CN102232995A - Preparation method of total flavonoids in medicago sativa L. - Google Patents
Preparation method of total flavonoids in medicago sativa L. Download PDFInfo
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- CN102232995A CN102232995A CN2011101178830A CN201110117883A CN102232995A CN 102232995 A CN102232995 A CN 102232995A CN 2011101178830 A CN2011101178830 A CN 2011101178830A CN 201110117883 A CN201110117883 A CN 201110117883A CN 102232995 A CN102232995 A CN 102232995A
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Abstract
The invention discloses a preparation method of total flavonoids in medicago sativa L. The preparation method comprises the following steps: smashing medicago sativa L. medicinal material, performing reflux extraction 1-3 times by adopting ethanol solution, merging extract, filtering the merged extract with an ultrafiltration membrane, collecting filtrate, adjusting alkalinity and then concentrating the filtrate with a nano-filtration membrane, adjusting acidity of concentrated solution, precipitating the concentrated solution, filtering out precipitate, dispersing the precipitate with hot water, extracting the dispersed precipitate with petroleum ether 1-3 times after the dispersed precipitate becomes cold, removing fat-soluble impurities, evaporating faffinate to dryness, further carrying out reflux dissolution on crystals by adopting ethanol and drying the dissolved crystals, thus obtaining the total flavonoids in medicago sativa L.. The preparation method has the following advantages: the preparation method is simple to operate and short in production period; the ethanol is mostly adopted as the solvent in the extraction and purification processes, so the environmental pollution is low; and the preparation method has industrialization significance.
Description
Technical field:
The invention belongs to the Separation of Natural Products field, especially relate to a kind of method of using ultrafilter membrane and the refining alfalfa total flavones of NF membrane.
Background technology:
Alfalfa Medicago sativa L. is perennial perennial root herbaceous plant, and kind surplus this genus has 70 approximately is distributed in mediterranean region, South-West Asia, the Central Asia and Africa.Alfalfa is in the history in existing more than 2000 year of China plantation, mainly in animal husbandry as feed applications.Among the peoplely be used for the treatment of diseases such as bacillary dysentery, cough due to lung-heat, jaundice, vesical calculus as traditional medical herbs, wherein flavone compound is main functional component monoid.
Flavonoid substances is a kind of significant secondary metabolite of clover.The flavones ingredient of alfalfa platymiscium mainly contains following several: flavone and glycoside thereof, flavonol and glycoside thereof, osajin, isoflavan, chalcone derivative, flavanone and isoflavanone etc.Its glycosyl part mostly is glucose or glucuronic acid greatly, and the report of galactose and rhamnose is also arranged, Resina Ferulae acidylate that also has or coffee acylate.Flavone is proved has many physiologically actives such as non-oxidizability, active anticancer, liver protective effect, estrogen action etc.Because people have recognized many physiologically actives of flavone, people are also increasing gradually for the demand of flavonoid food, and the flavone resource of therefore developing Herba Medicaginis seems particularly important.
The report of existing extraction alfalfa total flavones is still rare, mainly lays particular emphasis on the assay of alfalfa flavone.As " comparative study of alfalfa different cultivars and Various Seasonal flavone amount " that Xu Wenyan delivers, it is reference substance that the document adopts tricin, and the alfalfa of different cultivars is measured comparison in the flavone amount of Different Harvesting Time.Mentioned that the isolation and purification method of Herba Medicaginis flavone has means such as resin adsorption method, solvent extraction and adverse current chromatogram in the document " separation of Herba Medicaginis flavone and biotransformation progress thereof ", but it has not been carried out further concrete narration.
Summary of the invention:
1, goal of the invention: the object of the present invention is to provide a kind of method that is applicable to preparation of industrialization alfalfa total flavones.
