CN101550196A - Method for extracting pine seed polysaccharides of Korean pine - Google Patents
Method for extracting pine seed polysaccharides of Korean pine Download PDFInfo
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- CN101550196A CN101550196A CNA2009100719911A CN200910071991A CN101550196A CN 101550196 A CN101550196 A CN 101550196A CN A2009100719911 A CNA2009100719911 A CN A2009100719911A CN 200910071991 A CN200910071991 A CN 200910071991A CN 101550196 A CN101550196 A CN 101550196A
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- pine
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- korean pine
- seed polysaccharides
- polysaccharides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
A method for extracting pine seed polysaccharides of Korean pine relates to a method for preparing pine seed polysaccharides of Korean pine. The method of the invention settles the problems of low extraction rate, low activity and tedious production process in the traditional method for extracting pine seed polysaccharides of Korean pine. The method for extracting pine seed polysaccharides of Korean pine comprises the following steps: selecting pine seed of Korean pine, crushing, degreasing, extracting with a highfield, separating the raffinate with a supercentrifuge, eliminating the impurity, condensing with a vacuum scraper-type film, freeze-drying with a vacuum freeze-dryer for obtaining the freeze-dried powder of pine seed polysaccharides of Korean pine. The pine seed polysaccharides of Korean pine prepared according to the invention is a natural extract and has no side effect to the human body. The pine seed polysaccharides of Korean pine of the invention has the functions of reinforcing the immunologic function, anti-tumor function, reducing the blood fat, reducing the blood pressure, anticoagulant function, antithrombotic function, reducing fat, beautifying, protecting skin, etc. The pine seed polysaccharides of Korean pine can be applied for fields of food, health product, cosmetic, medicine, biochemical engineering, etc.
Description
Technical field
The present invention relates to a kind of pine seed polysaccharides of Korean pine preparation method.
Background technology
Pine seed polysaccharides of Korean pine is the sp act factor of Korean pine pinenut, has effects such as raise immunity, antitumor, reducing blood-fat, hypotensive, anticoagulation, antithrombotic, fat-reducing, beauty and skin care.Can be applicable to fields such as food, healthcare products, makeup, medicine, biochemical industry.
Pine seed polysaccharides of Korean pine can be widely used in food, medicine, healthcare products, cosmetics production at present, is the worldwide multifunctional product of fashionable America and Europe, Japan and Korea S., and its market outlook are boundless.Though it is at present a lot of to the research of pine seed polysaccharides of Korean pine, but the extracting method of pine seed polysaccharides of Korean pine is mainly based on supersonic method and reflux extraction method, with producing a large amount of free radicals in the supersonic method extraction pine seed polysaccharides of Korean pine process, destroy the pine seed polysaccharides of Korean pine physiologically active, and the reflux extraction method is a kind of high temperature abstraction technique, can make pine seed polysaccharides of Korean pine lose physiological function equally, and the extraction yield of two kinds of methods is relatively low.This invention proposes highfield extraction pine seed polysaccharides of Korean pine, has well kept activity, has very high nutritive value, can be used as the raw material of food, medicine, healthcare products, makeup.
Summary of the invention
Low in order to solve the pine seed polysaccharides of Korean pine extraction yield, active not high problem the invention provides the method that a kind of highfield legal system is equipped with pine seed polysaccharides of Korean pine, can effectively improve the extraction yield and the product activity of pine seed polysaccharides of Korean pine.Among the present invention, a kind of method for extracting pine seed polysaccharides of Korean pine, the step that it is characterized in that the method that pine seed polysaccharides of Korean pine extracts is as follows: one, the extraction of pine seed polysaccharides of Korean pine: carry out the screening of Korean pine pinenut earlier, choose pine nuts of Korean pine, the drying of plucking in fresh autumn, shell, pulverize, with supercritical carbon dioxide extraction equipment skimming treatment 60 minutes, pressure 30Mpa, 45 ℃ of temperature.The ratio that after the skimming treatment with the solid-liquid ratio is 1g: 25mL～1g: 40mL adds the Korean pine pinenut powder and the aqueous solution respectively, with highfield extraction 50～60 minutes, obtain containing the pine seed polysaccharides of Korean pine extraction liquid, carry out solid-liquid separation with the horizontal helical type whizzer with the speed of 1800～2000r/min at last, isolate extracting solution and residue, with residue is the ratio adding aqueous solution of 1g: 25mL～1g: 40mL again with the solid-liquid ratio, proceeding highfield extracts and centrifugation, extract 3 times continuously, remove residue, united extraction liquid.Two, concentrate: the pine seed polysaccharides of Korean pine extracting solution is adopted vacuum scraper-type thin film concentration, and concentrated condition is 45～55 ℃ of temperature, and vacuum tightness is 0.1～0.15mbar, obtains Korean pine pinenut Crude polysaccharides concentrated solution; Three, purifying: it is 20cm that Korean pine pinenut Crude polysaccharides concentrated solution is added diameter by fluid distributor, it highly is the high efficiency chromatography chromatography column of 250cm, sodium chloride solution wash-out with concentration, flow velocity is 100mL～250mL/h, get the pine seed polysaccharides of Korean pine elutriant, use vacuum scraper-type thin film concentration equipment dense again.Four, drying: being ground into 60 order pressed powders after with pine seed polysaccharides of Korean pine concentrated solution vacuum-freeze-dry under 0.4～0.7mbar, temperature-40～-50 ℃ condition, promptly get the pine seed polysaccharides of Korean pine lyophilized powder with the vacuum-freeze-dry machine.
