CN102432582A - Preparation method of proanthocyanidin - Google Patents
Preparation method of proanthocyanidin Download PDFInfo
- Publication number
- CN102432582A CN102432582A CN2011104500582A CN201110450058A CN102432582A CN 102432582 A CN102432582 A CN 102432582A CN 2011104500582 A CN2011104500582 A CN 2011104500582A CN 201110450058 A CN201110450058 A CN 201110450058A CN 102432582 A CN102432582 A CN 102432582A
- Authority
- CN
- China
- Prior art keywords
- extraction
- pycnogenols
- extract
- preparation
- water
- 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.)
- Pending
Links
Images
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a preparation method of proanthocyanidin. In the method, grape seed, pine bark, purple potato or any other plant with high proanthocyanidin content is used as a raw material, an ethanol aqueous solution is used as an extraction solvent, and a double water phase extraction method is utilized to efficiently prepare proanthocyanidin from a crude proanthocyanidin extract. The invention has the advantages of high product yield, high product purity, low solvent consumption, low cost and the like, and can easily implement industrial production.
Description
Technical field
The invention belongs to the biological extraction technical field, relate to a kind of preparation method of pycnogenols.
Background technology
Pycnogenols, English name are Oligomeric Proantho Cyanidins (OPC), are a kind of Vitamin P complexs that special molecular structure is arranged, and are the most effective natural antioxidantss of radical in the removing human body of generally acknowledging in the world at present.Be generally the reddish-brown powder, little, the puckery of gas, water-soluble and most organic solvent.Be generally Semen Vitis viniferae extract, French maritime pine bark extract or purple extract potato etc.Pycnogenols is a kind of new and effective inhibitor, and the free-radical scavengers of imitating the most by force that is so far to be found has very strong activity in vivo.The Green Tea Extract oxidation capacity that experiment showed, OPC is 50 times of vitamin E, ascorbic 20 times, and absorb rapidly fully.Pycnogenols all is widely used in fields such as healthcare products and makeup.Through retrieval, the extraction preparation method of pycnogenols takes passages as follows:
One Chinese patent application number: 201110126763.7 titles: a kind of extraction process of extracting pycnogenols from pinecone shell; The present invention relates to a kind of extraction process of extracting pycnogenols from pinecone shell; Belong to food technology field; Its extraction process is: pulverize, pinecone shell is through being crushed to the 40-60 order, and is subsequent use; Pinecone shell powder is got in degreasing, adds 8-12 and doubly measures the sherwood oil immersion more than 24 hours, and supersound process was filtered more than 25 minutes, got degreasing pinecone shell powder, and is subsequent use; Extract, in fat pinecone shell powder and 1: 20 ratio of 40% alcoholic acid solid-to-liquid ratio, soak more than 24 hours, ultrasonic oscillation extraction 1 hour filters, and being evaporated to does not have the alcohol flavor, and the adding distil water dilution is subsequent use; Purifying with macroporous resin column on the extracting solution, is placed more than 24 hours, and with the washing of 2BV/h flow velocity, washing is resolved with ethanol 4-6BV, and the effluent concentrating under reduced pressure reclaims ethanol, 60-80 ℃ of vacuum-drying, finished product.Beneficial effect is: for pycnogenols production provides a kind of wide material sources, quantity abundant renewable green resource.
One Chinese patent application number: the preparation method of 201110091574.0 1 kinds of rose Root of Kirilow Rhodiola pycnogenolss the present invention relates to a kind of preparation method of rose Root of Kirilow Rhodiola pycnogenols; This method is a raw material with rose Root of Kirilow Rhodiola rhizome; Earlier with its pulverizing, sieve; With 50% alcohol reflux 2 hours, the first extract of pycnogenols; Again this first extract is carried out removal of impurities, high concentration ethanol removes glucide, and sherwood oil removes the lipid material; Use ethyl acetate extraction then, separate height and gather pycnogenols and oligomeric procyanidolics; At last again with macroporous adsorbent resin to height gather, oligomeric procyanidolics carries out purifying, high purity of gathering pycnogenols reaches 95.0% after the lyophilize, oligomeric procyanidolics purity reaches 88.3%.This method technology is simple, pollution-free, is easy to suitability for industrialized production; The pycnogenols purity that obtains is high, the Medicines and Health Product raw material that can be applicable to the natural pigment foodstuff additive and have antioxygenation.
