CN102078357A - Preparation method of Gynura bicolor total flavone extract - Google Patents
Preparation method of Gynura bicolor total flavone extract Download PDFInfo
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- CN102078357A CN102078357A CN 201010611189 CN201010611189A CN102078357A CN 102078357 A CN102078357 A CN 102078357A CN 201010611189 CN201010611189 CN 201010611189 CN 201010611189 A CN201010611189 A CN 201010611189A CN 102078357 A CN102078357 A CN 102078357A
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Abstract
The invention discloses a preparation method of a Gynura bicolor total flavone extract. The method comprises the following steps: (1) drying and grinding Gynura bicolor; (2) extracting with ethanol or methanol, mixing extracting solutions, and concentrating under reduced pressure to obtain extractum; (3) adding water in the extractum obtained in the step (2), standing to cool, centrifuging to remove precipitates and obtain supernatant for standby; performing adsorption on the supernatant obtained in the step (3) by utilizing macroporous adsorption resin, and performing gradient elution with ethanol; (5) collecting the ethanolic elution solution obtained in the step (4) to concentrate under reduced pressure, adsorbing with macroporous resin, and performing gradient elution with ethanol; and (6) concentrating and drying the ethanolic elution solution obtained in the step (5) to obtain the Gynura bicolor total flavone extract.
Description
Technical field:
The present invention relates to from the Chinese medicine GynurabicolorDC, extract the method for preparing total flavones.
Background technology:
GynurabicolorDC (Gynura bicolor DC.) is the Compositae herbaceos perennial, this plant herb have invigorate blood circulation, the effect of hemostasis, removing toxic substances and promoting subsidence of swelling, be used for the treatment of dysmenorrhea, metrorrhagia, hemoptysis, wound hemorrhage, ulcer and do not close up for a long time; Its root has the function of promoting flow of QI and blood, is used for the treatment of to stop stasis of blood stomachache, metrorrhagia, malaria puerperal.Isolating chemical constituent mainly contains compositions such as flavonoid from GynurabicolorDC at present, but Shang Weiyou is at the report of the preparation technology aspect of GynurabicolorDC total flavones.
Summary of the invention:
The invention provides a kind of preparation method of GynurabicolorDC extractive of general flavone, this method may further comprise the steps:
(1) with the GynurabicolorDC drying and crushing;
(2) with ethanol or methanol extraction, merge extractive liquid,, concentrating under reduced pressure becomes extractum;
(3) step (2) extractum is added water and place Cryoprecipitation, the centrifugal precipitation of going, supernatant is standby;
(4) macroporous adsorbent resin on the supernatant that (3) are obtained is used ethanol gradient elution;
(5) collect step (4) ethanol elution concentrating under reduced pressure, go up macroporous resin again, use ethanol gradient elution;
(6) step (5) ethanol elution concentrate drying gets the GynurabicolorDC extractive of general flavone.
Wherein the extracting method of step (2) is every kilogram of GynurabicolorDC medical material, adding 8-12L concentration is ethanol or the methanol of 70%-80%, and hot reflux or dipping or percolation extract 2-4 time, and each 1-3h is extracted in hot reflux, dipping or percolation extracted merge extractive liquid, each 15 days.
Adding the water yield in the step (3) is 8-10 times of water of extractum weight ratio.
Macroporous resin described in the step (4) is a D101 type macroporous resin, and the weight ratio of GynurabicolorDC is described in macroporous resin and the step (1): 0.5-5: 1.
Eluting solvent adopts macroporous resin volume ratio 10-15 20% ethanol, 40% ethanol gradient elution doubly in the step (4), merges 40% ethanol elution.
Macroporous resin described in the step (5) is a D101 type macroporous resin, and the weight ratio of GynurabicolorDC is described in macroporous resin and the step (1): 0.5-5: 1.
Eluting adopts macroporous resin volume ratio 10-15 20% ethanol, 40% ethanol gradient elution doubly in the step (5), merges 40% ethanol elution.
Advantage of the present invention have following some:
(1) the present invention adopts alcohol extraction in conjunction with the macroporous resin enrichment method total flavones in the GynurabicolorDC to be made with extra care, and can effectively improve general flavone content, records general flavone content through ultraviolet spectrophotometry and all is higher than 50% in rutin.
