CN102718737A - 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
- Publication number
- CN102718737A CN102718737A CN201210194965XA CN201210194965A CN102718737A CN 102718737 A CN102718737 A CN 102718737A CN 201210194965X A CN201210194965X A CN 201210194965XA CN 201210194965 A CN201210194965 A CN 201210194965A CN 102718737 A CN102718737 A CN 102718737A
- Authority
- CN
- China
- Prior art keywords
- pycnogenols
- rosa roxburghii
- time
- volume
- collecting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
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 the pycnogenols preparing technical field, be specifically related to prepare the method for Rosa roxburghii pycnogenols with Rosa roxburghii pulp.
Two, background technology
Pycnogenols is a kind of Vitamin P complex that special molecular structure is arranged; Mostly be the reddish-brown powder; Little, the puckery of gas; Be the most effective natural antioxidants of radical in the removing human body of generally acknowledging in the world at present, have that protection is cardiovascular, functions such as preventing hypertension, antitumor action, radiation resistance, beauty treatment are crease-resistant, delay senility, antianaphylaxis, vision protection, treatment inflammation.
Rosa roxburghii is the common wild fruit in area, China west and south.Fruit of Grossularia burejensis Berger contains abundant vitamins C; Every hectogram fresh fruit Vitamin C content is 2000mg, therefore is referred to as " king of dimension C ", and pulp is sour and astringent; It is poor to eat mouthfeel raw; So Rosa roxburghii is processed into the Sucus Rosae Normalis preservation, and processes 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 the pycnogenols composition, has good pharmaceutical use and nutritive value, liked by the human consumer.
The preparation method of existing pycnogenols, as on November 02nd, 2011 disclosed publication number be " a kind of preparation method of rose Root of Kirilow Rhodiola pycnogenols " patent of CN102229592A, disclosed method is to be raw material with rose Root of Kirilow Rhodiola rhizome; Extract through alcoholic solvent; The sherwood oil grease removal, high concentration ethanol removes sugar, column chromatographic isolation and purification; Lyophilize and content＞95%, the pycnogenols of yield＞88.3%.The main drawback of this method is: 1. only be difficult to remove small molecules or the macromole impurity in the extracting solution with deposition or extraction, these impurity can influence quality product.2. can only prepare a kind of product of pycnogenols.3. such scheme is to extracting, separate the residue that produces in the pycnogenols 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 objective of the invention is to prepare the weak point of pycnogenols, a kind of method for preparing the Rosa roxburghii pycnogenols with Rosa roxburghii pulp is provided to existing method.This method raw material is a Rosa roxburghii pulp, and wide material sources, cheap and easy to get reduce production costs effectively; When preparing the Rosa roxburghii pycnogenols, also make 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, does not have " three wastes " discharging, helps environmental protection; Characteristics 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 Rosa roxburghii pycnogenols is dissolvable in water in the certain density ethanolic soln by the catechin of different quantities or the chromocor compound of l-Epicatechol be combined into, extracts in the available ethanolic soln cluster needling pear flesh residue; Rosa roxburghii pycnogenols molecular weight much smaller than the molecular weight of protein, polysaccharide, can be realized separating between 300～2000Da through ultrafiltration; Phenyl on the Rosa roxburghii pycnogenols molecule forms hydrophobic interaction with the macroporous adsorbent resin that by vinylbenzene or toluylene is skeleton, and therefore, available this type macroporous adsorbent resin carries out purifying to the Rosa roxburghii pycnogenols, prepares highly purified Rosa roxburghii pycnogenols.