One Chinese patent application number: the method for oligomeric procyanidolics in 201110031451.8 1 kinds of extraction separation pinus yunnanensis barks, earlier with raw materials pretreatment, with fresh pinus yunnanensis bark; Sort out uncontaminated part, dry in indoor, the control raw material moisture is 8～10%; Pulverize, cross 20 mesh sieves; Extract again,, press solid-liquid ratio 1: 2～10 add to extract solvents, extract or microwave extraction 1～4 time in boiling condition refluxed with pretreated raw material; To extract solution and merge, suction filtration, filtrating is condensed into medicinal extract; Separate at last; To extract the water dissolution medicinal extract of 3～6 times of weight of raw material, to filter, filtrating is with chloroform extraction degreasing 2 times; The volume ratio of chloroform and medicinal extract water dissolution solution is 1: 3; Water layer after the degreasing adds sodium-chlor to saturated, uses ethyl acetate extraction again 3 times, and the volume ratio of ETHYLE ACETATE and saturation water is 1: 1; Is to remove under 0.02～0.08MPa condition to desolvate with extraction liquid at 70 ± 2 ℃, pressure, concentrates and promptly gets oligomeric procyanidolics.The inventive method technological process is simple, equipment is simple, raw material is easy to get, easy to utilize.
One Chinese patent application number: the process for extracting of anthocyanogen and pycnogenols constituents the invention discloses the process for extracting of anthocyanogen and pycnogenols constituents in a kind of bogberry fruit in the 201010503367.7 bogberry fruits; May further comprise the steps: earlier with bogberry fruit break process; Behind the enzyme enzymolysis; Under pH value 1.0～5.5 conditions, carry out flooding, get aqueous extract and residue; Again residue is carried out the alcohol extracting extraction, concentrated extract reclaims alcohol, gets the alcohol extracting liquid concentrator; Aqueous extract and alcohol extracting liquid concentrator are merged,, with the water washing macroporous adsorbent resin after, resolve with aqueous alcohol solutions through absorption with macroporous adsorbent resin, desorbed solution is concentrated, dry, must contain the mixture of anthocyanogen and pycnogenols constituents; Method technology of the present invention is simple, Device-General is strong, less investment, yield is high, cost is low, be suitable for large-scale production; The gained mixture can be used as the raw material of food, skin care products, pharmaceutical preparations or uses as additive.
One Chinese patent application number: 201010525734.3 black fruit lyceum pycnogenols products and preparation method thereof the present invention relates to a kind of black fruit lyceum pycnogenols product; This product is a raw material with the black fruit lyceum fresh fruit, and the oligomeric procyanidolics content that after separation and purification, obtains is 40%～70%, the high polymer procyanidin content is 10%～35%, other impurity is 10%～40% lilac red powder-product.The invention also discloses the preparation method of this product simultaneously.The present invention adopts membrane separation technique, and method is simple, fast, has not only avoided the use of virose organic reagent, and the product property homogeneous that obtains, stable and reduced production cost effectively can be used the Medicines and Health Product raw material with antioxygenation.
One Chinese patent application number: 201010188041.X extracts pycnogenols from wine mud method the invention discloses a kind of method of from wine mud, extracting pycnogenols; Comprise following content: the concentration that in wine mud, adds 1～2 times of volume is 80%～90% ethanolic soln stirring extraction; Redeposition separates and the collection extracting solution; Respectively with gauze and filter paper filtering extracting solution and collection filtrating; The heating evaporation of will filtrating reclaims ethanol, and last heating evaporation drying is removed moisture and obtained grape pycnogenols product.Method of the present invention is used for extracting pycnogenols from wine mud; Can the grape pycnogenols of discarding in the wine mud be extracted; Turn waste into wealth; For the production of grape pycnogenols provides a kind of new raw material sources, and can overcome the defective that the solvent usage quantity is big, extraction time is long, production cost is high that present process for extracting exists.
One Chinese patent application number: the process for extracting of 200910048064.8 1 kinds of oligomeric procyanidolics the invention discloses a kind of method of extracting oligomeric procyanidolics; It comprises the steps: the plant material that contains oligomeric procyanidolics with macroporous adsorptive resins on the crude extract of solvent extraction gained; Remove protein and polyose impurity with water elution; Carry out gradient elution with one or more and water in the following organic solvent as eluent more afterwards: ethanol, methyl alcohol and acetone; Collection is that the upper solution behind 4: 1: 5 the mixing solutions standing demix of propyl carbinol, acetic acid and water is a developping agent with volume ratio; The Rf value is 0.2～0.5 wash-out part on the silica gel thin-layer chromatography plate, promptly gets the oligomeric procyanidolics extract.Than prior art, method purity of the present invention and yield all are significantly increased, and the oligomeric procyanidolics yield can reach more than 80%, product purity >=50%, and basically all more than 80%, and this method technology is easy, and cost is low, is easy to industrialization.
