CN101244119A - Method for extracting polyoses and active principle from cyclocarya paliurus - Google Patents
Method for extracting polyoses and active principle from cyclocarya paliurus Download PDFInfo
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- CN101244119A CN101244119A CNA2008100734724A CN200810073472A CN101244119A CN 101244119 A CN101244119 A CN 101244119A CN A2008100734724 A CNA2008100734724 A CN A2008100734724A CN 200810073472 A CN200810073472 A CN 200810073472A CN 101244119 A CN101244119 A CN 101244119A
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- cyclocarya paliurus
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- paliurus iljinskaja
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Abstract
The invention discloses a method for extracting polysaccharide and effective components from cyclocarya paliurus, which comprises the steps as follows: immersing cyclocarya paliurus leaves with hot water, filtering, the filtrate successively passing through two pieces of membrane under the pressure of 0.01 to 0.2MPa, separating the filtrate by the first membrane, concentrating the filtrate, precipitating by ethanol, obtaining big molecular polysaccharide by filtering precipitate; the leaky filtrate passing through the first going through the second membrane, concentrating the filtrate, precipitating with ethanol, obtaining big molecular polysaccharide and small molecular polysaccharide and processing the leaky filtrate to get organic molecules. The other technique of the invention comprises the steps as follows: reflux extracting cyclocarya paliurus with ethanol, concentrating and recycling ethanol, adsorption with macroporous resin after dilution, elution, concentrating and drying, then getting small organic molecular products. Treating the dregs after filtering as the steps of the first technique, the products of big molecular polysaccharide and small molecular polysaccharide can be obtained. The method for extracting polysaccharide and effective components from cyclocarya paliurus has the advantages of simple technology, ability to acquire a plurality of effective components, no pollution of solvent, recyclability, no wastewater and dregs, simple equipment and low investment.
Description
Technical field:
The present invention relates to the extracting method of effective ingredients in plant, specifically is the method for extracting polysaccharide and effective ingredient from Cyclocarya paliurus Iljinskaja.
Background technology:
Cyclocarya paliurus Iljinskaja [cyclocarya paliurus (Batal.) lljinsk] is Dicotyledoneae [Dicotyledneae] Juglandaceae [Juglangdaceae], is the rare distinctive a kind of tall and big magaphanerophytes of China.Cyclocarya paliurus Iljinskaja contains the polysaccharide material and the effective ingredient of abundant hypoglycemic activity, and it also contains trace element chromium, nickel, lithium, selenium and the vanadium with ILA, can participate in the carbohydrate metabolism of human body, can also improve the carbohydrate tolerance of diabetic mice.
At present, the Cyclocarya paliurus Iljinskaja extraction of effective components has caused extensive concern, Chinese patent application number is 87101852 to disclose a kind of " extracting method of Cyclocarya paliurus Iljinskaja sweetener ", Chinese patent application number is 02113548.7 to disclose a kind of " method of extraction separation multiple components from Cyclocarya paliurus Iljinskaja ", these methods all are to adopt different resin decolorization, remove impurity, effective ingredient such as absorption Cyclocarya paliurus Iljinskaja polysaccharide, the reuse organic solvent washes out, concentrate drying gets product, though can isolate the Cyclocarya paliurus Iljinskaja polysaccharide, different components such as Cyclocarya paliurus Iljinskaja flavone, but yield is low, product purity is not high, complex process, equipment investment is big, the product cost height; And need in the production process to use a large amount of bronsted lowry acids and bases bronsted lowries, and organic solvent such as aliphatic alcohol, a large amount of high concentrated organic wastewaters of generation need reinvestment to handle, otherwise with contaminated environment.
Summary of the invention:
The objective of the invention is for overcoming the deficiencies in the prior art, and a kind of yield height, purity height are disclosed, equipment is simple, cost is low, free from environmental pollution extracts the method for polysaccharide and effective ingredient from Cyclocarya paliurus Iljinskaja.
