CN102718737B - Method of using roxburgh rose pulp to prepare roxburgh rose procyanidine - Google Patents
Method of using roxburgh rose pulp to prepare roxburgh rose procyanidine Download PDFInfo
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Abstract
The invention discloses a method of using roxburgh rose pulp to prepare roxburgh rose procyanidine and belongs to the technical field of procyanidine preparation. The method includes: using roxburgh rose pulp sold on the market as raw materials, preparing roxburgh rose pulp juice, extracting procyanidine, preparing ultrafiltrate and roxburgh rose procyanidine purified solution, and finally preparing roxburgh rose procyanidine powder. The roxburgh rose pulp used as the raw materials is extensive in source, cheap and easy to obtain, and various products such as roxburgh rose pulp juice and the like are obtained while the roxburgh rose procyanidine is prepared, so that comprehensive utilization of the roxburgh rose pulp is realized; the method is simple in equipment, mild in reaction condition, energy-saving and safe in production; material resources are fully used in the production process, 'three wastes' (waste gas, waste water and waste residues) are avoided, and environment protection is facilitated; and the roxburgh rose procyanidine product produced by the method is high in purity, dissolubility and antioxidant capacity. Further, the method is widely applicable to procyanidine preparation, and products prepared by the method can be widely applied to industries of cosmetics, health care products, pharmaceuticals and the like.
Description
One, technical field
The invention belongs to pycnogenols preparing technical field, be specifically related to prepare with Rosa roxburghii pulp the method for Rosa roxburghii pycnogenols.
Two, background technology
Pycnogenols is a kind of Vitamin P complex that has special molecular structure; mostly be reddish-brown powder; gas is micro-, puckery; be the current generally acknowledged the most effective natural antioxidants of removing people interior free yl in the world, have that protection is cardiovascular, a function such as preventing hypertension, antitumor action, radiation resistance, beauty treatment are crease-resistant, delay senility, antianaphylaxis, vision protection, treatment inflammation.
Rosa roxburghii is the Southwestern China portion common wild fruit in area.Fruit of Grossularia burejensis Berger contains abundant vitamins C, every hectogram fresh fruit Vitamin C content is 2000mg, therefore be referred to as " king of Vc ", pulp is sour and astringent, eat mouthfeel raw poor, therefore Rosa roxburghii is processed into Sucus Rosae Normalis preservation, and makes multiple roxburgh rose beverage or medicines and health protection product, as strengthening SOD Sucus Rosae Normalis, Rosa roxburghii Li Kang drink etc.Research recently shows that Rosa roxburghii contains pycnogenols composition, has good pharmaceutical use and nutritive value, liked by human consumer.
The preparation method of existing pycnogenols, as " a kind of preparation method of Rhodiola rosea proanthocyanidin " patent that on November 02nd, 2011, disclosed publication number was CN102229592A, disclosed method is to take Rhodiola rosea rhizome as raw material, through alcoholic solvent, extract, sherwood oil grease removal, high concentration ethanol is except sugar, column chromatographic isolation and purification, lyophilize and content > 95%, the pycnogenols of yield > 88.3%.The main drawback of the method is: 1. only with precipitation or extraction, be difficult to remove small molecules or the macromole impurity in extracting solution, these impurity can affect quality product.2. can only prepare a kind of product of pycnogenols.3. the residue that such scheme produces not to extracting, in separating procyanidine process and waste liquid fully utilizes or harmless treatment, not only contaminate environment but also be unfavorable for Sustainable development.
Three, summary of the invention
The object of the invention is to prepare for existing method the weak point of pycnogenols, a kind of method of preparing Rosa roxburghii pycnogenols with Rosa roxburghii pulp is provided.The method raw material is Rosa roxburghii pulp, and wide material sources, cheap and easy to get, reduce production costs effectively; When preparing Rosa roxburghii pycnogenols, also make the multiple products such as Rosa roxburghii pulp and juice and food and feed additive, realized the comprehensive utilization of Rosa roxburghii pulp; Easy and simple to handle, equipment is simple, and reaction conditions is gentle, save energy, production safety; The inventive method makes the most of material resources in process of production, without " three wastes " discharge, is conducive to environmental protection; The features such as the Rosa roxburghii pycnogenols product purity that the present invention produces is all high, and solvability is good, and resistance of oxidation is strong.