One Chinese patent application number: 201010125513.7 1 kinds of method the present invention that from Semen Vitis viniferae, extract pycnogenolss provide a kind of method of from Semen Vitis viniferae, extracting pycnogenols, and material is put into extractor, and extracting solvent is water or aqueous ethanol; Consumption is 3～10 times of volume quality of material; Temperature is 45～100 ℃, and the time is 20～60 minutes, through successively each jar being extracted; Make that the active constituent content of extracting solution successively decreases successively in each jar; Again the extracting solution that active constituent content is the highest in each jar is carried out discharge opeing, get into the extractor that behind the circulation step material that carries out repeatedly solvent extraction is belonged to and carry out deslagging and add material, novel solvent adds when material extracts for the last time; Move at a distance from a unit afterwards, carry out multiple extraction back discharge opeing.The present invention guarantees that the material of each extraction unit and solvent remain bigger effective constituent concentration difference; Can accelerate extraction rate; Improve the concentration of final solvent effective constituent, under the prerequisite that guarantees higher extraction yield, have characteristics such as the solvent of saving, save energy.
One Chinese patent application number: the preparation method of 201010103007.8 1 kinds of grape pip procyanidins the invention discloses a kind of preparation method of grape pip procyanidin; It comprises following content: earlier use temperature to be 85-95 ℃ the aqueous solution lixiviate Semen Vitis viniferae, filter and obtain grape pip procyanidin crude extract solution; Again crude extract solution heating evaporation is concentrated, add the dissolve with ethanol pycnogenols in the liquid concentrator and remove throw out, obtain grape pip procyanidin extraction using alcohol solution; Then ethanol extract is carried out fractionation by adsorption through column chromatography, use the aqueous ethanolic solution wash-out of 30%-40% again, collect elutriant, dry back obtains the Procyanidcic Oligomers product.Solvent load and extraction cost can be raised the efficiency, reduced to this method.
One Chinese patent application number: what 200910035924.4 1 kinds of methods of from raspberry, extracting pycnogenolss the present invention relates to is a kind of method of from the raw material raspberry, extracting pycnogenols; It is characterized in that it is extraction agent that this method adopts ethanol; Extraction process is included under the normal pressure; The control alcohol concn, extract temperature, solid-liquid ratio, extraction time four conditions, extracting solution through filter, refining purifying, concentrate, drying obtains finished product, refining purifying adopts macroporous adsorbent resin.
Advantage of the present invention: procyanidin content is high in the raspberry; And adopt the efficient of extraction method high, can obviously improve the solubility rate of pycnogenols, and keep original structure and activity; Avoided the chemical synthesis by product many; Particularly the isomer of product is difficult to separate, and causes product purity not high, thereby it has application widely in fields such as food, medicines.Cost of the present invention is low, extraction efficiency is high, can obviously improve the solubility rate of pycnogenols, and keeps original structure and activity, and technology is simple, efficient, quick, the discharging of waste liquid amount is few.
One Chinese patent application number: the preparation method of 201010241351.3 1 kinds of procyanidin extract of lycium ruthenicum murr the present invention relates to a kind of preparation method of procyanidin extract of lycium ruthenicum murr; This method is a raw material with black fruit lyceum juice or black fruit lyceum liquid concentrator; After nonpolar macroporous adsorption resin separates; Be eluted to sugar-free with deionized water, use hydrochloric acid-ethanolic soln wash-out again, obtain containing the elutriant of pycnogenols; The elutriant that will contain pycnogenols then concentrates or after nf membrane concentrates, obtains the pycnogenols liquid concentrator through vacuum decompression; At last with liquid concentrator after the spray-dried or lyophilize, can obtain procyanidin content >=50%, total polyphenols content >=50%, anthocyanin content >=1% procyanidin extract of lycium ruthenicum murr.The present invention adopts membrane separation technique set column chromatography for separation technology; Not only effectively reduce production cost; Shortened the time of extraction separation; Reduced the energy consumption in the technological process, and products obtained therefrom purity is high, stable performance, the Medicines and Health Product raw material that can be applicable to the natural pigment foodstuff additive and have antioxygenation.
Lee antelope, Yang Xueying, high clouds etc. utilize propyl alcohol-ammonium sulfate double-aqueous phase system and ultrasonic coupled method that anti-oxidation active substance in the Semen Vitis viniferae is carried out extraction separation.The result shows that this method can be extracted anti-oxidation active substance effectively from Semen Vitis viniferae, and extract has good antioxidant activity; Extract is respectively 75.0% and 92.0% to the clearance rate of illumination vitamin G ultra-oxygen anion free radical and Fenton reaction hydroxy radical qiao, is 74.5% to the inhibiting rate of Yelkin TTS MDA.The anti-oxidant activity of this method extract is higher than the anti-oxidant activity of ethanol, ethyl acetate backflow extraction method extract.This method is easy and simple to handle, mild condition, environmental friendliness.
