to over 99 percent and effectively solves the technical problem of difficult direct absorption by human bodies, which is caused by large proanthocyanidin particle size and low active ingredient content. The invention also provides a nano-scale pine bark extract prepared by the method.
Description
Technical field
The present invention relates to natural product and foodstuff additive field, particularly from Cortex Pini, extract anthocyanidin as healthy food material, or as the multiple fields such as batching of additive application in medicine, makeup.
Background technology
Contain the powerful antioxidant oligomeric proanthocyanidin in the extract of French coast Cortex Pini and other kind pine tree barks.Contain multiple amino acids in the pine tree bark extract, a large amount of scientific researches is verified both at home and abroad, the pycnogenols that extracts from Cortex Pini is the most powerful effective anti-ageing material of finding up to now, can improve well modern's sub-health status, makes more people's good health and a long life.
Pycnogenols class material is that the 4-glycol is polymerized by the flavan-3-alcohol of different numbers or flavane-3, wherein 2～4 aggressiveness is called oligomeric procyanidolics (Proanthocyanidin Oligomers is called for short OPC).Generally being present in the skin of fruit and the wooden real part of plant, is the polyphenolic compound that extensively is present in the plant.The ability that pycnogenols has strong anti-oxidation, removes the free radical ability and microcirculation in human body is improved is one of present strong, the most effective oxygen free radical scavenger of finding and lipid peroxidation inhibitor.Antioxidant effect in vivo is about 50 times of vitamin-E in vivo far above vitamin-E and vitamins C, ascorbic 20 times.Be used widely at cosmetic field and field of health care food in the world at present.The external pycnogenols preparation of producing is as VITAMIN, and having of becoming that people often take delays senility and the protective foods of the function such as beauty treatment.As far back as the fifties French scientist just find from Cortex Pini, to extract a large amount of pycnogenolss, can contain 85% pycnogenols in its extract.Then find that Semen Vitis viniferae is the better resource of extracting pycnogenols the seventies, Proanthocyanidin from Grape-seed Extracts can be up to 95%.
The home and abroad has reported that multiple separation prepares the method for pycnogenols, comprise that mainly extracting method commonly used is milling process, organic solvent extractionprocess, water extract-alcohol precipitation-resin adsorption method, supercritical carbon dioxide extraction method, column chromatography etc., as a kind of traditional method was: a pulverized the plant material of drying; The b preparation contains the leach liquor of pycnogenols; C extracts oligomeric procyanidolics with polar organic solvent; D separates out oligomeric procyanidolics with non-polar organic solvent from polar organic solvent; E makes purification process to the product of separating out.Although solvent extration equipment is simple, process cost is low, and product content is not high when using separately, can only reach about 50%, can be considered as the pre-treatment step of preparation high assay proto cyaniding.Column chromatography is because equipment is simple, and procyanidin content is high and receive publicity in the product that obtains.The key of column chromatography is to select suitable filler.Make filler with dextran or C-18 bonded silica gel, although can obtain the higher pycnogenols of content, filler expensive is difficult to be applied to large-scale commercial production; Although it is lower to make the filler price with poly-phthalein amine, but before charging, need raw material is carried out complicated pre-treatment, simultaneously because the higher pycnogenols strong adsorption on poly-phthalein amine of the polymerization degree is easy to make the post effect to reduce, need to use the alkali lye frequent regeneration, also be not suitable for suitability for industrialized production.