The objective of the invention is to realize like this: a kind of method for preparing the Rosa roxburghii pycnogenols with Rosa roxburghii pulp: with commercially available Rosa roxburghii pulp is raw material; Prepare the Rosa roxburghii pulp and juice earlier; Pycnogenols is extracted in the back; Refabrication ultrafiltrated and Rosa roxburghii pycnogenols purification solution prepare Rosa roxburghii pycnogenols powder at last.Its concrete grammar step is following:
(1) preparation Rosa roxburghii pulp and juice
With commercially available Rosa roxburghii pulp is raw material; Pulverize with kibbler earlier; 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 the extractor, stir to extract to pump into after 15～30 minutes and carry out in the expeller squeezing the juice the first time.Collect fruit juice pressed liquor for the first time, place storage tank subsequent use; Again in the expeller that leaves the fruit juice press residue first time; Quality (g) in the fruit juice press residue first time: the volume of 15～25 ℃ of pure water (mL) is than the ratio that is 1: 5～20; Add pure water once more; Extract once more after 15～30 minutes and carry out squeezing the juice the second time, collect fruit juice press residue and the fruit juice pressed liquor second time for the second time respectively.For the second time of the fruit juice pressed liquor of collecting and after the fruit juice pressed liquor merges for the first time, be 0.1MPa in vacuum tightness, temperature be under 50 ℃ the condition till the volume(tric)fraction of vacuum concentration to soluble solids is 25～40%, as the Rosa roxburghii pulp and juice; For the fruit juice press residue of the collecting second time, as the raw material that extracts the Rosa roxburghii pycnogenols.
(2) extract the Rosa roxburghii pycnogenols
After the completion of (1) step; In fruit juice press residue quality (g) for the second time: 15～45 ℃ volume(tric)fraction is that the volume (mL) of 40～60% ethanolic solns is than the ratio that is 1: 10～30; After fruit juice press residue and ethanolic soln mix for the second time; Pump in the extractor, under agitation extract after 30～60 minutes and carry out vacuum filtration, collecting for the first time respectively, the Rosa roxburghii pycnogenols extracts slag and the Rosa roxburghii pycnogenols extracting solution first time.The Rosa roxburghii pycnogenols extracting solution first time for collecting places storage tank subsequent use.The Rosa roxburghii pycnogenols first time for collecting extracts slag; Extract the quality (g) of slag in Rosa roxburghii pycnogenols for the first time: 15～45 ℃ volume(tric)fraction is that the volume (mL) of 40～60% ethanolic solns is than the ratio that is 1: 5～20; Pump in the extractor after Rosa roxburghii pycnogenols extraction slag and ethanolic soln mix for the first time; Under agitation extract after 30～60 minutes and carry out vacuum filtration, collecting for the second time respectively, the Rosa roxburghii pycnogenols extracts slag and the Rosa roxburghii pycnogenols extracting solution second time.For Rosa roxburghii pycnogenols extraction second time slag, mix with rice slag or rice bran etc., as the feed of ruminating animals such as ox, sheep, rabbit; For the second time Rosa roxburghii pycnogenols extracting solution place storage tank and for the first time Rosa roxburghii pycnogenols extracting solution merge, promptly prepare Rosa roxburghii pycnogenols extracting solution, be used to prepare ultrafiltrated.
(3) preparation ultrafiltrated
After the completion of (2) step; The Rosa roxburghii pycnogenols united extraction liquid pump that (2) step prepared is gone in the ultra-fine filter that molecular weight cut-off is 5000～10000Da; Under the pressure of 0.1～0.2Mp, carry out the ultrafiltration first time, when the volume of trapped fluid reduces to original volume 1/10 till.Collect filtered solution of ultrafiltration for the first time and the trapped fluid of ultrafiltration for the first time respectively, the ultrafiltration first time filtered solution for collecting pumps in the storage tank subsequent use.For the ultrafiltration first time trapped fluid of collecting; After wherein adding pure water, being supplemented to original volume, under equal conditions carry out the ultrafiltration second time; Till when the trapped fluid volume is reduced to original volume 1/10, collect filtered solution of ultrafiltration for the second time and the trapped fluid of ultrafiltration for the second time respectively.For the ultrafiltration second time filtered solution of collecting, merge with the ultrafiltration first time filtered solution of collecting, just prepare the Rosa roxburghii pycnogenols and filter amalgamation liquid, be used for next step and adsorb the Rosa roxburghii pycnogenols; Ultrafiltration second time trapped fluid for collecting pumps in the spray-dryer, under 135～160 ℃, carries out spraying drying, promptly obtains Rosa roxburghii polyose-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) preparation Rosa roxburghii pycnogenols purification solution