The extraction of proanthocyanidin in the Semen Vitis viniferae of king's equality, purifying and analytical procedure research; The effects the many influence factors in extraction, purifying and the process for refining process; Confirmed optimum process condition: the aqueous acetone solution with 60% is a digestion agent; Solid-liquid ratio is 1: 10, and 40 ℃ were extracted 24 hours down.Add NaCl to digestion agent and make its phase-splitting, first the double water-phase technology is applied in the purge process of proanthocyanidin.Acetone phase vat liquor is used the different concentration ethanol eluant solution after resin absorption, elutriant obtains final product again behind ethyl acetate extraction, and the extraction yield of proanthocyanidin is 0.59%, and product purity is 98%.
At present, the commercially available prod of pycnogenols is many extracts from Semen Vitis viniferae, Cortex Pini or purple potato the inside, and used method is the macroporous resin adsorption elution method, and the subject matter that Amberlyst process exists is, needs the time long, handles that material quantity is beneath, product purity is low.A macroporous resin column; Each medicinal extract sample size of handling is merely 5% of adsorption stuffing; And the content of target substance is 0.1～10% in the medicinal extract; Even the thick product production that obtains after the lower process separation is seldom, the macroporous resin column of one ton of filler of a filling, and a flow process only can be produced several kilograms thick product.A flow process comprises medicinal extract dissolving written treaty 5% aqueous solution, is added to chromatography and lives in, and needs ten several hours; Washing needs ten several hours to the dissociant flush away that is not adsorbed again then; Carry out the wash-out first time with a certain proportion of water-etoh solvent then, remove non-active substance, need tens of hours; Elute the active substance position with another kind of solvent system tens of hours consuming time again afterwards again.Use neat solvent ethanol elution pillar at last, the flush away alkaline soluble materials.If the pillar pollution level is lighter, after ethanol was washed, water was replaced ethanol, can carry out separation next time.If pillar is seriously polluted, after alcohol is washed, washed, also to carry out the alkaline solution washing, washing is to neutral then; Again with acid solution washing, and then water is washed till neutrality, and regenerative process just is accomplished.From throwing the solution upper prop, wash pillar regeneration, whole requirements of process 4 days even longer time fully up to component.The double water-phase method has report, but the technology prematurity is breadboard preparation method, can't carry out large-scale industrial production.
Summary of the invention
It is little to the objective of the invention is to improve in the prior art pycnogenols raw material treatment capacity, in the impurity elimination purge process treatment time long, technical process is long; Difficulty is carried out operate continuously; Separating effect is undesirable, and the technical problem of difficult suitability for industrialized production provides a kind of preparation method of pycnogenols.
Technical scheme of the present invention is: with the liquid-phase extraction system that water extraction pycnogenols crude extract adopts aqueous ethanolic solution-water-soluble height to gather organic solvent-slightly water-soluble organic solvent, sepn process is lived separation circuit without chromatography, separates and all in liquid phase, carries out.Separation and purification from general extractive, drying obtain high purity raw cyanidin(e) product.
The present invention is achieved in that
The preparation method of pycnogenols is to adopt aqueous ethanolic solution extraction+liquid-liquid extraction method with pycnogenols crude extract separation purification method, and the pycnogenols aqueous ethanolic solution is concentrated extract and forms double-aqueous phase system with water-soluble organic polymer solvent ratios; Extract concentrated solution is distributed in double-aqueous phase system; Making it to reach in two mean concnss in mutually is 30～50% partition equilibrium, uses then with the immiscible extraction agent of two waters to extract, and tells extraction liquid; Earlier remove the impurity of polarity less than pycnogenols; Remaining double water-phase extracts with another fat-soluble extraction agent again, and after drying obtains the pycnogenols product, and its operational process of craft is:
1, pre-treatment: will contain the pycnogenols raw material through removal of impurities, coarse breaking or the section of cutting back are subsequent use.
2, extract: pretreated pycnogenols raw material is added in the extraction equipment, add 70% ethanolic soln in raw material and 1: 3 ratio of extracting solution, heat tracing extracts three times, and controlled temperature is 60～70 ℃, and soaking time is 0.5～1.5h, united extraction liquid.
3, extraction: extracting solution is added in the extraction equipment, add a certain amount of ethanol or water, regulating alcoholic acid content is 30%～40%, and adds water-soluble organic polymer, stirs, and leaves standstill 0.5～1.5h and forms two phases, obtains the phase extraction liquid; In last phase extraction liquid, add the extraction of liposoluble extraction agent, separating and extracting liquid, and organic solvent is reclaimed in distillation.
4, drying: vacuum-drying, controlled temperature are below 60 ℃, and vacuum tightness is 0.08 >=MPa, obtain high purity raw cyanidin(e) product.