Among the present invention, in method for extracting pine seed polysaccharides of Korean pine, adopt the highfield auxiliary extraction to cooperate the method for the centrifugal cycling extraction of horizontal helical type, make pine seed polysaccharides of Korean pine be able to abundant release, make the extraction yield of polysaccharide can reach 85～92%, than the extraction yield of ultrasonic extraction or solvent refluxing extraction method high respectively 10～20% and 15～20%.Its specific activity extraction method ultrasonic extraction or solvent refluxing extraction method height 20～30%, improved the added economic value of pine seed polysaccharides of Korean pine greatly.Technology of the present invention is simple, extraction yield height, suitable promotion and application.The pine seed polysaccharides of Korean pine of the present invention's preparation is active high, can be used as the raw material that can be used as food, medicine, healthcare products, makeup.
Embodiment
Embodiment one: in this embodiment, a kind of method for extracting pine seed polysaccharides of Korean pine, the step that it is characterized in that the method that pine seed polysaccharides of Korean pine extracts is as follows: one, the extraction of pine seed polysaccharides of Korean pine: carry out the screening of Korean pine pinenut earlier, choose pine nuts of Korean pine, the drying of plucking in fresh autumn, shell, pulverize, with supercritical carbon dioxide extraction equipment skimming treatment 60 minutes, pressure 30Mpa, 45 ℃ of temperature.The ratio that after the skimming treatment with the solid-liquid ratio is 1g: 25mL～1g: 40mL adds the Korean pine pinenut powder and the aqueous solution respectively, with highfield extraction 50～60 minutes, obtain containing the pine seed polysaccharides of Korean pine extraction liquid, carry out solid-liquid separation with the horizontal helical type whizzer with the speed of 1800～2000r/min at last, isolate extracting solution and residue, with residue is the ratio adding aqueous solution of 1g: 25mL～1g: 40mL again with the solid-liquid ratio, proceeding highfield extracts and centrifugation, extract 3 times continuously, remove residue, united extraction liquid.Two, concentrate: the pine seed polysaccharides of Korean pine extracting solution is adopted vacuum scraper-type thin film concentration, and concentrated condition is 45～55 ℃ of temperature, and vacuum tightness is 0.1～0.15mbar, obtains Korean pine pinenut Crude polysaccharides concentrated solution; Three, purifying: it is 20cm that Korean pine pinenut Crude polysaccharides concentrated solution is added diameter by fluid distributor, it highly is the high efficiency chromatography chromatography column of 250cm, sodium chloride solution wash-out with concentration, flow velocity is 100mL～250mL/h, get the pine seed polysaccharides of Korean pine elutriant, use vacuum scraper-type thin film concentration equipment dense again.Four, drying: being ground into 60 order pressed powders after with pine seed polysaccharides of Korean pine concentrated solution vacuum-freeze-dry under 0.4～0.7mbar, temperature-40～-50 ℃ condition, promptly get the pine seed polysaccharides of Korean pine lyophilized powder with the vacuum-freeze-dry machine.Be: its feature extracts strength of electric field in step 1 be 80～90 kilovolts, high-voltage electric field strokes per minute 600～800 times, pulse-repetition 350～500Hz.Other is identical with embodiment one.
Embodiment three: what this embodiment and embodiment one were different is: it is characterized in that in the step 2 that solid content is 60%～70% in the concentrated solution.Other is identical with embodiment one.
Embodiment four: what this embodiment and embodiment one were different is: it is characterized in that high efficiency chromatography chromatography column purifying in the step 3, used solid-phase media is the X-5 macroporous resin, and the moving phase medium is for being 1.0%～1.5% sodium-chlor wash-out with mass concentration.Other is identical with embodiment one.
Embodiment five: what this embodiment and embodiment one were different is: the vacuum-freeze-dry time is 24～36 hours in the step 3.
The extraction yield of pine seed polysaccharides of Korean pine is 85～90% in this embodiment, and purity is 75～80%, and the gained pine seed polysaccharides of Korean pine is active high, quality better.