After the completion of (3) step; The Rosa roxburghii pycnogenols filtration amalgamation liquid of (3) step preparation is pumped in the adsorption resin column (Amberlite XAD7HP or ADS-17 or DM130); Be to adsorb under 2～6 times/hour the condition of resin column volume at flow velocity; Till when in mistake post effluent, the Rosa roxburghii pycnogenols occurring, collect the post effluent excessively that takes off the Rosa roxburghii pycnogenols.For the adsorption resin column of load Rosa roxburghii pycnogenols, earlier the pure water with 1～3 times of resin column volume washs, in order to go out the impurity of interlaminar resin, the collection washings.Adsorption resin column for the load Rosa roxburghii pycnogenols after the pure water washing; Using volume(tric)fraction is that 50～70% ethanolic soln carries out wash-out under 2～6 times/hour the condition of eluent flow rate as the polymeric adsorbent column volume; With the absorbancy of UV spectrophotometer measuring elutriant at 280nm; Till elutriant was not when 280nm has absorbancy, being collected in 280nm had the elutriant of absorbancy and the adsorption resin column of unloading Rosa roxburghii pycnogenols.At 280nm the elutriant of absorbancy is arranged for what collect, be used to prepare 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 behind post liquid and the pure water washing adsorption resin column of crossing that takes off the Rosa roxburghii pycnogenols for collecting pumps into biochemistry pool and handles, and discharge back up to standard.
(5) preparation Rosa roxburghii pycnogenols powder
After the completion of (4) step; The Rosa roxburghii pycnogenols elutriant that (4) step was collected pumps in the counter-osmosis device; At working pressure is to carry out reverse osmosis concentration under 1.5～2.5Mpa; Till the mass concentration of Rosa roxburghii pycnogenols reached 8～15% o'clock in liquid concentrator, collect r-o-respectively and see through liquid and liquid concentrator.R-o-filtered solution for collecting can be used for extracting once more the Rosa roxburghii pycnogenols; Reverse osmosis concentrated liquid for collecting places vacuum decker, is 0.06～0.09MPa in vacuum tightness, and temperature is under 50～60 ℃ the condition, to carry out vacuum concentration, when no ethanol is distinguished the flavor of in liquid concentrator till, collect vacuum condensation liquid and vacuum concentration liquid respectively.Vacuum concentration liquid for collecting pumps in the spray-drier, is 130～150 ℃ at EAT, and air outlet temperature is 80～95 ℃, and the spraying centrifuge speed is under 8090～12000 rev/mins the condition, to carry out spraying drying.Collect dried powder, just obtained molecular-weight average 846Da, purity and be 90～95% Rosa roxburghii pycnogenols product.For the vacuum condensation liquid of collecting, for volume(tric)fraction is 30～75% ethanolic soln, using volume(tric)fraction is can be used for once more extracting or wash-out Rosa roxburghii pycnogenols after 95% ethanol is regulated concentration.
After the present invention adopts technique scheme, mainly contain following effect:
1, raw material of the present invention is a Rosa roxburghii pulp, and wide material sources are cheap and easy to get, reduced production cost effectively.
2, the inventive method is also prepared Rosa roxburghii pulp and juice and food and feed additive simultaneously when preparing the Rosa roxburghii pycnogenols, improves the utility value of Rosa roxburghii.
3, the present invention is simple at the production process production unit, simple to operate when reducing cost save energy again, guarantee production safety.
4, the present invention in process of production, both no coupling product generates, and does not also have " three wastes " to produce, all materials obtain recycle, belong to green bio Chemicals preparation method.
5, the Rosa roxburghii pycnogenols product purity of the present invention's production 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 specify the present invention.