Above-described liquid-liquid extraction method is the three phase extraction system of aqueous ethanolic solution-water-soluble organic polymer solvent-slightly water-soluble organic solvent.
Above-described raw material is that Semen Vitis viniferae, Cortex Pini or purple potato etc. contain the higher plant of pycnogenols.
Above-described shipwreck is dissolved extraction agent, comprises one or more mixtures in sherwood oil, ETHYLE ACETATE, the butanols, and add-on is 1～1.5 times of raw-material weight.
Above-described water-soluble organic polymer extraction agent; Comprise the methyl W 166; Polyoxyethylene glycol; Volpo S 10, one or more mixtures in Vinylpyrrolidone polymer, hydroxypropyl VISOSE, methylcellulose gum, VISOSE, ROHM, SEPIGEL 305 and ROHM and the verivate thereof, add-on be extracting solution weight 2～4%.
Above-described stirring is for centrifugal phase-splitting is evenly stirred.
Above-described extraction equipment, thickening equipment and extraction equipment comprise one or more equipment in retort, reaction kettle and the reactor that adopts stainless steel, enamel and duraluminum making.
Characteristics of the present invention are:
The preparation method of pycnogenols of the present invention; It is aqueous ethanolic solution-water-soluble organic polymer solvent-slightly water-soluble organic solvent three phase extraction method; Optionally directly enrichment and separation and purification obtain the pycnogenols head product; Sepn process is lived separation circuit without chromatography, separates and all in liquid phase, carries out.The pycnogenols head product is through concentrating, obtaining 98% high-purity pycnogenols after the crystallization.This method is compared with traditional macroporous adsorption resin chromatography method in the past, and it is big to have treatment capacity, and technical process is short; Can carry out operate continuously, advantage that separation efficiency is high; Its production efficiency is 3～10 times of traditional method, and is homogeneous system, is easy to the continuous production operation.
Description of drawings
Fig. 1 is a process flow diagram of the present invention;
Specific embodiments
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Embodiment one:
To add through pycnogenols raw material 5 weight parts of removal of impurities, coarse breaking or the section of cutting in the stainless steel reaction jar; Add in raw material and 1: 3 weight part ratio of 70% ethanol, heat tracing extracts three times, and controlled temperature is 50～60 ℃; Soaking time is 1.2h, united extraction liquid.Extracting solution is added in the stainless steel cauldron, add extracting solution 2% ROHM and water or ethanol, adjusting alcoholic acid content is 30～40% ethanol of solution; Stir, leave standstill 1.5h and form two phases, obtain the phase extraction liquid; Add shipwreck dissolve with water-soluble two-phase extraction agent ethyl acetate-sherwood oil 4 weight parts (5: 1, v/v) extraction, separating and extracting liquid; And distillating filtering liquid reclaims organic solvent; Last controlled temperature is below 60 ℃, and vacuum tightness is to carry out vacuum-drying more than the 0.08Mpa, obtains high purity raw cyanidin(e) product.
Product pycnogenols yield is 0.58%, and it is 98.3% that product uses high effective liquid chromatography for measuring purity.
Embodiment two:
To add through pycnogenols raw material 5 weight parts of removal of impurities, coarse breaking or the section of cutting in the stainless steel reaction jar; Add in raw material and 1: 3 weight part ratio of 70% ethanol, heat tracing extracts three times, and controlled temperature is 50～60 ℃; Soaking time is 1.2h, united extraction liquid.The medicinal extract of extracting solution is added in the enamel reaction still again, add extracting solution 3% methyl W 166 and water or ethanol, adjusting alcoholic acid content is 30～40% ethanol of solution; Stir, leave standstill 1h and form two phases, obtain the phase extraction liquid; Add shipwreck dissolve with water-soluble two-phase extraction agent ethyl acetate-sherwood oil 4 weight parts (5: 1, v/v) extraction, separating and extracting liquid; Distillating filtering liquid reclaims organic solvent; Last controlled temperature is below 60 ℃, and vacuum tightness is to carry out vacuum-drying more than the 0.08Mpa, obtains high purity raw cyanidin(e) product.
Product chlorogenicacid yield is 0.53%, and it is 98.1% that product uses high effective liquid chromatography for measuring purity.