Processing step of the present invention is:
1, leaf of Cyclocarya paliurus Iljinskaja is pulverized, placed the lixiviate jar;
2, add entry, under 70 ℃ of temperature, soaked 3-5 hour;
3, above-mentioned soak is filtered the Cyclocarya paliurus Iljinskaja leachate, and temperature reduces to 20～35 ℃, pH value is 6-8, the leaf slag is discarded;
4, filtrate is sent into double membrane separation assemblies through compression pump order under 0.01～0.2Mpa operating pressure;
5, by the first heavy membrance separation spare, hold back and isolate spissated Cyclocarya paliurus Iljinskaja fiber, protein, pectin, polysaccharide, concentrate Cyclocarya paliurus Iljinskaja membrane filtration solution, get Cyclocarya paliurus Iljinskaja macromolecular substances concentrated solution, add ethanol again to containing alcohol amount 70-85%, leave standstill filtration, the centrifugalize precipitation gets the macromolecular polysaccharide product;
6, residual filtrate is by the second heavy membrance separation spare, hold back isolated Cyclocarya paliurus Iljinskaja Organic substance, micromolecular polysaccharide is sent from second outlet, through concentrating, add ethanol to containing alcohol amount 70-85% precipitation, leave standstill filtration, the centrifugalize precipitation, vacuum drying gets Cyclocarya paliurus Iljinskaja Organic substance product, micromolecular polysaccharide;
7, residual filtrate is discharged from solvent outlet.
Another kind of processing step of the present invention is:
1, leaf of Cyclocarya paliurus Iljinskaja is pulverized, placed the lixiviate jar;
2, the ethanol of adding 75%, heating and refluxing extraction;
3, said extracted liquid is filtered with 250 mesh filter screens;
4, filtrate concentrates, and reclaims ethanol;
5, behind the concentrated solution thin up, use macroporous resin adsorption;
6, the ethanol eluting, concentrate, drying obtains the organic molecule product;
7, the leaf slag after the filtration adds entry, under 70 ℃ of temperature, soaks 3-5 hour;
8, filter the Cyclocarya paliurus Iljinskaja leachate, and temperature reduces to 20～35 ℃, pH value is 6-8, the leaf slag is discarded;
9, filtrate is sent into double membrane separation assemblies through compression pump order under 0.01～0.2Mpa operating pressure;
10, by the first heavy film, hold back and isolate spissated Cyclocarya paliurus Iljinskaja fiber, protein, pectin, polysaccharide, concentrate the Cyclocarya paliurus Iljinskaja polysaccharide solution, get Cyclocarya paliurus Iljinskaja polysaccharide concentrated solution, add ethanol again, leave standstill filtration to containing alcohol amount 70-85%, the centrifugalize precipitation gets the macromolecular polysaccharide product;
11, residual filtrate is by the second heavy film, hold back isolated Cyclocarya paliurus Iljinskaja Organic substance, micromolecular polysaccharide is sent from second outlet, through concentrating, add ethanol to containing alcohol amount 70-85% precipitation, leave standstill filtration, the centrifugalize precipitation, vacuum drying, 70 ℃ of baking temperatures get Cyclocarya paliurus Iljinskaja Organic substance product, micromolecular polysaccharide;
12, residual filtrate is discharged from solvent outlet.
The water of described adding and leaf of Cyclocarya paliurus Iljinskaja weight part ratio are 10～15: 1; Described leachate weighs membrane separation assemblies by first through first order compression pump under 0.01～0.08Mpa operating pressure; First order residual filtrate weighs membrane separation assemblies by second through second level compression pump under 0.05～0.10Mpa operating pressure.
The baking temperature of described concentrated Cyclocarya paliurus Iljinskaja polyose≤75 ℃.
Described concentrated Cyclocarya paliurus Iljinskaja solution baking temperature is 50～70 ℃.
The invention has the advantages that:
1, separation, extraction and a concentrated step finish, and technology is simple, once can get multiple product, and can produce continuously;
2, yield height, the product purity height, the gained polyoses content reaches 50%;
3, the solvent of Shi Yonging is recyclable recycles, conservation, and cost descends greatly;
4, solvent for use is pollution-free, does not also produce any waste water and dregs that influences environment;
5, equipment is simple, invests low.