Embodiment 1
A kind ofly prepare the method for Rosa roxburghii pycnogenols with Rosa roxburghii pulp, concrete steps are following:
(1) preparation Rosa roxburghii pulp and juice
With commercially available Rosa roxburghii pulp is raw material; Pulverize with kibbler earlier; 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 the extractor, stir to extract to pump into after 15 minutes and carry out in the expeller squeezing the juice the first time.Collect fruit juice pressed liquor for the first time, place storage tank subsequent use; Again in the expeller that leaves the fruit juice press residue first time; Quality (g) in the fruit juice press residue first time: the volume of 15 ℃ of pure water (mL) is than the ratio that is 1: 5; Add once more after pure water mixes; Extract once more after 15 minutes and carry out squeezing the juice the second time, collect fruit juice press residue and the fruit juice pressed liquor second time for the second time respectively.For the second time of the fruit juice pressed liquor of collecting and after the fruit juice pressed liquor merges for the first time, be 0.1MPa in vacuum tightness, temperature be under 50 ℃ the condition till the volume(tric)fraction of vacuum concentration to soluble solids is 25～40%, as the Rosa roxburghii pulp and juice; For the fruit juice press residue of the collecting second time, as the raw material that extracts the Rosa roxburghii pycnogenols.
(2) extract the Rosa roxburghii pycnogenols
After the completion of (1) step; In fruit juice press residue quality (g) for the second time: 15 ℃ volume(tric)fraction is that the volume (mL) of 40% ethanolic soln is than the ratio that is 1: 10; Pump in the extractor after fruit juice press residue and ethanolic soln mix for the second time; Under agitation extract after 30 minutes and carry out vacuum filtration, collecting for the first time respectively, the Rosa roxburghii pycnogenols extracts slag and the Rosa roxburghii pycnogenols extracting solution first time.The Rosa roxburghii pycnogenols extracting solution first time for collecting places storage tank subsequent use.The Rosa roxburghii pycnogenols first time for collecting extracts slag; Extract the quality (g) of slag in Rosa roxburghii pycnogenols for the first time: 15 ℃ volume(tric)fraction is that the volume (mL) of 40% ethanolic soln is than the ratio that is 1: 5; Pump in the extractor after Rosa roxburghii pycnogenols extraction slag and ethanolic soln mix for the first time; Under agitation extract after 30 minutes and carry out vacuum filtration, collecting for the second time respectively, the Rosa roxburghii pycnogenols extracts slag and the Rosa roxburghii pycnogenols extracting solution second time.For Rosa roxburghii pycnogenols extraction second time slag, mix with rice slag or rice bran etc., as the feed of ruminating animals such as ox, sheep, rabbit; For the second time Rosa roxburghii pycnogenols extracting solution place storage tank and for the first time Rosa roxburghii pycnogenols extracting solution merge, promptly prepare Rosa roxburghii pycnogenols extracting solution, be used to prepare ultrafiltrated.
(3) preparation ultrafiltrated
(2) step went into the Rosa roxburghii pycnogenols united extraction liquid pump that (2) step prepared in the ultra-fine filter that molecular weight cut-off is 5000Da after accomplishing, and under the pressure of 0.10Mp, carried out the ultrafiltration first time, when the volume of trapped fluid reduces to original volume 1/10 till.Collect filtered solution of ultrafiltration for the first time and the trapped fluid of ultrafiltration for the first time respectively, the ultrafiltration first time filtered solution for collecting pumps in the storage tank subsequent use; Ultrafiltration first time trapped fluid for collecting after wherein adding pure water, being supplemented to original volume, under equal conditions carries out the ultrafiltration second time, when the trapped fluid volume is reduced to original volume 1/10 till.Collect filtered solution of ultrafiltration for the second time and the trapped fluid of ultrafiltration for the second time respectively; For the ultrafiltration second time filtered solution of collecting; Merge with the ultrafiltration first time filtered solution of collecting, just prepare the Rosa roxburghii pycnogenols and filter amalgamation liquid, be used for next step and adsorb the Rosa roxburghii pycnogenols; Ultrafiltration second time trapped fluid for collecting pumps in the spray-dryer, under 135 ℃, carries out spraying drying, promptly obtains Rosa roxburghii polyose-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) preparation Rosa roxburghii pycnogenols purification solution
After the completion of (3) step; The Rosa roxburghii pycnogenols filtration amalgamation liquid of (3) step preparation is pumped in the adsorption resin column (Amberlite XAD7HP or ADS-17 or DM130); Be to adsorb under 2 times/hour the condition of resin column volume at flow velocity; Till when in mistake post effluent, the Rosa roxburghii pycnogenols occurring, collect the post effluent excessively that takes off the Rosa roxburghii pycnogenols.For the adsorption resin column of load Rosa roxburghii pycnogenols, earlier the pure water with 1 times of resin column volume washs, in order to go out the impurity of interlaminar resin, the collection washings.Adsorption resin column for the load Rosa roxburghii pycnogenols after the pure water washing; Using volume(tric)fraction is that 50% ethanolic soln carries out wash-out under 2 times/hour the condition of eluent flow rate as the polymeric adsorbent column volume; With the absorbancy of UV spectrophotometer measuring elutriant at 280nm; Till elutriant was not when 280nm has absorbancy, being collected in 280nm had the elutriant of absorbancy and the adsorption resin column of unloading Rosa roxburghii pycnogenols.At 280nm the elutriant of absorbancy is arranged for what collect, be used to prepare 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 behind post liquid and the pure water washing adsorption resin column of crossing that takes off the Rosa roxburghii pycnogenols for collecting pumps into biochemistry pool and handles, and discharge back up to standard.