Principle of the present invention is: the chromocor compound that Rosa roxburghii pycnogenols is combined into by catechin or the l-Epicatechol of different quantities, be dissolvable in water in certain density ethanolic soln, and available ethanolic soln extracts from Rosa roxburghii pulp residue; Rosa roxburghii pycnogenols molecular weight, between 300～2000Da, much smaller than the molecular weight of protein, polysaccharide, can be realized by ultrafiltration separated; Phenyl on Rosa roxburghii pycnogenols molecule forms hydrophobic interaction with the macroporous adsorbent resin that is skeleton by vinylbenzene or toluylene, and therefore, available this class macroporous adsorbent resin carries out purifying to Rosa roxburghii pycnogenols, prepares highly purified Rosa roxburghii pycnogenols.
The object of the present invention is achieved like this: a kind of method of preparing Rosa roxburghii pycnogenols with Rosa roxburghii pulp: the commercially available Rosa roxburghii pulp of take is raw material, first prepare Rosa roxburghii pulp and juice, rear extraction pycnogenols, prepare again ultrafiltrated and Rosa roxburghii pycnogenols purification solution, finally prepare Rosa roxburghii pycnogenols powder.Its concrete grammar step is as follows:
(1) prepare Rosa roxburghii pulp and juice
The commercially available Rosa roxburghii pulp of take is raw material, first with pulverizer, pulverize, again in Single Roxburgh Rose Fruit meat quality (g): the volume of 15～25 ℃ of pure water (mL) is than the ratio that is 1: 10～30, Rosa roxburghii pulp and pure water after pulverizing are pumped in extractor, stir extraction and pump in expeller and squeeze the juice for the first time after 15～30 minutes.Collect juice extracting liquid for the first time, be placed in storage tank standby; Again in leaving the expeller of juice extracting slag for the first time, in the quality of juice extracting slag (g) for the first time: the volume of 15～25 ℃ of pure water (mL) is than the ratio that is 1: 5～20, again add pure water, again extract after 15～30 minutes and squeeze the juice for the second time, collect respectively juice extracting slag and for the second time juice extracting liquid for the second time.For the liquid of juice extracting for the second time of collecting, and after juice extracting liquid merges for the first time, in vacuum tightness, be 0.1MPa, temperature be under the condition of 50 ℃ till vacuum concentration to the volume fraction of soluble solids is 25～40%, as Rosa roxburghii pulp and juice; For the slag of juice extracting for the second time of collecting, as the raw material that extracts Rosa roxburghii pycnogenols.
(2) extract Rosa roxburghii pycnogenols
After (1) step completes, in juice extracting slag amount (g) for the second time: the volume fraction of 15～45 ℃ is that the volume (mL) of 40～60% ethanolic solns is than the ratio that is 1: 10～30, after juice extracting slag mixes with ethanolic soln for the second time, pump in extractor, under agitation extract after 30～60 minutes and carry out vacuum filtration, collect respectively Rosa roxburghii pycnogenols extraction slag and for the first time Rosa roxburghii pycnogenols extracting solution for the first time.The pycnogenols of Rosa roxburghii for the first time extracting solution for collecting, is placed in storage tank standby.For the pycnogenols of Rosa roxburghii for the first time of collecting, extract slag, in Rosa roxburghii pycnogenols for the first time, extract the quality (g) of slag: the volume fraction of 15～45 ℃ is that the volume (mL) of 40～60% ethanolic solns is than the ratio that is 1: 5～20, Rosa roxburghii pycnogenols extracts after slag mixes with ethanolic soln and pumps in extractor for the first time, under agitation extract after 30～60 minutes and carry out vacuum filtration, collect respectively Rosa roxburghii pycnogenols extraction slag and for the second time Rosa roxburghii pycnogenols extracting solution for the second time.For the slag of Rosa roxburghii pycnogenols extraction for the second time, mix with rice slag or rice bran etc., as the feed of the ruminating animals such as ox, sheep, rabbit; For Rosa roxburghii pycnogenols extracting solution for the second time, be placed in storage tank, and Rosa roxburghii pycnogenols extracting solution merges for the first time, prepares Rosa roxburghii pycnogenols extracting solution, for the preparation of ultrafiltrated.