Be applied at present among the preparation method of industrialization extraction the extraction of Cortex Pini pycnogenols be tended to adopt counter-current extraction.Cross solvent extraction is improved a kind of new separation means on the basis of conventional solvent extraction process, it has utilized in the conventional solvent extraction process, the density variation of solvent and material and immiscible characteristic, to extract first concentrated solution packs in the extraction tower, as extract solvent density and greatly then add from cat head, like this extraction solvent since the action of gravity slow decreasing at the bottom of the tower, draw up cat head with pump again, reciprocation cycle, the little extraction solvent of density owing to buoyancy rises to cat head, is back at the bottom of the tower then by advancing at the bottom of the tower again, replenish during this time and constantly new solvent, and so forth circulation.And find that in actual applications by the oligomeric former blue and white element that this method extracts with Cortex Pini, the highest effective content of its OPC only has 95%, and the dry powder particle diameter is very large, is difficult to make human body fully to absorb.Owing to the anthocyanidin in the Cortex Pini is not carried out at present the technique of low cost, high efficiency extraction, therefore the Cortex Pini that falls of many forest farms is taken as waste more and throws away, and has caused a large amount of wastes of resource.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, excessive for Cortex Pini Massonianae extract particle diameter in the prior art, be difficult to by the quick situation about absorbing of human body, a kind of new nano-scale pine bark extract preparation method is provided, to improve the effective constituent of Cortex Pini Massonianae extract, and the degraded that reduces or slow down anthocyanidin, obtain that a kind of solvability is good, good stability, low, the trickle high purity Cortex Pini Massonianae extract that easily is absorbed by the body of particle diameter of viscosity, its former blue and white effect composition that have can reach more than 99%.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
A kind of preparation method of nano-scale pine bark extract, described preparation method carries out as follows:
(a) raw material is processed: will collect pine tree pine needle and Cortex Pini brachymemma, choose clean, and then clean with deionized water.
(b) filtrate extraction process: raw material is packed in the extractor, add the water of 5～10 times of amounts as extracting solvent, extracting temperature is 50～80 degrees centigrade, and extraction time is 5～8 hours; Preferable amount is 8 times of water as extracting solvent, and extracting temperature is 80 degrees centigrade, and extraction time is 6 hours.
(c) reclaim the solvent concentration: carry out reclaim under reduced pressure in the extracting solution importing vacuum concentrator with step (b) gained, temperature is 50～80 degrees centigrade, and vacuum tightness is 0.07～0.10, and concentrated solution is 1: 2 with the amount ratio of raw material; Preferred temperature is 70 degrees centigrade, and vacuum degree control is more than 0.07, the amount ratio of concentrated solution and raw material be 1: 2 for good.
Also can carry out secondary concentration to concentrated solution, with the utilization ratio in further realization extraction tower space.
(d) high performance counter current extraction treatment: put the concentrated solution of step (c) gained into extraction tower, use organic solvent ethyl acetate extraction 1～4 time; Consumption is 1～2 times; Cycle index is 4～8 times; Evenly add ethyl acetate at the bottom of the extraction tower and carry out extraction to filtrate; The product of separated and collected different sites; The ethyl acetate consumption is 2 times of concentrated solution during experiment, and cycle index is 5 times, through different extraction towers, separate collection filtrate.
(e) dilution process: the ethyl acetate after will extracting reclaims, and obtains thick paste; The thick paste that makes is added the appropriate amount of deionized water dilution.
(f) water-soluble processing: add the slightly acidic distilled water through the electrolysis processing of 6～8 times of volumes, the pH value of described slightly acidic distilled water is 4-7, obtains outstanding mixed liquid after the mixing.Preferably use the electrolytic aqueous solution of 8 times of volumes, preferred pH value is 5-5.5.
(g) liquid phase intercalation is processed: add the surface-modifying agent more than 0.5%～5%, use ultrasonic cell disintegration equipment to carry out the iterative cycles ultrasonication, surface-modifying agent is entered in the structure of Cortex Pini Procyanidcic Oligomers extract.
(h) nanometer is processed: the outstanding mixed liquid of gained is pulverized with NS1001L 2K type wet process disintegrator, made extract not only reach nano level but also can keep its biological activity; Or use other more senior grinding plant to carry out nanometer and process; The particle diameter of procyanidin extract reaches 10～60 nanometers in the mixed liquid of processing rear overhang.
