CN102659873A - Method for extracting nicotifiorin from nymphaea candida presl - Google Patents
Method for extracting nicotifiorin from nymphaea candida presl Download PDFInfo
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- CN102659873A CN102659873A CN2012101151616A CN201210115161A CN102659873A CN 102659873 A CN102659873 A CN 102659873A CN 2012101151616 A CN2012101151616 A CN 2012101151616A CN 201210115161 A CN201210115161 A CN 201210115161A CN 102659873 A CN102659873 A CN 102659873A
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Abstract
The invention discloses a method for extracting nicotifiorin from nymphaea candida presl. The method comprises the following steps: crushing nymphaea candida presl; adding 6-15 folds of water, and performing refluxing extraction for 2-3 times; filtering an extract solution; adding the extract solution into an ultrafiltration membrane system for ultrafiltration; adding a permeated solution into a nanofiltration membrane system for concentration; regulating pH value of a concentrated solution to 2-5; standing, and precipitating; filtering out undissolved substances; extracting a filtrate with ethyl acetate; collecting the extract solution; concentrating the extract solution till a small volume; crystallizing, and recrystallizing crystals with an ethanol solution; and drying to obtain the nicotifiorin. After the adoption of the method for extracting the nicotifiorin from the nymphaea candida presl, the technical process and the operation are simple, the using amount of organic reagents is small and the industrial production is easily realized.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, particularly relate to a kind of method of from water lily, extracting Nicotifiorin.
Background technology
Nicotifiorin is the luxuriant and rich with fragrance alcohol of camphane-3-O-rutinoside again, is a kind of flavonoid glycoside material, CAS 17650-84-9, and molecular formula C27H30O5, molecular weight 594.5, molecular structural formula does
Water lily is the dry flower of Nymphaeceae Nymphaea Nymphaea candida; Received people's " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Uygur medicine fascicle version in 1998; Having the heat of falling quenches the thirst; The benefit heart protects brain, and the effect of ataralgesia is usually used in treating cold, fever, headache cough and pharyngalgia disease such as induce sweat.Modern study shows, contains multiple Flavonoid substances in the water lily, has stronger antioxygenation, and Nicotifiorin is exactly an effective constituent wherein, the bibliographical information mass percent is arranged up to 3.82%.
From water lily, extract the method for Nicotifiorin, adopt the resin column method more." the flavonol glycosides constituents analysis in the dimension medicine water lily " delivered like people such as document Zhao Jun; The process for extracting of Nicotifiorin is that water lily is extracted with methanol eddy in the document; Concentrated extract is used sherwood oil, ETHYLE ACETATE, n-butanol extraction successively, propyl carbinol part again through polymeric amide and gel column repeatedly purifying obtain Nicotifiorin.Also having Zhao Jun also is to have discussed this kind method in paper " four kinds medicinal plant chemical ingredients and bioactivity research " thereof.This class methods complex operation, the organic reagent consumption is big, is not suitable for industriallization.
Also have glycoside conversion to obtain in addition through Nicotifiorin.As " preparing the method for the non-alcohol of down-3-O-rutinoside and contain kaempferol-3-O-rutinoside composition for external application " at Chinese patent (application number 200780038247.0); This patent disclosed method is mainly to be to be raw material with green tea; Extraction contains the glycoside of kaempferol-3-O-rutinoside, carries out the biological enzymolysis conversion then and obtains kaempferol-3-O-rutinoside.But the glycoside content of Nicotifiorin is less in this kind method raw material, and leaching process also is comparatively loaded down with trivial details.
Summary of the invention
The objective of the invention is to solve the deficiency and the defective of prior art, a kind of method of from water lily, extracting Nicotifiorin is provided.
The objective of the invention is to realize through following technical scheme:
It is broken to get water lily pollen, adds 6-15 times of water gaging refluxing extraction, extracts 2-3 time, behind the extracting liquid filtering; Add the ultrafiltration membrane system ultrafiltration, add the nf membrane system again through liquid and concentrate, liquid concentrator is regulated pH2-5; Place deposition, the filtering insolubles, filtrating is used ethyl acetate extraction; Collect extraction liquid and concentrate the small volume crystallization, crystallisate is used the ethanolic soln recrystallization again, is drying to obtain.
Described ultra-filtration membrane is a hollow cellulose film of holding back component 2000-10000.The hollow cellulose film of preferred molecular weight cut-off 2000.
Described nf membrane is the hollow cellulose film of molecular weight cut-off 100-500.The hollow cellulose film of preferred molecular weight cut-off 400.