Claims (7)
1. the preparation method of a pycnogenols; It is characterized in that: adopt aqueous ethanolic solution extraction+liquid-liquid extraction method pycnogenols crude extract separation purification method; The pycnogenols aqueous ethanolic solution is concentrated extract and with water-soluble organic polymer solvent ratios composition double-aqueous phase system, extract concentrated solution distributed in double-aqueous phase system, and making it to reach in two mean concnss in mutually is 30～50% partition equilibrium; Use then with the immiscible extraction agent of two waters and extract; Tell extraction liquid, remove the impurity of polarity less than pycnogenols earlier, remaining double water-phase extracts with another fat-soluble extraction agent again; After drying obtains the pycnogenols product, and its operational process of craft is:
(1) pre-treatment: will contain the pycnogenols raw material through removal of impurities, coarse breaking or the section of cutting back are subsequent use.；
(2) extract: pretreated pycnogenols raw material is added in the extraction equipment, add 70% ethanolic soln in raw material and 1: 3 ratio of extracting solution, heat tracing extracts three times, and controlled temperature is 60～70 ℃, and soaking time is 0.5～1.5h, united extraction liquid.
(3) extraction: extracting solution is added in the extraction equipment, add a certain amount of ethanol or water, regulating alcoholic acid content is 30%～40%; And add water-soluble organic polymer; Stir, leave standstill 0.5～1.5h and form two phases, obtain the phase extraction liquid: in last phase extraction liquid, add the extraction of liposoluble extraction agent; Separating and extracting liquid, and organic solvent is reclaimed in distillation;
(4) drying: vacuum-drying, controlled temperature are below 60 ℃, and vacuum tightness is 0.08 >=MPa, obtain high purity raw cyanidin(e) product.
2. the preparation method of pycnogenols according to claim 1 is characterized in that: the three phase extraction system of aqueous ethanolic solution-water-soluble organic polymer solvent-slightly water-soluble organic solvent.
3. according to the preparation method of the said pycnogenols of claim 1, it is characterized in that: described raw material comprises that Semen Vitis viniferae, Cortex Pini and purple potato etc. contain the plant of pycnogenols.
4. according to the preparation method of the said pycnogenols of claim 1, it is characterized in that: described shipwreck is dissolved extraction agent, comprises one or more mixtures in sherwood oil, ETHYLE ACETATE, the butanols, and add-on is 1～1.5 times of weight of raw material.
5. according to the preparation method of the said pycnogenols of claim 1; It is characterized in that: described water-soluble organic polymer extraction agent; Comprise the methyl W 166, polyoxyethylene glycol, Volpo S 10; One or more mixtures in Vinylpyrrolidone polymer, hydroxypropyl VISOSE, methylcellulose gum, VISOSE, ROHM, SEPIGEL 305 and ROHM and the verivate thereof, add-on are 2～4% of extracting solution weight.
6. according to the preparation method of the said pycnogenols of claim 1, it is characterized in that: described stirring, for centrifugal phase-splitting is evenly stirred.
7. according to the preparation method of the said pycnogenols of claim 1; It is characterized in that: described extraction equipment, thickening equipment and extraction equipment comprise one or more equipment in retort, reaction kettle and the reactor that adopts stainless steel, enamel and duraluminum making.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104500582A CN102432582A (en) | 2011-12-29 | 2011-12-29 | Preparation method of proanthocyanidin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104500582A CN102432582A (en) | 2011-12-29 | 2011-12-29 | Preparation method of proanthocyanidin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102432582A true CN102432582A (en) | 2012-05-02 |
Family
ID=45980972
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104500582A Pending CN102432582A (en) | 2011-12-29 | 2011-12-29 | Preparation method of proanthocyanidin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102432582A (en) |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420969A (en) * | 2013-08-05 | 2013-12-04 | 江苏大学 | Method for extracting anthocyanidin in grape juice |
| CN103472056A (en) * | 2013-09-23 | 2013-12-25 | 集美大学 | Method for determining vitamin in fruits and vegetables by purple sweet potato anthocyanin and preparation method of purple sweet potato anthocyanin |