Description of drawings:
Fig. 1 is the process chart of the embodiment of the invention 1;
Fig. 2 is the process chart of the embodiment of the invention 2.
The specific embodiment:
The invention will be further described below in conjunction with specific embodiment, but be not the qualification to content of the present invention.
Embodiment 1
Get 1 kilogram of leaf of Cyclocarya paliurus Iljinskaja, pulverize, leaf fragment＜2cm adds 10 kg of water, heats to 70 ℃, keeps this temperature, soaks 5 hours, extracts 3 times; Filter with 250 mesh filter screens, get the Cyclocarya paliurus Iljinskaja leachate, discarded leaf slag can be used for making fertilizer etc.; The leachate pH value is 6, leachate is cooled to 25～30 ℃, through first order compression pump, under 0.02～0.05Mpa operating pressure, weigh ultrafilter membrane (molecular cut off is 10000) separation assembly by first, by the first heavy film, hold back and isolate spissated Cyclocarya paliurus Iljinskaja fiber, protein, pectin, polysaccharide etc. are sent from first outlet, concentrate the Cyclocarya paliurus Iljinskaja polysaccharide solution, get Cyclocarya paliurus Iljinskaja polysaccharide concentrated solution, add ethanol again to containing alcohol amount 70-85%, leave standstill, with 150-250 purpose strainer filtering precipitation, under 70 ℃, carry out vacuum drying, get macromolecular polysaccharide product (0.85%); Residual filtrate is sent into second heavy film (molecular cut off the is 1000) separation assembly through second level compression pump under 0.05～0.1Mpa operating pressure; By the second heavy film, hold back isolated Cyclocarya paliurus Iljinskaja Organic substance, micromolecular polysaccharide is sent from second outlet, through concentrating, add ethanol to containing alcohol amount 70-85% precipitation, leave standstill, with 150-250 purpose strainer filtering, centrifugation, vacuum drying, 70 ℃ of baking temperatures get Cyclocarya paliurus Iljinskaja Organic substance product, micromolecular polysaccharide (1.12%); Residual filtrate is discharged from solvent outlet, environment friendly and pollution-free processing.
Selected film is the film of relative molecular mass 10000.
Embodiment 2
Get 1 kilogram of leaf of Cyclocarya paliurus Iljinskaja, pulverize, add 75%EtOH, reflux 5 hours, filter with 250 mesh filter screens, get Cyclocarya paliurus Iljinskaja EtOH extracting solution, concentrated extracting solution reclaims EtOH, concentrated solution thin up, carry out macroporous resin adsorption then, eluting, ethanol eluting, concentrated, dry obtains the organic molecule product; After the leaf slag is removed ethanol, add 10 kilograms in water, heat, keep this temperature, soaked 5 hours, extract 3 times to 70 ℃.Filter with 250 mesh filter screens, get Cyclocarya paliurus Iljinskaja polysaccharide leachate, discarded leaf slag can be used for composting etc.The leachate pH value is 6, leachate is cooled to 25～30 ℃, through first order compression pump, under 0.02～0.05Mpa operating pressure, weigh ultrafilter membrane (molecular cut off is 10000) separation assembly by first, by the first heavy film, hold back and isolate spissated Cyclocarya paliurus Iljinskaja fiber, protein, pectin, polysaccharide, send from first outlet, concentrate the Cyclocarya paliurus Iljinskaja polysaccharide solution, get Cyclocarya paliurus Iljinskaja polysaccharide concentrated solution, add ethanol again to containing alcohol amount 70-85%, leave standstill, with 150-250 purpose strainer filtering precipitation, under 70 ℃, carry out vacuum drying, get polyose (0.92%).Residual filtrate weighs film (molecular cut off be 1000) separation assembly by second through second level compression pump under 0.05～0.08Mpa operating pressure, hold back and isolate Cyclocarya paliurus Iljinskaja water soluble organic substance, micromolecular polysaccharide, through concentrating, add ethanol to containing alcohol amount 70-85% precipitation, leave standstill, precipitate with 150-250 purpose strainer filtering, vacuum drying, 70 ℃ of baking temperatures get Cyclocarya paliurus Iljinskaja Organic substance product, micromolecular polysaccharide (0.96%).Residual filtrate is discharged from solvent outlet, environment friendly and pollution-free processing.