(5) preparation Rosa roxburghii pycnogenols powder
After the completion of (4) step; The Rosa roxburghii pycnogenols elutriant that (4) step was collected pumps in the counter-osmosis device; At working pressure is to carry out reverse osmosis concentration under the 1.5Mpa, till the mass concentration of Rosa roxburghii pycnogenols reached 8% o'clock in liquid concentrator, collects r-o-respectively and sees through liquid and liquid concentrator.R-o-filtered solution for collecting can be used for extracting once more the Rosa roxburghii pycnogenols; Reverse osmosis concentrated liquid for collecting places vacuum decker, is 0.06MPa in vacuum tightness, and temperature is under 50 ℃ the condition, to carry out vacuum concentration, when no ethanol is distinguished the flavor of in liquid concentrator till, collect vacuum condensation liquid and vacuum concentration liquid respectively.Vacuum concentration liquid for collecting pumps in the spray-drier, is 130 ℃ at EAT, and air outlet temperature is 80 ℃, and the spraying centrifuge speed is under 8000 rev/mins the condition, to carry out spraying drying; Collect dried powder, just obtained molecular-weight average 846Da, purity and be 90% Rosa roxburghii pycnogenols powder.For the vacuum condensation liquid of collecting, for volume(tric)fraction is 30% ethanolic soln, using volume(tric)fraction is can be used for once more extracting or wash-out Rosa roxburghii pycnogenols after 95% ethanol is regulated concentration.
Embodiment 2
A kind ofly prepare the method for 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) extracted 25 minutes than the ratio that is 1: 20; The quality (g) of fruit juice press residue for the first time: 20 ℃ of pure water volumes (mL) extracted 25 minutes than the ratio that is 1: 10, and the volume(tric)fraction of merging pressed liquor vacuum concentration to soluble solids is till 30%;
In (2) step, fruit juice press residue quality (g) for the second time: 30 ℃ volume(tric)fraction be the volume (mL) of 60% ethanolic soln than the ratio that is 1: 20, extracted 45 minutes; For the first time the Rosa roxburghii pycnogenols extracts slag amount (g): 30 ℃ volume(tric)fraction be 50% volumes of aqueous ethanol (mL) than the ratio that is 1: 10, extracted 45 minutes;
In (3) step, the ultra-fine filter molecular weight cut-off is 7000Da, under the pressure of 0.15Mp, carries out the ultrafiltration first time, and the spraying drying temperature is 140 ℃;
In (4) step; The absorption flow velocity is 4 times/hour of resin column volume, for the adsorption resin column of the load Rosa roxburghii pycnogenols of collecting, washs with the pure water of 2 times of resin column volumes; Elutriant ethanol volume(tric)fraction is 60%, and the flow velocity of elutriant is 4 times/hour of resin column volume;
In (5) step, the r-o-working pressure is 2.0Mpa, till the mass concentration of Rosa roxburghii pycnogenols reached 11% o'clock in the liquid concentrator; Vacuum concentration vacuum tightness is 0.07MPa; Temperature is 55 ℃, and spraying drying network access temperature is 140 ℃, and going out to net temperature is 90 ℃; The spraying centrifuge speed is 10000 rev/mins, and acquisition molecular-weight average 846Da, purity are 92% Rosa roxburghii pycnogenols powder.