(3) prepare ultrafiltrated
After (2) step completes, the Rosa roxburghii pycnogenols united extraction liquid pump that (2) step is prepared enters in the ultra-fine filter that molecular weight cut-off is 5000～10000Da, under the pressure of 0.1～0.2Mp, carry out ultrafiltration for the first time, until the volume of trapped fluid is while reducing to original volume 1/10.Collect respectively ultrafiltration filtered solution and for the first time ultrafiltration trapped fluid for the first time, the filtered solution of ultrafiltration for the first time for collecting, pumps in storage tank standby.For the trapped fluid of ultrafiltration for the first time of collecting, add wherein pure water, be supplemented to after original volume, under equal conditions carry out ultrafiltration for the second time, until trapped fluid volume while being reduced to original volume 1/10, is collected respectively ultrafiltration filtered solution and for the second time ultrafiltration trapped fluid for the second time.For the filtered solution of ultrafiltration for the second time of collecting, merge with the filtered solution of ultrafiltration for the first time of collecting, just prepare Rosa roxburghii pycnogenols and filter amalgamation liquid, for next step, adsorb Rosa roxburghii pycnogenols; The trapped fluid of ultrafiltration for the second time for collecting, pumps in spray-dryer, sprays dry at 135～160 ℃, obtains Polysaccharides from Rosa roxburghii protein powder, wherein contains a small amount of Rosa roxburghii pycnogenols, and this powder can be used for making products and health products additive agent.
(4) prepare Rosa roxburghii pycnogenols purification solution
After (3) step completes, Rosa roxburghii pycnogenols prepared by (3) step filters amalgamation liquid and pumps in adsorption resin column (AmberliteXAD7HP or ADS-17 or DM130), at flow velocity, be to adsorb under the condition of 2～6 times/hour of resin column volume, until cross while there is Rosa roxburghii pycnogenols in post effluent liquid, that collects de-Rosa roxburghii pycnogenols crosses post effluent liquid.For the adsorption resin column of load Rosa roxburghii pycnogenols, first with the pure water of 1～3 times of resin column volume, wash, in order to go out the impurity of interlaminar resin, collect washings.Adsorption resin column for the load Rosa roxburghii pycnogenols after pure water washing, the ethanolic soln that is 50～70% by volume fraction is to carry out wash-out under the condition of 2～6 times/hour of polymeric adsorbent column volume at eluent flow rate, absorbancy with UV spectrophotometer measuring elutriant at 280nm, until elutriant is at 280nm during without absorbancy, being collected in 280nm has the elutriant of absorbancy and the adsorption resin column of unloading Rosa roxburghii pycnogenols.For what collect, at 280nm, there is the elutriant of absorbancy, for the preparation of Rosa roxburghii pycnogenols powder.For the adsorption resin column of unloading Rosa roxburghii pycnogenols, after the pure water washing with 1 times of resin column volume, can be recycled; The washings after post liquid and pure water washing adsorption resin column of crossing for the de-Rosa roxburghii pycnogenols of collecting, pumps into biochemistry pool and processes, rear discharge up to standard.