2, technical scheme:
A kind of preparation method of alfalfa total flavones, it is characterized in that comprising following steps: with the alfalfa pulverizing medicinal materials, adopt ethanol liquid reflux, extract, 1～3 time, merge extractive liquid, filters through ultrafilter membrane, collect filtered solution, transfer alkali to pH9～11, to concentrate through NF membrane again, the concentrated solution acid adjustment is to pH1～4 precipitations, leach precipitation, disperse, put petroleum ether extraction 1～3 time of cold back with hot water, the weeding of grease solubility impurity, the raffinate evaporate to dryness adopts alcohol crystal 1～4 time again, is drying to obtain the alfalfa total flavones.
Described ethanol liquid is 60～80% ethanol waters, and extraction time is 0.5～2h.
Described ultrafilter membrane is selected inorganic ceramic film for use, and material is aluminium oxide, zirconium oxide, stibium oxide or titanium oxide, holds back particle range 10～20nm, and filtration pressure is 500～1000kPa.
The solvent of described accent alkali is 5% sodium hydroxide solution, and the solvent of acid adjustment is 3% hydrochloric acid solution.
Described NF membrane is selected organic hybrid films for use, and material is polyesters, polyethylene kind or polyamide-based, and molecular cut off is 100～200, and filtration pressure is 1000～1500kPa.
Advantage of the present invention is the following aspects:
1. this process using membrane-membrane separates, and simple to operate, the extraction ratio height has been removed most of impurity;
2. adopt inorganic ceramic film separation efficiency height, but low-temperature operation makes good product quality;
In sum, the present invention has mild condition, operation is few, and advantages such as preparation amount is big, energy savings are suitable for industrialization and amplify.
Further specify the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment:
Embodiment 1:
Alfalfa medical material 1kg, pulverize, adopt 60% ethanol liquid reflux, extract, 3 times, each 0.5h, merge extractive liquid, adds ultrafiltration in the alumina ceramic membrane, and interception is 20nm, filtration pressure is 500kPa, collect ultrafiltrate and add 5% sodium hydroxide and transfer alkali to add to the pH9 in the polyesters composite nanometer filtering film of molecular retention amount 200 to concentrate again, filtrations pressure is 1000kPa, and the collection concentrated solution adds 3% hydrochloric acid acid adjustment and precipitates to pH4, leach precipitation, use the hot water dissolving, put equivalent petroleum ether extraction 3 times of cold back, the weeding of grease solubility impurity, the raffinate evaporate to dryness, adopt alcohol reflux more dissolving crystallized 2 times, be drying to obtain alfalfa total flavones 3.7g, content 87.7%.
Embodiment 2:
Alfalfa medical material 10kg, pulverize, adopt 80% ethanol liquid reflux, extract, 2h, extracting solution adds ultrafiltration in the titanium oxide ceramics film, interception is 10nm, and filtration pressure is 1000kPa, collects ultrafiltrate and adds 5% sodium hydroxide and transfer alkali to add to the pH11 in the polyethylene kind composite nanometer filtering film of molecular retention amount 100 to concentrate again, filtration pressure is 1500kPa, collect concentrated solution and add 3% hydrochloric acid acid adjustment and precipitate to pH1, leach precipitation, use the hot water dissolving, put equivalent petroleum ether extraction 1 time of cold back, the weeding of grease solubility impurity, the raffinate evaporate to dryness adopts alcohol reflux dissolving crystallized 3 times again, be drying to obtain alfalfa total flavones 35.7g, content 85.9%.
Embodiment 3:
Alfalfa medical material 10kg, pulverize, adopt 70% ethanol liquid reflux, extract, 2 times, each 1h, merge extractive liquid, adds ultrafiltration in the stibium oxide ceramic membrane, and interception is 20nm, filtration pressure is 800kPa, collect ultrafiltrate and add 5% sodium hydroxide and transfer alkali to add to the pH10 in the polyamide-based composite nanometer filtering film of molecular retention amount 200 to concentrate again, filtrations pressure is 1400kPa, and the collection concentrated solution adds 3% hydrochloric acid acid adjustment and precipitates to pH2, leach precipitation, use the hot water dissolving, put equivalent petroleum ether extraction 2 times of cold back, the weeding of grease solubility impurity, the raffinate evaporate to dryness, adopt alcohol reflux more dissolving crystallized 1 time, be drying to obtain alfalfa total flavones 36.8g, content 82.3%.