Embodiment 3
A kind ofly prepare the method for 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) extracted 30 minutes than the ratio that is 1: 30; The quality (g) of fruit juice press residue for the first time: 25 ℃ of pure water volumes (mL) extracted 30 minutes than the ratio that is 1: 10, and the volume(tric)fraction of merging pressed liquor vacuum concentration to soluble solids is 40%;
In (2) step, fruit juice press residue quality (g) for the second time: 45 ℃ volume(tric)fraction be the volume (mL) of 60% ethanolic soln than the ratio that is 1: 30, extracted 60 minutes; For the first time the Rosa roxburghii pycnogenols extracts slag amount (g): 45 ℃ volume(tric)fraction be 60% volumes of aqueous ethanol (mL) than the ratio that is 1: 10, extracted 60 minutes;
In (3) step, the ultra-fine filter molecular weight cut-off is 10000Da, under the pressure of 0.2Mp, carries out the ultrafiltration first time, and the spraying drying temperature is 150 ℃;
In (4) step; The absorption flow velocity is 6 times/hour of resin column volume, for the adsorption resin column of the load Rosa roxburghii pycnogenols of collecting, washs with the pure water of 3 times of resin column volumes; Elutriant ethanol volume(tric)fraction is 70%, and the flow velocity of elutriant is 6 times/hour of resin column volume;
In (5) step, the r-o-working pressure is 2.5Mpa, till the mass concentration of Rosa roxburghii pycnogenols reached 15% o'clock in the liquid concentrator; Vacuum concentration vacuum tightness is 0.09MPa; Temperature is 60 ℃, and spraying drying network access temperature is 150 ℃, and going out to net temperature is 95 ℃; The spraying centrifuge speed is 12000 rev/mins, and acquisition molecular-weight average 846Da, purity are 96% Rosa roxburghii pycnogenols powder.
Claims (1)
1. one kind prepares the method for Rosa roxburghii pycnogenols with Rosa roxburghii pulp, it is characterized in that the concrete grammar step is following:
(1) extracts Blackthorn pear fruit-juice
With commercially available Rosa roxburghii pulp is raw material; Pulverize with kibbler earlier; 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 the extractor, stir to extract to pump into after 15～30 minutes and carry out in the expeller squeezing the juice the first time; Collect fruit juice pressed liquor for the first time, place storage tank; Again in the expeller that leaves the fruit juice press residue first time; Quality (g) in the fruit juice press residue first time: the volume of 15～25 ℃ of pure water (mL) is than the ratio that is 1: 5～20; Add once more after pure water mixes; Extract once more after 15～30 minutes and carry out squeezing the juice the second time, collect fruit juice press residue and the fruit juice pressed liquor second time for the second time respectively; For the second time the fruit juice pressed liquor is positioned in the storage tank with after the first time, the fruit juice pressed liquor merged, and is 0.1MPa in vacuum tightness, temperature be under 50 ℃ the condition till the volume(tric)fraction of vacuum concentration to soluble solids is 25～40%;
(2) extract the Rosa roxburghii pycnogenols
After the completion of (1) step; In fruit juice press residue quality (g) for the second time: 15～45 ℃ volume(tric)fraction is that the volume (mL) of 40～60% ethanolic solns is than the ratio that is 1: 10～30; After fruit juice press residue and ethanolic soln mix for the second time; Pump in the extractor, under agitation extract after 30～60 minutes and carry out vacuum filtration, collecting for the first time respectively, the Rosa roxburghii pycnogenols extracts slag and the Rosa roxburghii pycnogenols extracting solution first time; The Rosa roxburghii pycnogenols extracting solution first time with collecting places storage tank; The Rosa roxburghii pycnogenols first time for collecting extracts slag; Extract the quality (g) of slag in Rosa roxburghii pycnogenols for the first time: 15～45 ℃ volume(tric)fraction is that the volume (mL) of 40～60% ethanolic solns is than the ratio that is 1: 5～20; Pump in the extractor after Rosa roxburghii pycnogenols extraction slag and ethanolic soln mix for the first time; Under agitation extract after 30～60 minutes and carry out vacuum filtration, collecting for the second time respectively, the Rosa roxburghii pycnogenols extracts slag and the Rosa roxburghii pycnogenols extracting solution second time; For the Rosa roxburghii pycnogenols extracting solution second time, place jar, with the Rosa roxburghii pycnogenols extracting solution merging first time;