(5) prepare Rosa roxburghii pycnogenols powder
After (4) step completes, the Rosa roxburghii pycnogenols elutriant that (4) step is collected pumps in counter-osmosis device, at working pressure, be under 1.5～2.5Mpa, to carry out reverse osmosis concentration, until when the mass concentration of Rosa roxburghii pycnogenols reaches 8～15% in concentrated solution, collect respectively reverse osmosis and see through liquid and concentrated solution.Reverse osmosis filtered solution for collecting, can be used for again extracting Rosa roxburghii pycnogenols; Reverse osmosis concentrated liquid for collecting, is placed in vacuum decker, in vacuum tightness, is 0.06～0.09MPa, and temperature is, under the condition of 50～60 ℃, to carry out vacuum concentration, until in concentrated solution during without ethanol taste, collect respectively vacuum condensation liquid and vacuum concentration liquid.Vacuum concentration liquid for collecting, pumps in spray-drier, in inlet temperature, is 130～150 ℃, and air outlet temperature is 80～95 ℃, and spraying centrifuge speed is, under the condition of 8090～12000 revs/min, spray and be dried.Collect dried powder, the Rosa roxburghii pycnogenols product that just to have obtained molecular-weight average 846Da, purity be 90～95%.For the vacuum condensation liquid of collecting, be the ethanolic soln that volume fraction is 30～75%, the ethanol that is 95% by volume fraction can be again for extracting or wash-out Rosa roxburghii pycnogenols after regulating concentration.
The present invention adopts after technique scheme, mainly contains following effect:
1, raw material of the present invention is Rosa roxburghii pulp, and wide material sources are cheap and easy to get, effectively reduced production cost.
2, the inventive method, when preparing Rosa roxburghii pycnogenols, is also prepared Rosa roxburghii pulp and juice and food and feed additive simultaneously, improves the utility value of Rosa roxburghii.
3, the present invention is simple at production process production unit, simple to operate when reducing costs save energy again, guarantee production safety.
4, in process of production, both no coupling product generated in the present invention, did not also have " three wastes " to produce, and all materials obtain recycle, belong to green bio Chemicals preparation method.
5, the Rosa roxburghii pycnogenols product purity that the present invention produces is all high, and solvability is good, and resistance of oxidation is strong, can be widely used in the industries such as food, medicine, makeup and healthcare products.
Embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment 1
A method of preparing Rosa roxburghii pycnogenols with Rosa roxburghii pulp, concrete steps are as follows:
(1) prepare Rosa roxburghii pulp and juice
The commercially available Rosa roxburghii pulp of take is raw material, first with pulverizer, pulverize, again in Single Roxburgh Rose Fruit meat quality (g): the volume of 15 ℃ of pure water (mL) is than the ratio that is 1: 10, Rosa roxburghii pulp and pure water after pulverizing are pumped in extractor, stir extraction and pump in expeller and squeeze the juice for the first time after 15 minutes.Collect juice extracting liquid for the first time, be placed in storage tank standby; Again in leaving the expeller of juice extracting slag for the first time, in the quality of juice extracting slag (g) for the first time: the volume of 15 ℃ of pure water (mL) is than the ratio that is 1: 5, after again adding pure water to mix, again extract after 15 minutes and squeeze the juice for the second time, collect respectively juice extracting slag and for the second time juice extracting liquid for the second time.For the liquid of juice extracting for the second time of collecting, and after juice extracting liquid merges for the first time, in vacuum tightness, be 0.1MPa, temperature be under the condition of 50 ℃ till vacuum concentration to the volume fraction of soluble solids is 25～40%, as Rosa roxburghii pulp and juice; For the slag of juice extracting for the second time of collecting, as the raw material that extracts Rosa roxburghii pycnogenols.
(2) extract Rosa roxburghii pycnogenols
After (1) step completes, in juice extracting slag amount (g) for the second time: the volume fraction of 15 ℃ is that the volume (mL) of 40% ethanolic soln is than the ratio that is 1: 10, juice extracting slag pumps in extractor after mixing with ethanolic soln for the second time, under agitation extract after 30 minutes and carry out vacuum filtration, collect respectively Rosa roxburghii pycnogenols extraction slag and for the first time Rosa roxburghii pycnogenols extracting solution for the first time.The pycnogenols of Rosa roxburghii for the first time extracting solution for collecting, is placed in storage tank standby.For the pycnogenols of Rosa roxburghii for the first time of collecting, extract slag, in Rosa roxburghii pycnogenols for the first time, extract the quality (g) of slag: the volume fraction of 15 ℃ is that the volume (mL) of 40% ethanolic soln is than the ratio that is 1: 5, Rosa roxburghii pycnogenols extracts after slag mixes with ethanolic soln and pumps in extractor for the first time, under agitation extract after 30 minutes and carry out vacuum filtration, collect respectively Rosa roxburghii pycnogenols extraction slag and for the second time Rosa roxburghii pycnogenols extracting solution for the second time.For the slag of Rosa roxburghii pycnogenols extraction for the second time, mix with rice slag or rice bran etc., as the feed of the ruminating animals such as ox, sheep, rabbit; For Rosa roxburghii pycnogenols extracting solution for the second time, be placed in storage tank, and Rosa roxburghii pycnogenols extracting solution merges for the first time, prepares Rosa roxburghii pycnogenols extracting solution, for the preparation of ultrafiltrated.