(2) the present invention has increased after the GynurabicolorDC alcohol extraction and has added the heavy step of water-cooled, can make low polar impurity sedimentation eliminations such as chlorophyll, and the flavonoid high polarity becomes fractionation in supernatant, makes that general flavone content is improved in the solution.
(3) macroporous adsorbent resin is to be monomer with styrene and propionic ester, and the adding Ethenylbenzene is a cross-linking agent, and toluene, dimethylbenzene are porogen, and their polymerizations that is cross-linked with each other have formed porous skeleton structure.The resin absorption effect is the Van der Waals force that relies between it and the molecule (adsorbate) that is adsorbed, carry out physical absorption by its huge specific surface and work, the organifying compound is according to having absorption affinity and molecular weight size thereof separately to reach separation, purification, remove impurity, various objectives such as concentrated through certain solvent elution.Except that containing flavones ingredient, also contain impurity such as polysaccharide, micromolecule aminoacid in the GynurabicolorDC.Adopt macroporous resin water-pure gradient elution method, flavone is better separated with impurity, improve flavones content in the finished product.
(4) used the method for macroporous resin secondary eluting among the present invention, the GynurabicolorDC total flavones is increased to 50% from the refining back of macropore first time content 30%, has improved general flavone content.
The specific embodiment
Optimal process embodiment
This test adopts following 4 kinds of methods to prepare the GynurabicolorDC extractive of general flavone, according to the determined by ultraviolet spectrophotometry general flavone content, and compares:
A, alcohol extraction are followed the example of: 100g GynurabicolorDC medicinal material coarse powder, add 12 times of amounts of medical material weight and 10 times of amount 70% alcohol reflux twice respectively, and extraction time was respectively 2 hours, 1 hour, filtered merge extractive liquid, and concentrate drying.
B, ethanol extract from water precipitation: 100g GynurabicolorDC medicinal material coarse powder, add twice of 12 times of amounts of medical material weight and 10 times amount, 70% alcohol reflux respectively, extraction time was respectively 2 hours, 1 hour, filter, merge extractive liquid, also is condensed into extractum, and extractum adds 10 times of water gaging dissolvings of weight ratio, Cryoprecipitation 12 hours, centrifugal, the supernatant concentration drying.
C, alcohol extracting-water precipitating are in conjunction with the macroporous resin method for refining: 100g GynurabicolorDC medicinal material coarse powder, add twice of 12 times of amounts of medical material weight and 10 times amount, 70% alcohol reflux respectively, extraction time was respectively 2 hours, 1 hour, filter, merge extractive liquid, also is condensed into extractum, extractum adds 10 times of water gaging dissolvings of weight ratio, Cryoprecipitation 12 hours, centrifugal, supernatant adds in the 50gD101 macroporous resin, with 10 times of volume 20% ethanol of macroporous resin, 40% ethanol gradient elution, collect 40% ethanol elution, concentrate drying respectively.
D, alcohol extracting-water precipitating are in conjunction with the macroporous resin method of re-refining: 100g GynurabicolorDC medicinal material coarse powder, add twice of 12 times of amounts of medical material weight and 10 times amount, 70% alcohol reflux respectively, extraction time was respectively 2 hours, 1 hour, filtered, and merge extractive liquid, also is condensed into extractum, extractum adds 10 times of water gaging dissolvings of weight ratio, Cryoprecipitation 12 hours, centrifugal, supernatant adds the 50gD101 macroporous resin, with 10 times of volume 20% ethanol of macroporous resin, 40% ethanol gradient elution, collect 40% ethanol elution respectively.40% ethanol elution is concentrated into does not have the alcohol flavor, adds in the 50gD101 macroporous resin, with 10 times of volume 20% ethanol of macroporous resin, 40% ethanol gradient elution, collects 40% ethanol elution, concentrate drying respectively.
The content of total flavone assay method:
The preparation of reference substance solution: precision takes by weighing rutin standard substance 5.0mg in the 25mL volumetric flask, with 70% ethanol ultrasonic dissolution, and standardize solution, getting concentration is 0.2mgmL
-1The rutin titer.
The preparation of sample solution: precision pipettes GynurabicolorDC extractive of general flavone 0.5g in the volumetric flask of 25mL, adds that 70% ethanol is ultrasonic to make dissolving, shakes up promptly.