(3) preparation ultrafiltrated
After the completion of (2) step; The Rosa roxburghii pycnogenols united extraction liquid pump that (2) step prepared is gone in the ultra-fine filter that molecular weight cut-off is 5000～10000Da; Under the pressure of 0.1～0.2Mp, carry out the ultrafiltration first time, collect filtered solution of ultrafiltration for the first time and the trapped fluid of ultrafiltration for the first time respectively till when the volume of trapped fluid reduces to original volume 1/10; Ultrafiltration first time filtered solution for collecting pumps in the storage tank; For the ultrafiltration first time trapped fluid of collecting; After wherein adding pure water, being supplemented to original volume, under equal conditions carry out the ultrafiltration second time; Till when the trapped fluid volume is reduced to original volume 1/10, collect filtered solution of ultrafiltration for the second time and the trapped fluid of ultrafiltration for the second time respectively; For the ultrafiltration second time filtered solution of collecting, merge with the ultrafiltration first time filtered solution of collecting; Ultrafiltration second time trapped fluid for collecting pumps in the spray-dryer, under 135～160 ℃, carries out spraying drying;
(4) preparation Rosa roxburghii pycnogenols purification solution
After the completion of (3) step; The Rosa roxburghii pycnogenols filtration amalgamation liquid of (3) step preparation is pumped in the adsorption resin column (Amberlite XAD7HP or ADS-17 or DM130); Be to adsorb under 2～6 times/hour the condition of resin column volume at flow velocity; Till when in mistake post effluent, the Rosa roxburghii pycnogenols occurring, collect the post effluent excessively that takes off the Rosa roxburghii pycnogenols; For the adsorption resin column of load Rosa roxburghii pycnogenols, the pure water with 1～3 times of resin column volume washs earlier, collects washings; Adsorption resin column for the load Rosa roxburghii pycnogenols after the pure water washing; Using volume(tric)fraction is that 50～70% ethanolic soln carries out wash-out under 2～6 times/hour the condition of eluent flow rate as the polymeric adsorbent column volume; With the absorbancy of UV spectrophotometer measuring elutriant at 280nm; Till elutriant was not when 280nm has absorbancy, being collected in 280nm had the elutriant of absorbancy and the polymeric adsorbent of unloading Rosa roxburghii pycnogenols;
(5) preparation Rosa roxburghii pycnogenols powder
(4) step went on foot the Rosa roxburghii pycnogenols elutriant of collecting with (4) and pumps into respectively in the counter-osmosis device after accomplishing, and was to carry out reverse osmosis concentration under 1.5～2.5Mpa at working pressure, till the mass concentration of Rosa roxburghii pycnogenols reached 8～15% o'clock in liquid concentrator; Collect r-o-respectively and see through liquid and liquid concentrator; Reverse osmosis concentrated liquid for collecting places vacuum decker, is 0.06～0.09MPa in vacuum tightness, and temperature is under 50～60 ℃ the condition, to carry out vacuum concentration, when no ethanol is distinguished the flavor of in liquid concentrator till, collect phlegma and liquid concentrator respectively; Liquid concentrator for collecting pumps in the spray-drier, is 130～150 ℃ at EAT, and air outlet temperature is 80～95 ℃, and the spraying centrifuge speed is under 8000～12000 rev/mins the condition, to carry out spraying drying; Collect dried powder, just obtained molecular-weight average 846Da, purity and be 90～95% Rosa roxburghii pycnogenols powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210194965.XA CN102718737B (en) | 2012-05-31 | 2012-05-31 | Method of using roxburgh rose pulp to prepare roxburgh rose procyanidine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210194965.XA CN102718737B (en) | 2012-05-31 | 2012-05-31 | Method of using roxburgh rose pulp to prepare roxburgh rose procyanidine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102718737A true CN102718737A (en) | 2012-10-10 |