Claims (6)
1, extracts the method for polysaccharide and effective ingredient from Cyclocarya paliurus Iljinskaja, comprise the steps:
(1) leaf of Cyclocarya paliurus Iljinskaja is pulverized, placed the lixiviate jar;
(2) add entry, under 70 ℃ of temperature, soaked 3-5 hour;
(3) filter the Cyclocarya paliurus Iljinskaja leachate, and temperature reduces to 20～35 ℃, the leaf slag is discarded;
(4) filtrate is sent into double membrane separation assemblies through compression pump order under 0.01～0.2Mpa operating pressure;
(5) by the first heavy film, hold back and isolate spissated Cyclocarya paliurus Iljinskaja fiber, protein, pectin, polysaccharide, concentrate the Cyclocarya paliurus Iljinskaja filtering solution, get Cyclocarya paliurus Iljinskaja polysaccharide concentrated solution, add ethanol again, leave standstill filtration to containing alcohol amount 70-85%, the centrifugalize precipitation gets the macromolecular polysaccharide product;
(6) residual filtrate is held back and is isolated Cyclocarya paliurus Iljinskaja water soluble organic substance, micromolecular polysaccharide by the second heavy film, through concentrating, add ethanol to containing alcohol amount 70-85% precipitation, leave standstill filtration, the centrifugalize precipitation, vacuum drying gets Cyclocarya paliurus Iljinskaja Organic substance product, micromolecular polysaccharide;
(7) residual filtrate is discharged from solvent outlet.
2, extract the method for polysaccharide and effective ingredient from Cyclocarya paliurus Iljinskaja, comprise the steps:
(1) leaf of Cyclocarya paliurus Iljinskaja is pulverized, placed the lixiviate jar;
(2) alcohol heating reflux of adding 75%;
(3) said extracted liquid is filtered with 250 mesh filter screens;
(4) filtrate concentrates, and reclaims ethanol;
(5) behind the concentrated solution thin up, with big empty resin absorption;
(6) the ethanol eluting, concentrate, drying obtains the organic molecule product;
(7) the leaf slag after the filtration adds entry, under 70 ℃ of temperature, soaks 3-5 hour;
(8) filter the Cyclocarya paliurus Iljinskaja leachate, and temperature reduces to 20～35 ℃, the leaf slag is discarded;
(9) filtrate is sent into double membrane separation assemblies through compression pump order under 0.01～0.2Mpa operating pressure;
(10) by the first heavy film, hold back and isolate spissated Cyclocarya paliurus Iljinskaja fiber, protein, pectin, polysaccharide, concentrate the Cyclocarya paliurus Iljinskaja filtering solution, get Cyclocarya paliurus Iljinskaja polysaccharide concentrated solution, add ethanol again, leave standstill filtration to containing alcohol amount 70-85%, the centrifugalize precipitation gets the macromolecular polysaccharide product;
(11) residual filtrate is by the second heavy film, hold back isolated Cyclocarya paliurus Iljinskaja Organic substance, micromolecular polysaccharide is sent from second outlet, through concentrating, add ethanol to containing alcohol amount 70-85% precipitation, leave standstill filtration, the centrifugalize precipitation, vacuum drying, 70 ℃ of baking temperatures get Cyclocarya paliurus Iljinskaja Organic substance product, micromolecular polysaccharide;
(12) residual filtrate is discharged from solvent outlet.
3, method as claimed in claim 1 or 2 is characterized in that: the water of adding and leaf of Cyclocarya paliurus Iljinskaja weight part ratio are 10～15: 1.
4, method as claimed in claim 1 or 2 is characterized in that: the pH value of described leachate is 6-8.