The mensuration of general flavone content in the sample: precision pipettes sample solution 1ml and adds 0.1molL
-1AlCl
36H
2O 1.0mL with 70% ethanol standardize solution, shakes up, and measures absorbance in the 412nm place behind the placement 15min, according to rutin standard curve calculation sample general flavone content.
The results are shown in Table 1, the general flavone content that method D alcohol extracting-water precipitating obtains in conjunction with the macroporous resin method of re-refining is apparently higher than other three kinds of general flavone contents that method obtains.
The general flavone content that the different preparation methoies of table 1 are extract obtained
Product embodiments 1
GynurabicolorDC medicinal material coarse powder 1.0kg, after 48 hours, percolation extracts with 12 times of 70% alcohol dipping of medical material weight ratio, and percolation is shallow to the effluent color, and till the flavone reaction was not obvious, concentrating under reduced pressure was thick paste, adds 10 times of weight water of thick paste weight ratio, stirred Cryoprecipitation 12 hours.Put centrifuge sedimentation and centrifugation (2000 rev/mins of rotating speeds, 15 minutes), it is standby to get supernatant.
Supernatant adds in the 500gD101 macroporous resin, with 10 times of volume 20% ethanol of macroporous resin, 40% ethanol gradient ethanol elution, collects 40% ethanol elution respectively.40% ethanol elution is concentrated into does not have the alcohol flavor, add in the 500gD101 macroporous resin, with 10 times of volume 20% ethanol of macroporous resin, 40% ethanol gradient elution, collect 40% ethanol elution respectively, concentrate drying gets the GynurabicolorDC extractive of general flavone, and general flavone content is 57.12%.
Product embodiments 2
GynurabicolorDC medicinal material coarse powder 1.0kg extracts 2 times with 12 times of 70% alcohol heating reflux of medical material weight ratio, and each 2 hours, the extracting solution concentrating under reduced pressure was thick paste, added 10 times of weight water of thick paste weight ratio, stirred Cryoprecipitation 12 hours.Put centrifuge sedimentation and centrifugation (2000 rev/mins of rotating speeds, 15 minutes), it is standby to get supernatant.
Supernatant adds in the 1.0kgD101 macroporous resin, with 10 times of volume 20% ethanol of macroporous resin, 40% ethanol gradient elution, collects 40% ethanol elution respectively.40% ethanol elution is concentrated into does not have the alcohol flavor, add in the 500gD101 macroporous resin, with 10 times of volume 20% ethanol of macroporous resin, 40% ethanol gradient elution, collect 40% ethanol elution respectively, concentrate drying gets the GynurabicolorDC extractive of general flavone, and general flavone content is 58.91%.
Product embodiments 3
GynurabicolorDC medicinal material coarse powder 1.0kg, with 12 times of 80% ethanol 8L of medical material weight ratio, 6L merceration twice, each 15 days, the extracting solution concentrating under reduced pressure was thick paste, added 8 times of weight water of thick paste weight ratio, stirred Cryoprecipitation 12 hours.Put centrifuge sedimentation and centrifugation (2000 rev/mins of rotating speeds, 15 minutes), it is standby to get supernatant.
Supernatant adds in the 1.0kgD101 macroporous resin, respectively with 10 times of volume 20% ethanol of macroporous resin, 40% ethanol gradient elution, collect 40% ethanol elution, 40% ethanol elution is concentrated into does not have the alcohol flavor, adds in the 1.0kgD101 macroporous resin, respectively with 10 times of volume 20% ethanol of macroporous resin, 40% ethanol gradient elution, collect 40% ethanol elution, concentrate drying gets the GynurabicolorDC extractive of general flavone, and general flavone content is 56.11%.
Claims (7)
1. the preparation method of a GynurabicolorDC extractive of general flavone, it is characterized in that: this method may further comprise the steps:
(1) with the GynurabicolorDC drying and crushing;
(2) with ethanol or methanol extraction, merge extractive liquid,, concentrating under reduced pressure becomes extractum;
(3) step (2) extractum is added water and place Cryoprecipitation, the centrifugal precipitation of going, supernatant is standby;
(4) macroporous adsorbent resin on the supernatant that (3) are obtained is used ethanol gradient elution;
(5) collect step (4) ethanol elution concentrating under reduced pressure, go up macroporous resin again, use ethanol gradient elution;
(6) step (5) ethanol elution concentrate drying gets the GynurabicolorDC extractive of general flavone.