| CN103919879A (en) * | 2014-04-17 | 2014-07-16 | 陕西师范大学 | Preparation method of health products containing procyanidin and chlorogenic acid from apricot kernel skin |
| CN104341473A (en) * | 2014-09-25 | 2015-02-11 | 齐鲁工业大学 | Method for separating and enriching peony anthocyanin by using double-water-phase system |
| CN104787835A (en) * | 2015-04-29 | 2015-07-22 | 利穗科技(苏州)有限公司 | Method for extracting cefixime refined product in industrial waste liquor by utilizing chromatographic technique |
| CN104803960A (en) * | 2015-02-27 | 2015-07-29 | 云南民族大学 | Method for extracting and separating procyanidine of hawthorn fruit through low-temperature aqueous two phase cooling |
| CN104922220A (en) * | 2015-04-30 | 2015-09-23 | 西华大学 | Method for extracting Olea europaea leaf polyphenol by aqueous two phase system |
| CN105418573A (en) * | 2015-11-13 | 2016-03-23 | 大兴安岭林格贝寒带生物科技股份有限公司 | Industrialization method for extracting purple sweet potato anthocyanin from purple sweet potatoes |
| CN106749148A (en) * | 2016-11-25 | 2017-05-31 | 哈尔滨工业大学（威海） | A kind of method that OPC is extracted from hops |
| CN106755162A (en) * | 2016-12-01 | 2017-05-31 | 新疆海瑞盛生物工程股份有限公司 | A kind of method that enzyme process prepares fat-soluble grape pip procyanidin |
| CN107586286A (en) * | 2016-07-08 | 2018-01-16 | 罗红萍 | A kind of method that anthocyanidin is extracted from lycium ruthenicum |
| CN107739359A (en) * | 2017-11-30 | 2018-02-27 | 天津农学院 | A kind of method using double-aqueous phase system extracting procyanidins |
| CN111175399A (en) * | 2020-01-10 | 2020-05-19 | 西宁海关技术中心 | Method for detecting lycium ruthenicum high performance liquid chromatography fingerprint |
| CN113279287A (en) * | 2021-05-08 | 2021-08-20 | 荆楚理工学院 | Preparation method of visual freshness label based on lycium ruthenicum anthocyanin |
| CN113951557A (en) * | 2021-11-11 | 2022-01-21 | 郑州轻工业大学 | Grape seed procyanidin micro powder and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5882520A (en) * | 1995-10-26 | 1999-03-16 | The University Of Montana | Use of arabinogalactan in aqueous two phase extractions |
| CN101531652A (en) * | 2009-04-17 | 2009-09-16 | 大连理工大学 | Novel method for extracting anthocyanin in bilberry by double water phases |
| CN101781279A (en) * | 2010-01-29 | 2010-07-21 | 青岛大学 | Preparation method of grape seed procyanidin |
| WO2012040473A2 (en) * | 2010-09-24 | 2012-03-29 | The Regents Of The University Of Michigan | Solution microarrays and uses thereof |
-
2011
- 2011-12-29 CN CN2011104500582A patent/CN102432582A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5882520A (en) * | 1995-10-26 | 1999-03-16 | The University Of Montana | Use of arabinogalactan in aqueous two phase extractions |
| CN101531652A (en) * | 2009-04-17 | 2009-09-16 | 大连理工大学 | Novel method for extracting anthocyanin in bilberry by double water phases |
| CN101781279A (en) * | 2010-01-29 | 2010-07-21 | 青岛大学 | Preparation method of grape seed procyanidin |
| WO2012040473A2 (en) * | 2010-09-24 | 2012-03-29 | The Regents Of The University Of Michigan | Solution microarrays and uses thereof |
Non-Patent Citations (2)
| Title |
|---|
| 吴敏: "双水相萃取技术在药物提取与分离中的应用", 《中成药》, vol. 28, no. 10, 31 October 2006 (2006-10-31), pages 1505 - 1508 * |
| 李羚等: "双水相分离与超声提取耦合法从葡萄籽中提取抗氧化活性物质研究", 《酿酒科技》, no. 05, 31 December 2008 (2008-12-31) * |
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420969A (en) * | 2013-08-05 | 2013-12-04 | 江苏大学 | Method for extracting anthocyanidin in grape juice |
| CN103472056B (en) * | 2013-09-23 | 2016-04-20 | 集美大学 | Purple sweet potato anthocyanin measures the method for fruits and vegetables vitamin and the preparation method of purple sweet potato anthocyanin |
| CN103472056A (en) * | 2013-09-23 | 2013-12-25 | 集美大学 | Method for determining vitamin in fruits and vegetables by purple sweet potato anthocyanin and preparation method of purple sweet potato anthocyanin |
| CN103919879A (en) * | 2014-04-17 | 2014-07-16 | 陕西师范大学 | Preparation method of health products containing procyanidin and chlorogenic acid from apricot kernel skin |
| CN103919879B (en) * | 2014-04-17 | 2015-11-18 | 陕西师范大学 | The preparation method of a kind of almond peel procyanidin and chlorogenic acid health product |
| CN104341473A (en) * | 2014-09-25 | 2015-02-11 | 齐鲁工业大学 | Method for separating and enriching peony anthocyanin by using double-water-phase system |
| CN104341473B (en) * | 2014-09-25 | 2017-06-06 | 齐鲁工业大学 | A kind of method of double-aqueous phase system separation and concentration tree peony anthocyanin |
| CN104803960B (en) * | 2015-02-27 | 2017-09-22 | 云南民族大学 | A kind of method that separation FRUCTUS CRATAEGI OPC is extracted in low temperature aqueous two-phase cooling |