(i) being dried to powder and depolymerization processes: will through through the outstanding mixed liquid that contain Cortex Pini Massonianae extract that nanometer is processed being spray dried to the particulate powder after, pulverize the grinding depolymerization with airflow milling or other grinding plant are counter again.
(j) powder surface Passivation Treatment: will carry out Passivation Treatment through the Cortex Pini Massonianae extract injecting inert gas that depolymerization is processed, and reduce the nanoparticle surface electric charge, and reduce the reunion between nanoparticle.
(k) sterilization and packing are processed: nano level dry powder is carried out ultraviolet lamp sterilization, then packing.
The effective constituent of pycnogenols accounts for more than 99% of gross weight in the Cortex Pini Massonianae extract of producing by above technical process, and outward appearance is rust red toner powder, and the grain size of described Cortex Pini Massonianae extract is between 10nm～60nm.
Described this pycnogenols effective constituent can be made capsule or make tablet through tablet forming technique through filling process at the nano-scale pine bark extract more than 99%, is applied in the protective foods aspect.
Described this nano-scale pine bark extract water soluble, oil, alcohols and other liquid solvents can directly be absorbed by human oral cavity or Transdermal absorption or be used for the medicine injection.
As preferably, but can is in soft gelatin capsule after described this extract and the solvent, and described extract accounts for 0.01% weight of capsule preparations gross weight～99.99% weight, is applicable to oral health product or external use skin care.
As preferably, the direct can of described extract is in hard gelatin capsule, and described extract accounts for 1% weight of capsule preparations gross weight～100% weight, is applicable to oral health product.
As preferably, described extract joins in the matrix as additive, and described extract accounts for 0.1% weight of gross weight～80% weight, is applicable to skin protection cosmetics or preparation for external application to skin.
Compare with the preparation method who uses the high performance counter current extraction process to extract Cortex Pini anthocyanidin in the prior art, one of key feature among the preparation technology of nano-scale pine bark anthocyanidin provided by the present invention is first the extract of preparing with counter-current extraction to be proceeded water-soluble combination treatment, the slightly acidic distilled water through the electrolysis processing that adds 8 times of volumes, obtain outstanding mixed liquid after the mixing, then add surface-modifying agent, use ultrasonic cell disintegration equipment to carry out the iterative cycles ultrasonication, surface-modifying agent is entered in the structure of Cortex Pini Massonianae extract, and recycling nano-pulverization technique is carried out nanometer and is processed.This case the contriver find under study for action, if directly adopt counter-current extraction, the Cortex Pini raw material after the lixiviate still maintains naked eyes can seem red-purple, illustrates that still some anthocyanidin is not extracted.Experiment showed, and utilize treatment process of the present invention that make Cortex Pini Massonianae extract in preparation process, pycnogenols effective constituent can be brought up to more than 99%.
Pulverize by the nano level in outstanding mixed liquid, can make the solvability composition in the Cortex Pini Massonianae extract directly be dissolved in the liquid; The insoluble liquid component can form nano level water-in-oil or water oil-packaging type micro-emulsion with liquid; The insoluble solids component can form sol system or suspension with liquid.All the components is refine to nano level with various forms, reaches maximum utilization when composition can be absorbed by the body, and has enlarged drug effect and the utilization ratio of extract.
The present invention efficiently solves counter-current extraction, and to extract OPC purity not high enough, and the OPC powder particle is larger, and human body is difficult to the defective that directly absorbs.High-quality OPC is because good solubility in water and alcohols wherein, add that its color and luster is beautiful, evident in efficacy, extensively joined in the various bread and cheeses, both as nutrition-fortifying agent, substitute synthetic preservative as natural antiseptic agent again, improved the security of food, be subject to extensive welcome, market outlook are very wide.Present method technique is simple, and is easy to operate, is applicable to industrial production.
And the tankage of Cortex Pini after as the processing of a kind of forest farm, generally all abandoned, seldom recycle appreciation, this raw materials technology cost is low, for the lasting recycling of resource provides a kind of considerable parallel effective means, the recycling that Cortex Pini has carried out turning waste into wealth is appreciated, meet the Sustainable development rule, outstanding social effect is arranged.