(3) prepare ultrafiltrated
After (2) step completes, the Rosa roxburghii pycnogenols united extraction liquid pump that (2) step is prepared enters in the ultra-fine filter that molecular weight cut-off is 5000Da, under the pressure of 0.10Mp, carry out ultrafiltration for the first time, until the volume of trapped fluid is while reducing to original volume 1/10.Collect respectively ultrafiltration filtered solution and for the first time ultrafiltration trapped fluid for the first time, the filtered solution of ultrafiltration for the first time for collecting, pumps in storage tank standby; The trapped fluid of ultrafiltration for the first time for collecting, adds pure water wherein, is supplemented to after original volume, under equal conditions carries out ultrafiltration for the second time, until trapped fluid volume is while being reduced to original volume 1/10.Collect respectively ultrafiltration filtered solution and for the second time ultrafiltration trapped fluid for the second time, for the filtered solution of ultrafiltration for the second time of collecting, merge with the filtered solution of ultrafiltration for the first time of collecting, just prepare Rosa roxburghii pycnogenols and filter amalgamation liquid, for next step, adsorb Rosa roxburghii pycnogenols; The trapped fluid of ultrafiltration for the second time for collecting, pumps in spray-dryer, sprays dry at 135 ℃, obtains Polysaccharides from Rosa roxburghii protein powder, wherein contains a small amount of Rosa roxburghii pycnogenols, and this powder can be used for making products and health products additive agent.
(4) prepare Rosa roxburghii pycnogenols purification solution
After (3) step completes, Rosa roxburghii pycnogenols prepared by (3) step filters amalgamation liquid and pumps in adsorption resin column (AmberliteXAD7HP or ADS-17 or DM130), at flow velocity, be to adsorb under the condition of 2 times/hour of resin column volume, until cross while there is Rosa roxburghii pycnogenols in post effluent liquid, that collects de-Rosa roxburghii pycnogenols crosses post effluent liquid.For the adsorption resin column of load Rosa roxburghii pycnogenols, first with the pure water of 1 times of resin column volume, wash, in order to go out the impurity of interlaminar resin, collect washings.Adsorption resin column for the load Rosa roxburghii pycnogenols after pure water washing, the ethanolic soln that is 50% by volume fraction is to carry out wash-out under the condition of 2 times/hour of polymeric adsorbent column volume at eluent flow rate, absorbancy with UV spectrophotometer measuring elutriant at 280nm, until elutriant is at 280nm during without absorbancy, being collected in 280nm has the elutriant of absorbancy and the adsorption resin column of unloading Rosa roxburghii pycnogenols.For what collect, at 280nm, there is the elutriant of absorbancy, for the preparation of Rosa roxburghii pycnogenols powder.For the adsorption resin column of unloading Rosa roxburghii pycnogenols, after the pure water washing with 1 times of resin column volume, can be recycled; The washings after post liquid and pure water washing adsorption resin column of crossing for the de-Rosa roxburghii pycnogenols of collecting, pumps into biochemistry pool and processes, rear discharge up to standard.