| CN104803960A (en) * | 2015-02-27 | 2015-07-29 | 云南民族大学 | Method for extracting and separating procyanidine of hawthorn fruit through low-temperature aqueous two phase cooling |
| CN104787835B (en) * | 2015-04-29 | 2016-09-14 | 利穗科技(苏州)有限公司 | Chromatographic technique is utilized to extract the method for cefixime fine work in industrial wastes |
| CN104787835A (en) * | 2015-04-29 | 2015-07-22 | 利穗科技(苏州)有限公司 | Method for extracting cefixime refined product in industrial waste liquor by utilizing chromatographic technique |
| CN104922220A (en) * | 2015-04-30 | 2015-09-23 | 西华大学 | Method for extracting Olea europaea leaf polyphenol by aqueous two phase system |
| CN104922220B (en) * | 2015-04-30 | 2019-01-18 | 西华大学 | A kind of method of double-aqueous phase system extraction oil olive leaf polyphenol |
| CN105418573A (en) * | 2015-11-13 | 2016-03-23 | 大兴安岭林格贝寒带生物科技股份有限公司 | Industrialization method for extracting purple sweet potato anthocyanin from purple sweet potatoes |
| CN105418573B (en) * | 2015-11-13 | 2018-04-24 | 大兴安岭林格贝寒带生物科技股份有限公司 | The industrial method of purple sweet potato cyanidin is extracted from purple sweetpotato |
| CN107586286A (en) * | 2016-07-08 | 2018-01-16 | 罗红萍 | A kind of method that anthocyanidin is extracted from lycium ruthenicum |
| CN106749148A (en) * | 2016-11-25 | 2017-05-31 | 哈尔滨工业大学（威海） | A kind of method that OPC is extracted from hops |
| CN106755162A (en) * | 2016-12-01 | 2017-05-31 | 新疆海瑞盛生物工程股份有限公司 | A kind of method that enzyme process prepares fat-soluble grape pip procyanidin |
| CN107739359A (en) * | 2017-11-30 | 2018-02-27 | 天津农学院 | A kind of method using double-aqueous phase system extracting procyanidins |
| CN111175399A (en) * | 2020-01-10 | 2020-05-19 | 西宁海关技术中心 | Method for detecting lycium ruthenicum high performance liquid chromatography fingerprint |
| CN113279287A (en) * | 2021-05-08 | 2021-08-20 | 荆楚理工学院 | Preparation method of visual freshness label based on lycium ruthenicum anthocyanin |
| CN113951557A (en) * | 2021-11-11 | 2022-01-21 | 郑州轻工业大学 | Grape seed procyanidin micro powder and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102432582A (en) | Preparation method of proanthocyanidin | |
| CN101704867B (en) | Method for preparing naringin or hesperidin | |
| CN104710391B (en) | Method for extracting luteolin and beta-sitosterol from peanut shells | |
| CN102001947A (en) | Method for preparing honeysuckle chlorogenic acid | |
| CN102408320B (en) | Method for extracting and separating curcumin and curcuma oil from carcuma longa | |
| CN101463027B (en) | Method for extracting and separating flavone and anthocyanidin from elder fruit | |
| CN103463123A (en) | Method for extracting effective constituents from maca | |
| CN101774955A (en) | Method for preparing high-content trans-lutein crystals from dried marigold flower pellets | |
| CN104059947A (en) | Method for preparing high-purity sulforaphane | |
| CN106349324B (en) | The method of extraction separation crataegolic acid from olive growing leaves | |
| CN107325138A (en) | A kind of method of the main anthocyanin of four kinds of extraction separation and purification in pomace from blackcurrant | |
| CN100439319C (en) | Method for preparing salviol acid A | |
| CN101177648B (en) | Method for extracting grape seed oil and procyanidine from grape seeds by one-step process | |
| CN104292366A (en) | Method for simultaneously extracting arabinogalactan and dihydroquercetin from dahurian larch | |
| CN104000935B (en) | A kind of method that anti-oxidant phenolic acid is extracted in the slag from jacket | |
| CN105503981B (en) | The method that violet cabbage anthocyanidin is extracted from violet cabbage | |
| CN109021042B (en) | Method for extracting high-purity oleuropein from olive leaves | |
| CN104027367A (en) | Method for separating and purifying total polyphenol in redrlowered loropetalum by utilizing macroporous resin | |
| CN110922413A (en) | Extraction and separation method of glabridin | |
| CN105616477A (en) | Method for purifying polyphenol in lonicera edulis | |
| CN102432420B (en) | Method for extracting and separating beta-elemene from Lantana camara | |
| CN106397529B (en) | The method of extraction separation crataegolic acid from olive pomace | |
| CN102432419B (en) | Method for extracting and separating beta-elemene from Eupatorium adenophorum | |
| CN1456559A (en) | Method for extracting soybean isoflavone | |
| CN1281600C (en) | Method for extracting high purity seabuckthorn flavone aglycone |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120502 |