2. the preparation method of GynurabicolorDC extractive of general flavone according to claim 1 is characterized in that: adding the water yield in the step (3) is 8-10 times of water of extractum weight ratio.
3. the preparation method of GynurabicolorDC extractive of general flavone according to claim 1 is characterized in that: macroporous resin described in the step (4) is a D101 type macroporous resin, and the weight ratio of GynurabicolorDC is described in macroporous resin and the step (1): 0.5-5: 1.
4. the preparation method of GynurabicolorDC extractive of general flavone according to claim 1 is characterized in that: macroporous resin described in the step (5) is a D101 type macroporous resin, and the weight ratio of GynurabicolorDC is described in macroporous resin and the step (1): 0.5-5: 1.
5. according to the preparation method of the arbitrary described GynurabicolorDC extractive of general flavone of claim 1 to 4, it is characterized in that: the extracting method of step (2) is every kilogram of GynurabicolorDC medical material, adding 8-12L concentration is ethanol or the methanol of 70%-80%, hot reflux or dipping or percolation extract 2-4 time, each 1-3h is extracted in hot reflux, dipping or percolation extracted merge extractive liquid, each 15 days.
6. require the preparation method of 1 to 4 arbitrary described GynurabicolorDC extractive of general flavone according to claim, it is characterized in that: eluting solvent adopts macroporous resin volume ratio 10-15 20% ethanol, 40% ethanol gradient elution doubly in the step (4), merges 40% ethanol elution.
7. require the preparation method of 1 to 4 arbitrary described GynurabicolorDC extractive of general flavone according to claim, it is characterized in that: eluting solvent adopts macroporous resin volume ratio 10-15 20% ethanol, 40% ethanol gradient elution doubly in the step (5), merges 40% ethanol elution.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102690324A (en) * | 2012-06-18 | 2012-09-26 | 江苏省中国科学院植物研究所 | Gynura bicolor protein extract, and preparation method and application thereof |
| CN102911511A (en) * | 2011-08-02 | 2013-02-06 | 苏州宝泽堂医药科技有限公司 | Method for extracting purple pigment and total flavonoids from fresh gynura bicolor |
| CN102920753A (en) * | 2012-11-05 | 2013-02-13 | 江苏省中国科学院植物研究所 | Dichromatism gmelin sealavender herb extractive and application thereof |
| CN103463159A (en) * | 2013-09-17 | 2013-12-25 | 江苏省中国科学院植物研究所 | Method for extracting and separating total flavonoids from fresh stem and leaves of gynura bicolor |
| CN106344641A (en) * | 2016-10-19 | 2017-01-25 | 中国农业科学院北京畜牧兽医研究所 | Method for preparing total flavonoid extract of alfalfa |
-
2010
- 2010-12-29 CN CN 201010611189 patent/CN102078357A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《时珍国医国药》 20100131 裴咏萍等 大孔树脂对红凤菜总黄酮的吸附分离特性研究 8，9 第21卷, 第1期 * |
| 《江苏农业科学》 20090415 裴咏萍等 红凤菜总黄酮提取工艺的研究 , 第02期 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911511A (en) * | 2011-08-02 | 2013-02-06 | 苏州宝泽堂医药科技有限公司 | Method for extracting purple pigment and total flavonoids from fresh gynura bicolor |
| CN102690324A (en) * | 2012-06-18 | 2012-09-26 | 江苏省中国科学院植物研究所 | Gynura bicolor protein extract, and preparation method and application thereof |
| CN102690324B (en) * | 2012-06-18 | 2013-10-09 | 江苏省中国科学院植物研究所 | Gynura bicolor protein extract, and preparation method and application thereof |
| CN102920753A (en) * | 2012-11-05 | 2013-02-13 | 江苏省中国科学院植物研究所 | Dichromatism gmelin sealavender herb extractive and application thereof |
| CN103463159A (en) * | 2013-09-17 | 2013-12-25 | 江苏省中国科学院植物研究所 | Method for extracting and separating total flavonoids from fresh stem and leaves of gynura bicolor |
| CN106344641A (en) * | 2016-10-19 | 2017-01-25 | 中国农业科学院北京畜牧兽医研究所 | Method for preparing total flavonoid extract of alfalfa |
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Application publication date: 20110601 |