(5) prepare Rosa roxburghii pycnogenols powder
After (4) step completes, the Rosa roxburghii pycnogenols elutriant that (4) step is collected pumps in counter-osmosis device, at working pressure, be under 1.5Mpa, to carry out reverse osmosis concentration, until when the mass concentration of Rosa roxburghii pycnogenols reaches 8% in concentrated solution, collect respectively reverse osmosis and see through liquid and concentrated solution.Reverse osmosis filtered solution for collecting, can be used for again extracting Rosa roxburghii pycnogenols; Reverse osmosis concentrated liquid for collecting, is placed in vacuum decker, in vacuum tightness, is 0.06MPa, and temperature is, under the condition of 50 ℃, to carry out vacuum concentration, until in concentrated solution during without ethanol taste, collect respectively vacuum condensation liquid and vacuum concentration liquid.Vacuum concentration liquid for collecting, pumps in spray-drier, in inlet temperature, is 130 ℃, and air outlet temperature is 80 ℃, and spraying centrifuge speed is, under the condition of 8000 revs/min, spray and be dried; Collect dried powder, the Rosa roxburghii pycnogenols powder that just to have obtained molecular-weight average 846Da, purity be 90%.For the vacuum condensation liquid of collecting, be the ethanolic soln that volume fraction is 30%, the ethanol that is 95% by volume fraction can be again for extracting or wash-out Rosa roxburghii pycnogenols after regulating concentration.
Embodiment 2
A method of preparing Rosa roxburghii pycnogenols with Rosa roxburghii pulp, with embodiment 1, wherein:
In (1) step, Single Roxburgh Rose Fruit meat quality (g): the volume of 20 ℃ of pure water (mL), than the ratio that is 1: 20, extracts 25 minutes; The quality of juice extracting slag (g) for the first time: 20 ℃ of pure water volumes (mL), than the ratio that is 1: 10, extract 25 minutes, merges pressed liquor vacuum concentration to the volume fraction of soluble solids and is till 30%;
In (2) step, juice extracting slag amount (g) for the second time: the volume fraction of 30 ℃ be the volume (mL) of 60% ethanolic soln than the ratio that is 1: 20, extract 45 minutes; Rosa roxburghii pycnogenols extracts slag amount (g) for the first time: the volume fraction of 30 ℃ be 50% volumes of aqueous ethanol (mL) than the ratio that is 1: 10, extract 45 minutes;
In (3) step, ultra-fine filter molecular weight cut-off is 7000Da, carries out ultrafiltration for the first time under the pressure of 0.15Mp, and spraying drying temperature is 140 ℃;
In (4) step, absorption flow velocity is 4 times/hour of resin column volume, and the adsorption resin column for the load Rosa roxburghii pycnogenols of collecting, washs with the pure water of 2 times of resin column volumes, elutriant volume fraction of ethanol is 60%, and the flow velocity of elutriant is 4 times/hour of resin column volume;
In (5) step, reverse osmosis working pressure is 2.0Mpa, till when in concentrated solution, the mass concentration of Rosa roxburghii pycnogenols reaches 11%, vacuum concentration vacuum tightness is 0.07MPa, temperature is 55 ℃, and the dry network access temperature of spraying is 140 ℃, and going out net temperature is 90 ℃, spraying centrifuge speed is 10000 revs/min, the Rosa roxburghii pycnogenols powder that acquisition molecular-weight average 846Da, purity are 92%.
Embodiment 3
A method of preparing Rosa roxburghii pycnogenols with Rosa roxburghii pulp, with embodiment 1, wherein:
In (1) step, Single Roxburgh Rose Fruit meat quality (g): the volume of 25 ℃ of pure water (mL), than the ratio that is 1: 30, extracts 30 minutes; The quality of juice extracting slag (g) for the first time: 25 ℃ of pure water volumes (mL), than the ratio that is 1: 10, extract 30 minutes, merging pressed liquor vacuum concentration to the volume fraction of soluble solids is 40%;
In (2) step, juice extracting slag amount (g) for the second time: the volume fraction of 45 ℃ be the volume (mL) of 60% ethanolic soln than the ratio that is 1: 30, extract 60 minutes; Rosa roxburghii pycnogenols extracts slag amount (g) for the first time: the volume fraction of 45 ℃ be 60% volumes of aqueous ethanol (mL) than the ratio that is 1: 10, extract 60 minutes;
In (3) step, ultra-fine filter molecular weight cut-off is 10000Da, carries out ultrafiltration for the first time under the pressure of 0.2Mp, and spraying drying temperature is 150 ℃;
In (4) step, absorption flow velocity is 6 times/hour of resin column volume, and the adsorption resin column for the load Rosa roxburghii pycnogenols of collecting, washs with the pure water of 3 times of resin column volumes, elutriant volume fraction of ethanol is 70%, and the flow velocity of elutriant is 6 times/hour of resin column volume;
In (5) step, reverse osmosis working pressure is 2.5Mpa, till when in concentrated solution, the mass concentration of Rosa roxburghii pycnogenols reaches 15%, vacuum concentration vacuum tightness is 0.09MPa, temperature is 60 ℃, and the dry network access temperature of spraying is 150 ℃, and going out net temperature is 95 ℃, spraying centrifuge speed is 12000 revs/min, the Rosa roxburghii pycnogenols powder that acquisition molecular-weight average 846Da, purity are 96%.