| CN102718737B CN102718737B (en) | 2014-10-08 |
Family
ID=46944637
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210194965.XA Expired - Fee Related CN102718737B (en) | 2012-05-31 | 2012-05-31 | Method of using roxburgh rose pulp to prepare roxburgh rose procyanidine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102718737B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105754373A (en) * | 2016-03-09 | 2016-07-13 | 阿坝县天赐阳光生物科技有限公司 | Methods for processing vegetable pigments, vegetable beverages 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093748A (en) * | 2011-01-17 | 2011-06-15 | 重庆海巨农业发展有限公司 | Method for preparing radish red pigment homopolymer and radish proanthocyanidin from red-core radishes |
-
2012
- 2012-05-31 CN CN201210194965.XA patent/CN102718737B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093748A (en) * | 2011-01-17 | 2011-06-15 | 重庆海巨农业发展有限公司 | Method for preparing radish red pigment homopolymer and radish proanthocyanidin from red-core radishes |
Non-Patent Citations (1)
| Title |
|---|
| 王淑杰等: "葡萄籽原花青素提取工艺研究", 《石油化工应用》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105754373A (en) * | 2016-03-09 | 2016-07-13 | 阿坝县天赐阳光生物科技有限公司 | Methods for processing vegetable pigments, vegetable beverages 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102718737B (en) | 2014-10-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102718737B (en) | Method of using roxburgh rose pulp to prepare roxburgh rose procyanidine | |
| CN101912480B (en) | Method for preparing procyanidin extract of lycium ruthenicum murr | |
| CN101486651B (en) | Method for extracting chlorogenic acid from Eucommia leaves and use thereof | |
| CN103265520B (en) | Method for preparing oligomeric proanthocyanidins and tannin pigment from grape seeds after winemaking | |
| CN103333067B (en) | A kind of extracting method of high-purity chlorogenic acid | |
| CN105669800B (en) | A kind of combined extracting essential oil from citrus, pectin, aurantiamarin, the method for synephrine and limonin | |
| CN106220693B (en) | A method of extracting multiple-ear rock Ke phloridzin | |
| CN101053589B (en) | Method for extracting active constituent from Tibetan capillary | |
| CN105111177B (en) | Method for extracting procyanidine from peony hulls | |
| CN103494862B (en) | Method for extracting olive polyphenol from olive processing waste liquor | |
| CN103431327A (en) | Lycium ruthenicum tablets and production method thereof | |
| CN101838343A (en) | Method for preparing pectin by using waste sisal dregs | |
| CN104187456A (en) | Technical method for extracting dietary fiber from pear residue | |
| CN102093748B (en) | Method for preparing radish red pigment homopolymer and radish proanthocyanidin from red-core radishes | |
| CN102250195A (en) | Method for producing xanthoceraside | |
| CN107325138A (en) | A kind of method of the main anthocyanin of four kinds of extraction separation and purification in pomace from blackcurrant | |
| CN104557838A (en) | Method for extracting proantho cyanidins from litchi peels | |
| CN101828750B (en) | Method for extracting natural preservative from bamboo leaves | |
| CN103012544B (en) | A kind of method extracting saponin and polysaccharide from tea seed grouts | |
| CN102633764A (en) | Production process for preparing anthocyanin and pectin by black soya bean hull | |
| CN105061631A (en) | Extraction method and application of taraxacum polysaccharide | |
| CN102675910A (en) | Preparation method of high-color-value beet root red color | |
| CN102127048A (en) | Method for preparing tea polyphenol and theanine from summer and autumn green tea | |
| CN101759731B (en) | Extraction method of linseed gum and secoisolariciresin-ol diglucoside | |
| CN101433322B (en) | Functional food rich in anthocyanidin and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141008 Termination date: 20160531 |