Embodiment 4:
Alfalfa medical material 20kg, pulverize, adopt 750% ethanol liquid reflux, extract, 2 times, each 1.5h, merge extractive liquid, adds ultrafiltration in the zirconia ceramics film, and interception is 10nm, filtration pressure is 700kPa, collect ultrafiltrate and add 5% sodium hydroxide and transfer alkali to add to the pH11 in the polyesters composite nanometer filtering film of molecular retention amount 100 to concentrate again, filtrations pressure is 1200kPa, and the collection concentrated solution adds 3% hydrochloric acid acid adjustment and precipitates to pH3, leach precipitation, use the hot water dissolving, put equivalent petroleum ether extraction 3 times of cold back, the weeding of grease solubility impurity, the raffinate evaporate to dryness, adopt alcohol reflux more dissolving crystallized 4 times, be drying to obtain alfalfa total flavones 69.5g, content 84.9%.
Claims (3)
1. the preparation method of an alfalfa total flavones, it is characterized in that comprising following steps: with the alfalfa pulverizing medicinal materials, adopt ethanol liquid reflux, extract, 1～3 time, merge extractive liquid, filters through ultrafilter membrane, collect filtered solution, transfer alkali to pH9～11, to concentrate through NF membrane again, the concentrated solution acid adjustment is to pH1～4 precipitations, leach precipitation, disperse, put petroleum ether extraction 1～3 time of cold back with hot water, the weeding of grease solubility impurity, the raffinate evaporate to dryness adopts alcohol reflux dissolving crystallized again, is drying to obtain the alfalfa total flavones.
2. the preparation method of a kind of alfalfa total flavones as claimed in claim 1, it is characterized in that described ultrafilter membrane selects inorganic ceramic film for use, material is aluminium oxide, zirconium oxide, stibium oxide or titanium oxide, holds back particle range 10～20nm, and filtration pressure is 500～1000kPa.
3. the preparation method of a kind of alfalfa total flavones as claimed in claim 1, it is characterized in that described NF membrane selects organic hybrid films for use, material is polyesters, polyethylene kind or polyamide-based, and molecular cut off is 100～200, and filtration pressure is 1000～1500kPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101178830A CN102232995A (en) | 2011-05-06 | 2011-05-06 | Preparation method of total flavonoids in medicago sativa L. |
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| CN2011101178830A CN102232995A (en) | 2011-05-06 | 2011-05-06 | Preparation method of total flavonoids in medicago sativa L. |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818119A (en) * | 2015-04-27 | 2015-08-05 | 湖北中烟工业有限责任公司 | Cigarette alfalfa extract and preparation method thereof |
| CN104938853A (en) * | 2015-06-29 | 2015-09-30 | 江西农业大学 | Preparation and application of high-quality broiler chicken additive |
| CN117417006A (en) * | 2023-11-23 | 2024-01-19 | 青岛百发海水淡化有限公司 | Seawater desalination pretreatment process system in low-temperature state and operation method |
-
2011
- 2011-05-06 CN CN2011101178830A patent/CN102232995A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818119A (en) * | 2015-04-27 | 2015-08-05 | 湖北中烟工业有限责任公司 | Cigarette alfalfa extract and preparation method thereof |
| CN104938853A (en) * | 2015-06-29 | 2015-09-30 | 江西农业大学 | Preparation and application of high-quality broiler chicken additive |
| CN104938853B (en) * | 2015-06-29 | 2018-05-11 | 江西农业大学 | A kind of preparation and its application of quality broiler chicken additive |
| CN117417006A (en) * | 2023-11-23 | 2024-01-19 | 青岛百发海水淡化有限公司 | Seawater desalination pretreatment process system in low-temperature state and operation method |
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Application publication date: 20111109 |