In sum, nano-scale pine bark extract of the present invention and preparation method thereof, operating procedure is simple, convenient and easy.The experiment proved that, use method of the present invention, the effective constituent of pycnogenols can be up to more than 99%, and powder diameter is between 10～60nm.
The invention has the beneficial effects as follows:
1, develop a kind of solvability good, stablize, viscosity is low, the trickle Cortex Pini Massonianae extract that easily is absorbed by the body of particle diameter, can the balance the body immunologic function, promote hemopoietic function, eliminate free radical, anti-oxidant, improve immunological competence, thereby delay senility; For the disease that causes because of hypoimmunity, and the defect of autoimmunization system, such as rheumatoid arthritis, the ruthless sore of erythema etc., prevent effect.
2, added value of product is high, and the anthocyanidin that utilizes Cortex Pini to extract can be used for functional food and functional food additives exploitation, and more wide application prospect is arranged, and the added value of bringing is higher.Except medicinal use, also can be used as the batching of makeup, comprise sun-proof articles.
3, product purity is high, brought up to more than 99% by the pycnogenols effective constituent that this preparation method obtains, after nanometer technique step process, obtain the extract grain size between 10nm～60nm, can be directly water-soluble, oily, alcohols and other liquid solvents can directly be absorbed by human oral cavity or Transdermal absorption or be used for the medicine injection.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
Embodiment 1
The below is the indefiniteness embodiment preparation method of nano-scale pine bark extract:
(a) raw material is processed: will collect pine tree pine needle and Cortex Pini brachymemma, choose clean, and clean with deionized water.
(b) filtrate extraction process: raw material is packed in the extractor, add the water of 10 times of amounts as extracting solvent, extracting temperature is 80 degrees centigrade, and extraction time is 8 hours.
(c) concentration: carry out reclaim under reduced pressure in the extracting solution importing vacuum concentrator with gained, temperature is 80 degrees centigrade, and vacuum tightness is 0.10, and concentrated solution is 1: 2 with the amount ratio of raw material.
(d) high performance counter current extraction treatment: put concentrated solution into extraction tower, with organic solvent ethyl acetate extraction 2 times, consumption is 2 times, and cycle index is 4～5 times, evenly add ethyl acetate at the bottom of the extraction tower and carry out extraction to filtrate, the product of separated and collected different sites.
(e) dilution process: the ethyl acetate after will extracting reclaims, and obtains thick paste.Then carry out spraying drying after the thick paste that makes being added the appropriate amount of deionized water dilution, obtain extract after being dried.
(f) water-soluble processing: add the slightly acidic distilled water through the electrolysis processing of 8 times of volumes in the extract, the pH value of described slightly acidic distilled water is 5.5, obtains outstanding mixed liquid after the mixing.
(g) liquid phase intercalation is processed: the Cortex Pini Massonianae extract of gained is added 5% surface-modifying agent, use ultrasonic cell disintegration equipment to carry out the iterative cycles ultrasonication, surface-modifying agent is entered in the structure of this extract.
(h) nanometer is processed: the outstanding mixed liquid that will contain this extract is pulverized with NS1001L 2K type wet process disintegrator, makes described extract not only reach nano level but also can keep its biological activity.The particle diameter of procyanidin extract reaches 10～60 nanometers in the mixed liquid of processing rear overhang.
(i) being dried to powder and depolymerization processes: will through through the outstanding mixed liquid that nanometer is processed being spray dried to the particulate powder after, pulverize the grinding depolymerization with airflow milling is counter again.
(j) powder surface Passivation Treatment: the Cortex Pini Massonianae extract injecting carbon dioxide that will process through depolymerization, utilize Supersonic air-flow technology to carry out Passivation Treatment, reduce the nanoparticle surface electric charge, reduce the reunion between nanoparticle.