Claims (1)
1. with Rosa roxburghii pulp, prepare a method for Rosa roxburghii pycnogenols, it is characterized in that concrete grammar step is as follows:
(1) extract Blackthorn pear fruit-juice
The commercially available Rosa roxburghii pulp of take is raw material, first with pulverizer, pulverize, again in Single Roxburgh Rose Fruit meat quality (g): the volume of 15～25 ℃ of pure water (mL) is than the ratio that is 1: 10～30, Rosa roxburghii pulp and pure water after pulverizing are pumped in extractor, stir extraction and pump in expeller and squeeze the juice for the first time after 15～30 minutes; Collect juice extracting liquid for the first time, be placed in storage tank; Again in leaving the expeller of juice extracting slag for the first time, in the quality of juice extracting slag (g) for the first time: the volume of 15～25 ℃ of pure water (mL) is than the ratio that is 1: 5～20, after again adding pure water to mix, again extract after 15～30 minutes and squeeze the juice for the second time, collect respectively juice extracting slag and for the second time juice extracting liquid for the second time; Will be for the second time juice extracting liquid be positioned in storage tank with after juice extracting liquid merges for the first time, in vacuum tightness, be 0.1MPa, temperature be under the condition of 50 ℃ till vacuum concentration to the volume fraction of soluble solids is 25～40%;
(2) extract Rosa roxburghii pycnogenols
After (1) step completes, in juice extracting slag amount (g) for the second time: the volume fraction of 15～45 ℃ is that the volume (mL) of 40～60% ethanolic solns is than the ratio that is 1: 10～30, after juice extracting slag mixes with ethanolic soln for the second time, pump in extractor, under agitation extract after 30～60 minutes and carry out vacuum filtration, collect respectively Rosa roxburghii pycnogenols extraction slag and for the first time Rosa roxburghii pycnogenols extracting solution for the first time; The pycnogenols of Rosa roxburghii for the first time extracting solution by collecting, is placed in storage tank; For the pycnogenols of Rosa roxburghii for the first time of collecting, extract slag, in Rosa roxburghii pycnogenols for the first time, extract the quality (g) of slag: the volume fraction of 15～45 ℃ is that the volume (mL) of 40～60% ethanolic solns is than the ratio that is 1: 5～20, Rosa roxburghii pycnogenols extracts after slag mixes with ethanolic soln and pumps in extractor for the first time, under agitation extract after 30～60 minutes and carry out vacuum filtration, collect respectively Rosa roxburghii pycnogenols extraction slag and for the second time Rosa roxburghii pycnogenols extracting solution for the second time; For Rosa roxburghii pycnogenols extracting solution for the second time, be placed in tank, merge with Rosa roxburghii pycnogenols extracting solution for the first time;
(3) prepare ultrafiltrated
After (2) step completes, the Rosa roxburghii pycnogenols united extraction liquid pump that (2) step is prepared enters in the ultra-fine filter that molecular weight cut-off is 5000～10000Da, under the pressure of 0.1～0.2Mp, carry out ultrafiltration for the first time, until the volume of trapped fluid is collected respectively ultrafiltration filtered solution and for the first time ultrafiltration trapped fluid for the first time while reducing to original volume 1/10, the filtered solution of ultrafiltration for the first time for collecting, pumps in storage tank; For the trapped fluid of ultrafiltration for the first time of collecting, add wherein pure water, be supplemented to after original volume, under equal conditions carry out ultrafiltration for the second time, until trapped fluid volume while being reduced to original volume 1/10, is collected respectively ultrafiltration filtered solution and for the second time ultrafiltration trapped fluid for the second time; For the filtered solution of ultrafiltration for the second time of collecting, merge with the filtered solution of ultrafiltration for the first time of collecting; The trapped fluid of ultrafiltration for the second time for collecting, pumps in spray-dryer, sprays dry at 135～160 ℃;