5, method as claimed in claim 1 or 2 is characterized in that: described leachate weighs membrane separation assemblies by first through first order compression pump under 0.01～0.08Mpa operating pressure; First order residual filtrate weighs membrane separation assemblies by second through second level compression pump under 0.05～0.10Mpa operating pressure.
6, the method for claim 1 is characterized in that: leachate 150-250 purpose strainer filtering.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100734724A CN101244119A (en) | 2008-02-04 | 2008-02-04 | Method for extracting polyoses and active principle from cyclocarya paliurus |
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| CNA2008100734724A CN101244119A (en) | 2008-02-04 | 2008-02-04 | Method for extracting polyoses and active principle from cyclocarya paliurus |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899083A (en) * | 2010-07-28 | 2010-12-01 | 南京林业大学 | Preparation method of cyclocarya paliurus acid A |
| CN102488815A (en) * | 2011-12-15 | 2012-06-13 | 山东大学 | Buccal tablet for reducing blood sugar |
| CN102512959A (en) * | 2011-12-26 | 2012-06-27 | 郴州市明润生物制品有限公司 | Method for separating enriched effective components from plant extract |
| CN102525945A (en) * | 2012-01-11 | 2012-07-04 | 南京林业大学 | Preparation method for cyclocarya paliurus(Batal)Ijinskaja hypoglycemic granules |
| CN102552388A (en) * | 2012-01-11 | 2012-07-11 | 南京林业大学 | Cyclocarya paliurus capsule and preparation method thereof |
| CN103159597A (en) * | 2013-01-21 | 2013-06-19 | 李玉山 | Comprehensive exploration and utilization of active ingredients in branches and leaves of weeping willows |
| CN103494875A (en) * | 2013-09-30 | 2014-01-08 | 浙江大学 | Application of cyclocarya paliurus extract in preparation of medicament for preventing and treating leukemia |
| CN103694364A (en) * | 2013-12-10 | 2014-04-02 | 南昌大学 | Method for synchronously extracting, separating and purifying polysaccharides and flavones of cyclocarya paliurus |
| CN105031294A (en) * | 2015-07-10 | 2015-11-11 | 广西师范大学 | Dendrobium candidum polysaccharide and Cyclocarya paliurus buccal tablets and preparation method thereof |
| CN105054202A (en) * | 2015-08-28 | 2015-11-18 | 江西万茂科技有限公司 | Cyclocarya paliurus herbal plant drink and production technology thereof |
| CN105106300A (en) * | 2015-07-24 | 2015-12-02 | 中国药科大学 | Use of cyclocarya paliurus extract in preparation of drug for preventing and treating non-alcoholic fatty liver disease |
| CN106879413A (en) * | 2015-12-16 | 2017-06-23 | 无限极（中国）有限公司 | A kind of cultivation of selenium-rich blue or green money willow, extracts active ingredients and application |
| CN109021133A (en) * | 2018-07-24 | 2018-12-18 | 南昌大学 | A kind of discoloration method of the blue or green money willow polysaccharide of ultrasound-hydrogen peroxide combination macroreticular resin |
| CN109053924A (en) * | 2018-07-24 | 2018-12-21 | 南昌大学 | A kind of blue or green money willow extract and its application |
| CN109266702A (en) * | 2018-09-27 | 2019-01-25 | 温州科技职业学院 | A kind of method that blue or green money willow extracts polysaccharide |
| CN110183545A (en) * | 2019-06-14 | 2019-08-30 | 台州学院 | A kind of extraction of blue or green money willow polysaccharide and discoloration method |
| CN112778430A (en) * | 2021-01-12 | 2021-05-11 | 江西农业大学 | Sulfated modified cyclocarya paliurus polysaccharide and preparation method and application thereof |
| CN114098089A (en) * | 2021-10-22 | 2022-03-01 | 朗姿赛尔生物科技（广州）有限公司 | Composite peptide composition and composite peptide seasoning tea |
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2008