(k) sterilization and packing are processed: nano level dry powder is carried out ultraviolet lamp sterilization, then packing.
Going out effective constituent through preparation method's final purification of the present invention is 99% nano-scale pine bark Procyanidcic Oligomers extract, and water soluble, oil, alcohols and other liquid solvents can directly be absorbed by human oral cavity or Transdermal absorption or be used for the medicine injection.Through behind the nanometered disposal, the grain size of extract is between 10nm～60nm, and the extract outward appearance is rust red toner powder.
Embodiment 2
Below in conjunction with this embodiment effective constituent and the security of described extract are effectively detected:
This experiment utilizes the phenolic hydroxyl group that exists in the pycnogenols molecular structure to check, because pycnogenols can produce with the reaction of neutralized verdigris complex precipitant the brown color precipitation of indissoluble in neutral medium, after centrifugation, by Cu2+ excessive in the aas determination supernatant liquor, thereby can set up a kind of method of indirect measurement pycnogenols effective constituent.The advantages such as it is easy, quick that this detection method has, and reagent dosage is few are used for actual sample to measure, and the result is accurate.
Testing tool and reagent:
Adopt TAS-986 atomic absorption spectrophotometer (the general universal apparatus company limited of analysing in Beijing); Copper hollow-cathode discharge lamp (Shanghai electric light company); HH-4 digital display thermostat water bath (Changzhou Guohua Electric Appliance Co., Ltd.); Plus 420A acidometer (U.S. OrionN company); XYJ80-2 centrifugal precipitation mechanism (Jiangsu Medical Instruments factory).Pycnogenols standard reserving solution (3g/L): accurately take by weighing pycnogenols (99%) that 0.3g extracts by above-mentioned preparation method with water dissolution and be settled in the 100mL volumetric flask, be diluted to the standard solution of 0.3g/L; Neutralized verdigris solution (1g/L): the time spent is diluted to the standard solution of 0.1g/L.Above reagent is analytical pure, and water is secondary deionized water.
Detection method:
Pipetting a certain amount of pycnogenols standard solution is positioned in the 10mL centrifuge tube, the neutralized verdigris solution that adds 1mL 1g/L, be diluted with water to scale, fully mixing reacts 25min in 80 ℃ of water-baths, be chilled to centrifugation after the room temperature, the careful supernatant liquor 2mL that draws is diluted with water to scale in the 10mL colorimetric cylinder, take water as blank, spray into Air-acetylene Flame, measure its absorbancy (λ 324.7nm).
Detection formula:
Pipette successively 0.0,0.1,0.3,0.5,0.7,0.9 and the pycnogenols standard solution of 1.0mL 0.3g/L in the 10mL centrifuge tube, standard series concentration is respectively 0.0,3.0,9.0,15.0,21.0,27.0 and 30.0mg/L.Press determination of experimental method, pycnogenols is used the concentration drawing curve of liquid with absorbance A.Its equation of linear regression is A=-0.0023C (ms/L) 4-0.4091, and r=0.9991 can directly find the content of pycnogenols thus on the working curve.
Detected result:
Get 1mL pycnogenols standard solution, press its absorbancy of determination of experimental method.The result shows that in 20-85 ℃ of scope, along with the rising of temperature, precipitation increases, and absorbance reduces gradually; When temperature in 75～85 ℃ of scopes.The absorbance A value is little and stable, illustrates to precipitate at most this moment, reacts more complete; When temperature surpassed 85 ℃, along with the rising of temperature, precipitation reduced gradually, and absorbance increases gradually.Therefore, the present embodiment preferable reaction temperature is 80 ℃.
Press the experimental technique operation, the different time of reaction is measured its absorbancy in 80 ℃ of water-baths.The result shows that after the reaction times 20min, absorbance tends towards stability.Therefore the present embodiment preferred reaction time is 25min.