(4) prepare Rosa roxburghii pycnogenols purification solution
After (3) step completes, Rosa roxburghii pycnogenols prepared by (3) step filters amalgamation liquid and pumps in adsorption resin column AmberliteXAD7HP or ADS-17 or DM130, at flow velocity, be to adsorb under the condition of 2～6 times/hour of resin column volume, until cross while there is Rosa roxburghii pycnogenols in post effluent liquid, that collects de-Rosa roxburghii pycnogenols crosses post effluent liquid; For the adsorption resin column of load Rosa roxburghii pycnogenols, first with the pure water of 1～3 times of resin column volume, wash, collect washings; Adsorption resin column for the load Rosa roxburghii pycnogenols after pure water washing, the ethanolic soln that is 50～70% by volume fraction is to carry out wash-out under the condition of 2～6 times/hour of polymeric adsorbent column volume at eluent flow rate, absorbancy with UV spectrophotometer measuring elutriant at 280nm, until elutriant is at 280nm during without absorbancy, being collected in 280nm has the elutriant of absorbancy and the polymeric adsorbent of unloading Rosa roxburghii pycnogenols;
(5) prepare Rosa roxburghii pycnogenols powder
After (4) step completes, the Rosa roxburghii pycnogenols elutriant that (4) step is collected pumps into respectively in counter-osmosis device, at working pressure, be under 1.5～2.5Mpa, to carry out reverse osmosis concentration, until when in concentrated solution, the mass concentration of Rosa roxburghii pycnogenols reaches 8～15%; Collect respectively reverse osmosis and see through liquid and concentrated solution; Reverse osmosis concentrated liquid for collecting, is placed in vacuum decker, in vacuum tightness, is 0.06～0.09MPa, and temperature is, under the condition of 50～60 ℃, to carry out vacuum concentration, until in concentrated solution during without ethanol taste, collect respectively phlegma and concentrated solution; Concentrated solution for collecting, pumps in spray-drier, in inlet temperature, is 130～150 ℃, and air outlet temperature is 80～95 ℃, and spraying centrifuge speed is, under the condition of 8000～12000 revs/min, spray and be dried; Collect dried powder, the Rosa roxburghii pycnogenols powder that just to have obtained molecular-weight average 846Da, purity be 90～95%.
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| CN103054031A (en) * | 2013-01-30 | 2013-04-24 | 李保生 | Food additive roxburgh rose essence and production method |
| CN104472974A (en) * | 2014-12-17 | 2015-04-01 | 中国科学院过程工程研究所 | Comprehensive utilization method for raw material rich in polyphenol |
| CN105754373B (en) * | 2016-03-09 | 2017-08-08 | 阿坝县天赐阳光生物科技有限公司 | A kind of method of application fruits and vegetables vegetables pigment, vegetable beverage and Vegetable powder |
| CN110024893A (en) * | 2019-05-07 | 2019-07-19 | 贵阳学院 | A kind of preparation method of Ribes burejense health care tea |
| CN110200865A (en) * | 2019-05-12 | 2019-09-06 | 广州芊舟生物科技有限公司 | A kind of Fructus Rosae Normalis extract and its preparation method and application |
| CN114456246A (en) * | 2022-02-25 | 2022-05-10 | 瀚科(浙江)生物科技有限责任公司 | Method for improving antibacterial activity and thermal stability of roxburgh rose protein and application |
| CN115005398A (en) * | 2022-06-15 | 2022-09-06 | 长顺丹索亚刺梨庄园有限公司 | Method for preparing roxburgh rose ultrafine powder |
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