- 2008-02-04 CN CNA2008100734724A patent/CN101244119A/en active Pending
Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899083A (en) * | 2010-07-28 | 2010-12-01 | 南京林业大学 | Preparation method of cyclocarya paliurus acid A |
| CN102488815A (en) * | 2011-12-15 | 2012-06-13 | 山东大学 | Buccal tablet for reducing blood sugar |
| CN102512959A (en) * | 2011-12-26 | 2012-06-27 | 郴州市明润生物制品有限公司 | Method for separating enriched effective components from plant extract |
| CN102525945A (en) * | 2012-01-11 | 2012-07-04 | 南京林业大学 | Preparation method for cyclocarya paliurus(Batal)Ijinskaja hypoglycemic granules |
| CN102552388A (en) * | 2012-01-11 | 2012-07-11 | 南京林业大学 | Cyclocarya paliurus capsule and preparation method thereof |
| CN102525945B (en) * | 2012-01-11 | 2013-05-08 | 南京林业大学 | Preparation method for cyclocarya paliurus(Batal)Ijinskaja hypoglycemic granules |
| CN103159597A (en) * | 2013-01-21 | 2013-06-19 | 李玉山 | Comprehensive exploration and utilization of active ingredients in branches and leaves of weeping willows |
| CN103494875A (en) * | 2013-09-30 | 2014-01-08 | 浙江大学 | Application of cyclocarya paliurus extract in preparation of medicament for preventing and treating leukemia |
| CN103494875B (en) * | 2013-09-30 | 2015-04-29 | 浙江大学 | Application of cyclocarya paliurus extract in preparation of medicament for preventing and treating leukemia |
| CN103694364A (en) * | 2013-12-10 | 2014-04-02 | 南昌大学 | Method for synchronously extracting, separating and purifying polysaccharides and flavones of cyclocarya paliurus |
| CN105031294A (en) * | 2015-07-10 | 2015-11-11 | 广西师范大学 | Dendrobium candidum polysaccharide and Cyclocarya paliurus buccal tablets and preparation method thereof |
| CN105106300A (en) * | 2015-07-24 | 2015-12-02 | 中国药科大学 | Use of cyclocarya paliurus extract in preparation of drug for preventing and treating non-alcoholic fatty liver disease |
| CN105054202A (en) * | 2015-08-28 | 2015-11-18 | 江西万茂科技有限公司 | Cyclocarya paliurus herbal plant drink and production technology thereof |
| CN106879413A (en) * | 2015-12-16 | 2017-06-23 | 无限极（中国）有限公司 | A kind of cultivation of selenium-rich blue or green money willow, extracts active ingredients and application |
| CN109021133A (en) * | 2018-07-24 | 2018-12-18 | 南昌大学 | A kind of discoloration method of the blue or green money willow polysaccharide of ultrasound-hydrogen peroxide combination macroreticular resin |
| CN109053924A (en) * | 2018-07-24 | 2018-12-21 | 南昌大学 | A kind of blue or green money willow extract and its application |
| CN109021133B (en) * | 2018-07-24 | 2020-08-11 | 南昌大学 | Decolorizing method of cyclocarya paliurus polysaccharide by combining ultrasound and hydrogen peroxide with macroporous resin |
| CN109266702A (en) * | 2018-09-27 | 2019-01-25 | 温州科技职业学院 | A kind of method that blue or green money willow extracts polysaccharide |
| CN110183545A (en) * | 2019-06-14 | 2019-08-30 | 台州学院 | A kind of extraction of blue or green money willow polysaccharide and discoloration method |
| CN110183545B (en) * | 2019-06-14 | 2021-06-11 | 台州学院 | Extraction and decoloration method of cyclocarya paliurus polysaccharide |
| CN112778430A (en) * | 2021-01-12 | 2021-05-11 | 江西农业大学 | Sulfated modified cyclocarya paliurus polysaccharide and preparation method and application thereof |
| CN114098089A (en) * | 2021-10-22 | 2022-03-01 | 朗姿赛尔生物科技（广州）有限公司 | Composite peptide composition and composite peptide seasoning tea |
| CN114098089B (en) * | 2021-10-22 | 2023-06-23 | 朗姿赛尔生物科技（广州）有限公司 | Composite peptide composition and composite peptide seasoning tea |
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