Under different pH condition, test by experimental technique.PH value of solution is in the 5-7 scope, and the A value is little and stable, illustrates to precipitate at most this moment, reacts more complete.When pH＜5, because acidity of medium is excessive, precipitation is difficult for generating; After pH＞7, the solution alkalize, the mantoquita hydrolysis generates the copper hydroxide precipitation, makes measurement result higher.
Also investigated water and 0.1mol/mL Trisodium Citrate-NaOH, boric acid. borax, Potassium Hydrogen Phthalate-NaOH and 4 kinds of buffer systems of acetic acid sodium-acetate, when being lower time of reaction medium condition at water, absorbance is little and stable.This is because the organic acid part in rear 4 kinds of buffered soln has complexing action to cupric ion, on the impact that is formed with of precipitation.Therefore the present embodiment preferably water is the reaction medium of test experience.
The consumption of neutralized verdigris solution has certain impact to measurement result.Present embodiment selects the α-benzoinoxime of different amounts to test.The result shows: the precipitation agent consumption precipitates difficult the generation very little; Consumption is too many, causes typical curve crooked, and pH is the residual content of measuring Cu in the supernatant liquor on the impact of reaction, and the Cu consumption is too much, will increase dilution step.Consider, the neutralized verdigris solution 1mL of 1L is selected in this experiment.
The impact of interfering substance: verify through pycnogenols inclusion sterling: in the pycnogenols standard solution, add with doubly to starch, calcium stearate, Magnesium Stearate, the talcum powder solution of pycnogenols respectively, 2 times Walocel MT 20.000PV, dextrin are on measuring without impact; And with amino acid doubly mensuration is had interference, but in the ordinary course of things, aminoacids content is fewer in the pycnogenols.
Get respectively 11 parts of the standard solutions of 1mL pycnogenols, press the embodiment method and detect, relative standard deviation (RSD) is 1.1%～1.2%.
Accurately take by weighing an amount of 300mg dissolving of nanometer Cortex Pini Massonianae extract, constant volume is got its filtrate 10mL constant volume in the 100mL volumetric flask after filtering in the 100mL volumetric flask.Extracting sample solution 1ml presses determination of experimental method, the active constituent content of calculation sample, and the result is as described in Table 1.
The quality test results of table 1 Cortex Pini Massonianae extract
| OPC | ＞99％ |
| Moisture | 1.7％ |
| Ash | 0.2％ |
| Arsenic | Do not detect |
| Plumbous | Do not detect |
| Amino acid | ＞0.5％ |
| Average diameter of particles | 10-60nm |
Embodiment 3:
(1) described nano-scale pine bark extract in skin protection cosmetics as the purposes of additive:
Use joins in the matrix as additive through the nano-scale pine bark extract that above-mentioned preparation method obtains, and described extract accounts for 0.1% weight of gross weight～80% weight, is applicable to skin protection cosmetics.Matrix can be any form of liquid, solid, emulsion, paste.
The prescription of spot skin-care gel is removed in A, anti-ageing whitening
Use the 10G nano-scale pine bark extract, the 0.5G carbomer, the 1G sweet almond oil, the 0.5ML antiseptic-germicide, the 0.5G antioxidant adds the 10ML rose, and the surplus adding distil water is to 100ML, and mix and blend is abundant, makes the skin-care gel of anti-ageing whitening anti-wrinkling.
Contrast traditional whitening and remove the spot product: this product is because use nanometer, degree of functioning reaches 99% pycnogenols, directly is absorbed by the body therefore easilier pale skin progressively under the prerequisite of damaged epidermis not, the melanochrome of clearing up and discharging reaches safety and goes the simultaneously effect of skin care of spot.Using can go down in 2 weeks of this product makes the melanochrome distribution proportion descend 6%, uses continuously for 12 weeks, can reduce the melanochrome ratio up to 29%, and the result is as described in Table 2.