Advantage of the present invention is: method adopts membrane separation technique purifying Nicotifiorin, utilizes the water-soluble character of Nicotifiorin, and is different according to molecular weight; Select the film impurity trapped in different apertures, physical method, energy consumption is low; Easy and simple to handle, treatment capacity is big, and whole technology is easy to industriallization.
Embodiment
To combine embodiment to further specify the present invention below.
Embodiment 1:
Water lily pollen is broken, gets 10kg and adds 15 times of water gaging refluxing extraction, extracts 2 times, behind the extracting liquid filtering; Add the hollow cellulose film system ultrafiltration of holding back component 2000, add the suitable quantity of water dialysis, it is concentrated with 400 hollow cellulose film system again to see through liquid; Liquid concentrator is regulated pH3 with Hydrogen chloride, places deposition, the filtering insolubles; Filtrating is with equal-volume ethyl acetate extraction 3 times, and the collection extraction liquid is concentrated into 1/5 volume, crystallization; Crystallisate leaches and uses 90% ethanolic soln backflow dissolving-recrystallization again, dry pale yellow powder Nicotifiorin 367g, the content 93.5% of getting.
Embodiment 2:
Water lily pollen is broken, gets 10kg and adds 6 times of water gaging refluxing extraction, extracts 3 times, behind the extracting liquid filtering; Add the hollow cellulose film system ultrafiltration of holding back component 6000, add the suitable quantity of water dialysis, it is concentrated with 500 hollow cellulose film system again to see through liquid; Liquid concentrator is regulated pH4 with dilute sulphuric acid, places deposition, the filtering insolubles; Filtrating is with equal-volume ethyl acetate extraction 2 times, and the collection extraction liquid is concentrated into 1/7 volume, crystallization; Crystallisate leaches and uses 95% ethanolic soln backflow dissolving-recrystallization again, dry pale yellow powder Nicotifiorin 421g, the content 85.1% of getting.
Claims (3)
1. method of from water lily, extracting Nicotifiorin, it is characterized in that: it is broken to get water lily pollen, adds 6-15 times of water gaging refluxing extraction, extracts 2-3 time; Behind the extracting liquid filtering, add the ultrafiltration membrane system ultrafiltration, add the nf membrane system again through liquid and concentrate, liquid concentrator is regulated pH2-5; Place deposition, the filtering insolubles, filtrating is used ethyl acetate extraction; Collect extraction liquid and concentrate the small volume crystallization, crystallisate is used the ethanolic soln recrystallization again, is drying to obtain.
2. the method for from water lily, extracting Nicotifiorin according to claim 1 is characterized in that described ultra-filtration membrane is a hollow cellulose film of holding back component 2000-10000.
3. the method for from water lily, extracting Nicotifiorin according to claim 1 is characterized in that described nf membrane is the hollow cellulose film of molecular weight cut-off 100-500.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101151616A CN102659873A (en) | 2012-04-19 | 2012-04-19 | Method for extracting nicotifiorin from nymphaea candida presl |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101151616A CN102659873A (en) | 2012-04-19 | 2012-04-19 | Method for extracting nicotifiorin from nymphaea candida presl |
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| CN2012101151616A Pending CN102659873A (en) | 2012-04-19 | 2012-04-19 | Method for extracting nicotifiorin from nymphaea candida presl |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923138A (en) * | 2014-05-08 | 2014-07-16 | 江西天施康中药股份有限公司 | Preparation method and application of nicotiflorin |
| CN103965309A (en) * | 2014-05-22 | 2014-08-06 | 广西平果华莲科技研究所 | Extraction method of nymphaea tetragona ovary collagen |
| CN109956984A (en) * | 2019-04-23 | 2019-07-02 | 河南大学 | Extraction separation method of the Nicotifiorin in China rose |
-
2012
- 2012-04-19 CN CN2012101151616A patent/CN102659873A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923138A (en) * | 2014-05-08 | 2014-07-16 | 江西天施康中药股份有限公司 | Preparation method and application of nicotiflorin |
| CN103923138B (en) * | 2014-05-08 | 2016-03-23 | 江西天施康中药股份有限公司 | A kind of preparation method of Nicotifiorin and application thereof |
| CN103965309A (en) * | 2014-05-22 | 2014-08-06 | 广西平果华莲科技研究所 | Extraction method of nymphaea tetragona ovary collagen |
| CN109956984A (en) * | 2019-04-23 | 2019-07-02 | 河南大学 | Extraction separation method of the Nicotifiorin in China rose |
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Application publication date: 20120912 |