Claims (4)
- A kind of method for extracting pine seed polysaccharides of Korean pine, the step that it is characterized in that the method that pine seed polysaccharides of Korean pine extracts is as follows: one, the extraction of pine seed polysaccharides of Korean pine: carry out the screening of Korean pine pinenut earlier, choose pine nuts of Korean pine, the drying of plucking in fresh autumn, shell, pulverize, with supercritical carbon dioxide extraction equipment skimming treatment 60 minutes, pressure 30Mpa, 45 ℃ of temperature.The ratio that after the skimming treatment with the solid-liquid ratio is 1g: 25mL～1g: 40mL adds the Korean pine pinenut powder and the aqueous solution respectively, with highfield extraction 50～60 minutes, obtain containing the pine seed polysaccharides of Korean pine extraction liquid, carry out solid-liquid separation with the horizontal helical type whizzer with the speed of 1800～2000r/min at last, isolate extracting solution and residue, with residue is the ratio adding aqueous solution of 1g: 25mL～1g: 40mL again with the solid-liquid ratio, proceeding highfield extracts and centrifugation, extract 3 times continuously, remove residue, united extraction liquid.Two, concentrate: the pine seed polysaccharides of Korean pine extracting solution is adopted vacuum scraper-type thin film concentration, and concentrated condition is 45～55 ℃ of temperature, and vacuum tightness is 0.1～0.15mbar, obtains Korean pine pinenut Crude polysaccharides concentrated solution; Three, purifying: it is 20cm that Korean pine pinenut Crude polysaccharides concentrated solution is added diameter by fluid distributor, it highly is the high efficiency chromatography chromatography column of 250cm, sodium chloride solution wash-out with concentration, flow velocity is 100mL～250mL/h, get the pine seed polysaccharides of Korean pine elutriant, use vacuum scraper-type thin film concentration equipment dense again.Four, drying: being ground into 60 order pressed powders after with pine seed polysaccharides of Korean pine concentrated solution vacuum-freeze-dry under 0.4～0.7mbar, temperature-40～-50 ℃ condition, promptly get the pine seed polysaccharides of Korean pine lyophilized powder with the vacuum-freeze-dry machine.1, a kind of method for extracting pine seed polysaccharides of Korean pine according to claim 1 is characterized in that extraction strength of electric field is 80～90 kilovolts every square centimeter in the step 1, high-voltage electric field strokes per minute 600～800 times, pulse-repetition 350～500Hz.
- 2, a kind of method for extracting pine seed polysaccharides of Korean pine according to claim 1 is characterized in that in the step 2 that solid content is 60%～70% in the concentrated solution.
- 3, a kind of method for extracting pine seed polysaccharides of Korean pine according to claim 1, it is characterized in that high efficiency chromatography chromatography column purifying in the step 3, used solid-phase media is the X-5 macroporous resin, and the moving phase medium is for being 1.0%～1.5% sodium-chlor wash-out with mass concentration.
- 4, a kind of method for extracting pine seed polysaccharides of Korean pine according to claim 1 is characterized in that the vacuum-freeze-dry time is 24～36 hours in the step 4.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100719911A CN101550196A (en) | 2009-05-11 | 2009-05-11 | Method for extracting pine seed polysaccharides of Korean pine |
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| CNA2009100719911A CN101550196A (en) | 2009-05-11 | 2009-05-11 | Method for extracting pine seed polysaccharides of Korean pine |
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| CNA2009100719911A Pending CN101550196A (en) | 2009-05-11 | 2009-05-11 | Method for extracting pine seed polysaccharides of Korean pine |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020721A (en) * | 2011-01-13 | 2011-04-20 | 哈尔滨工业大学 | Preparation method of polysaccharide in pine cone from Pinus koraiensis |
| CN104311693A (en) * | 2014-11-20 | 2015-01-28 | 四川旭华制药有限公司 | Method for extracting polysaccharose from folium eriobotryae through microwaves |
| CN104448025A (en) * | 2014-12-23 | 2015-03-25 | 哈尔滨工业大学 | Single polysaccharide component PKP-E-2-2 of pinecone of pinus koraiensis and preparation method of single polysaccharide component PKP-E-2-2 |
-
2009
- 2009-05-11 CN CNA2009100719911A patent/CN101550196A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020721A (en) * | 2011-01-13 | 2011-04-20 | 哈尔滨工业大学 | Preparation method of polysaccharide in pine cone from Pinus koraiensis |
| CN104311693A (en) * | 2014-11-20 | 2015-01-28 | 四川旭华制药有限公司 | Method for extracting polysaccharose from folium eriobotryae through microwaves |
| CN104448025A (en) * | 2014-12-23 | 2015-03-25 | 哈尔滨工业大学 | Single polysaccharide component PKP-E-2-2 of pinecone of pinus koraiensis and preparation method of single polysaccharide component PKP-E-2-2 |
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Application publication date: 20091007 |