Detecting the contrast number is 30 people, is divided into two groups of A, B, every group of each 30 people.Use respectively traditional whitening cream and the whitening cream take nano-scale pine bark extract as prescription preparation to compare.After adhering to using for 54 weeks, traditional whitening cream is in the phenomenon that has a rebound aspect the control color spot, and A group part user skin occurs irritated.B group user does not have a rebound and allergic phenomena.
The result of use contrast of the traditional whitening product of table 2 and nano-scale pine bark extract whitening and spot eliminating cream
(2) application in healthcare products:
B, a kind of hard gelatin capsule by the nano-scale pine bark extract preparation
Directly can is in hard capsule for the nano-scale pine bark extract that use obtains through above-mentioned preparation method, and content accounts for 1% weight of hard capsule gross weight～100% weight.
C, a kind of by nano-scale pine bark extract preparation soft gelatin capsule
Use through nano-scale pine bark extract that above-mentioned preparation method obtains can with can after the solvent in soft capsule, content accounts for 0.01% weight of soft capsule gross weight～99.99% weight, is applicable to oral health product and external use skin care.
Get nano-scale pine bark extract 30%, mix with 70% raisin seed oil, through carrying out can after the sterilization flow process, can be made as the soft-gelatin capsule formulation of auxiliary disease treatment.
The nano level OPC fine powder that extracts according to preparation method of the present invention, effective constituent is high, can reach more than 99%, can reach 10～60 nanometers through fine powder particle diameter behind the nanometered disposal simultaneously, can be directly water-soluble, oily, alcohols and other liquid solvents, directly buccal absorption or Transdermal absorption or be used for the medicine injection.
Claims (5)
1. the preparation method of a nano-scale pine bark extract is characterized in that, described preparation method comprises the steps: at least
(a) filtrate extraction process: adopt water to extract for extracting solvent;
(b) high performance counter current extraction treatment: adopting the organic solvent ethyl acetate is solvent, and filtrate is extracted;
(c) concentration and recovery is processed: the solvent after will extracting reclaims, and obtains thick paste;
(d) dilution process: add the weakly acidic water solution through the electrolysis processing, obtain outstanding mixed liquid after the mixing;
(e) liquid phase intercalation is processed: add surface-modifying agent, use ultrasonic cell disintegration equipment to carry out the iterative cycles ultrasonication, surface-modifying agent is entered in the structure of extract;
(f) nanometer is processed: will hang mixed liquid and carry out the nanometer processing with grinding plant.
2. the preparation method of nano-scale pine bark extract according to claim 1 is characterized in that, described step comprises that also being dried to powder and depolymerization processes:
The outstanding mixed liquid that to process through nanometer be through after being spray dried to the particulate powder, pulverize the grinding depolymerization with airflow milling or other grinding plant are counter again.
3. the preparation method of nano-scale pine bark extract according to claim 2 is characterized in that, described step also comprises the powder surface Passivation Treatment:
To carry out Passivation Treatment through the Cortex Pini Massonianae extract injecting inert gas that depolymerization is processed, reduce the nanoparticle surface electric charge, reduce the reunion between nanoparticle.
4. the preparation method of nano-scale pine bark extract according to claim 1 is characterized in that, described liquid phase intercalation treatment process is to adopt the ultrasonic grinding technology.
5. the preparation method of nano-scale pine bark extract according to claim 3 is characterized in that, the Passivation Treatment of the described Cortex Pini Massonianae extract of processing through depolymerization is the Supersonic air-flow technical finesse of adopting nitrogen or carbonic acid gas.
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| CN102228248A (en) * | 2011-06-29 | 2011-11-02 | 中健行集团有限公司 | Energy-saving and environmentally-protected production process of Songzhen capsules |
| CN102488720B (en) * | 2011-11-28 | 2013-08-28 | 河南省康星药业股份有限公司 | Preparation method for submicron pine needle powder at normal temperature and special bidirectional air-flow screening machine |
| CN102746706B (en) * | 2012-07-31 | 2013-11-27 | 新疆林科院经济林研究所 | Preparation method and application of Korepine bark natural dye |
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