CN101380347A - Ainsliaea fragrans Champ total flavone extract and extraction method and use thereof - Google Patents
Ainsliaea fragrans Champ total flavone extract and extraction method and use thereof Download PDFInfo
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- CN101380347A CN101380347A CNA2008102280694A CN200810228069A CN101380347A CN 101380347 A CN101380347 A CN 101380347A CN A2008102280694 A CNA2008102280694 A CN A2008102280694A CN 200810228069 A CN200810228069 A CN 200810228069A CN 101380347 A CN101380347 A CN 101380347A
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Abstract
The invention belongs to the pharmaceutical technology field and provides an extract of total flavonoids of frangrant ainsliaea herb, an extraction method thereof and a use. The extract adopts the frangrant ainsliaea herb as a raw material, ethanol which is prepared by weak alkaline solutions with the different pH values is taken as an extraction solvent, the reflux extraction is adopted, the impurities are removed by the petroleum ether extraction, the separation and the enrichment are finally carried by macroporous resin, and the purity of the components of the obtained total flavonoids is 50-95 percent. The invention has simple process, convenient and safe operation and good repeatability and can be used for the industrial production. The invention further provides an application of the components of the total flavonoids or a preparation which is prepared by the total flavonoids and a pharmaceutically acceptable carrier in the prepration of drugs for treating acute and chronic cervicitis.
Description
Technical field
The invention belongs to medical technical field, relate to Ainsliaea fragrans Champ total flavone extract and extracting method thereof and purposes.
Background technology
Ainsliasa fragrans Champ is a medicine commonly used among the people, is the dry herb of feverfew Ainsliasa fragrans Champ (Ainsliaeafragrans Champ.).Sweet, the little hardship of Ainsliasa fragrans Champ nature and flavor, cool in nature is returned lung, Liver Channel.Has the heat clearing away tonify deficiency, cooling blood for hemostasis, effects such as eliminating damp, detoxifying.Cure mainly the asthenia hectic fever due to YIN-deficiency, lung rash hemoptysis, woman uterine bleeding, jaundice due to damp-heat, edema, swollen ulcer drug, scrofula tuberculosis, traumatic injury, venom etc.Treat diseases such as cervical erosion, endometritis, furuncle, thrush with Ainsliasa fragrans Champ preparation and folk remedy compatibility clinically.The few conventional Chinese medicine of Ainsliasa fragrans Champ conduct still belongs to blank in many aspects, remains further to be developed, in the hope of bringing into play its maximum effect.
Up to the present, the chemical compound of bibliographical information comprises the sesquiterpene lactones class, and three mushrooms, organic acid, flavonoid etc., Ainsliasa fragrans Champ preparation comprise Ainsliasa fragrans Champ sheet, compound recipe Ainsliasa fragrans Champ granule etc.Preparation technology's method of present commercially available Ainsliaea fragrans Champ. preparation is outmoded, all is the preparations after the simple extraction of Ainsliasa fragrans Champ process, and active constituent content is low, and day clothes dosage is big.For reducing taking dose, raising drug effect, the present invention adopts new method that Ainsliasa fragrans Champ is carried out extraction separation, obtains more highly purified extract, has improved active constituent content, reduces taking dose, improves curative effect.
Extraction separation for natural product, macroreticular resin absorbing method is a kind of very effective industrialized preparing process, this method is chosen (selecting Different concentrations of alcohol solvent and investigation to regulate pH value with weakly alkaline solution), oil-soluble impurities from extracting solvent the selection that is removed to eluant is optimized, carry out extraction separation under per step optimal conditions, general flavone content all is higher than the finding bibliographical information in the total flavonoid composition rate of transform, the purification thing.
Summary of the invention
The object of the present invention is to provide a kind of Ainsliaea fragrans Champ total flavone extract and extracting method thereof and purposes.
The present invention seeks to realize by following measure:
A kind of extracting method of Ainsliaea fragrans Champ total flavone comprises following processing step: 1. get drying, the Ainsliaea fragrans Champ. medical material of pulverizing is doubly measured alcoholic solution 30-100 ℃ reflux, extract, 2-4 time that concentration is 5%-90% with 6-15.Filter, filtrate concentrates.2. get extract concentrated solution, use petroleum ether extraction 2-4 time, keep macroporous resin column absorption on the water layer; Or directly get the extract concentrated solution upper prop.3. use 0%-15% alcoholic solution eluting macroporous resin column colourless to eluent, eluent is collected with the ethanol elution of 10%-95% in the back, reclaims ethanol, and evaporate to dryness is to the extractum shape, and vacuum drying is pulverized, ainsliaea fragrans champ-extract.
The step 1. ethanol extraction solution of described 5%-95% can be weakly alkaline solutions such as ammonia, calcium hydroxide, the sodium carbonate preparation of 7.5-10 with pH value.
Low polar macroporous resin such as D-101 resin etc. during the 2. described macroporous resin of step can be.
Content of total flavone is between 50%-95% in the extract of step described in 3..
The application of described ainsliaea fragrans champ-extract in the medicine of treatment acute and chronic cervicitis: with the total flavones is active component, is equipped with pharmaceutic adjuvant, is prepared into any dosage form on the pharmaceutics with known method.
Technology of the present invention is simple, easy and safe to operate, the rate of transform approximately from 37% be increased to 87%, extraction ratio improves 135% approximately, favorable repeatability can be used for suitability for industrialized production.
The specific embodiment
Embodiment 1:
Get Ainsliaea fragrans Champ. medical material 1kg, pulverize, cross 20 mesh sieves, in addition the 12000ml pH value is that the volume fraction of 9 aqua calcis preparation is 5% alcoholic solution, and reflux, extract, 2 hours is filtered also preservation filtrate, repetitive operation 3 times.Merge three times filtrate, filtrate is concentrated into and contains flavone 2mg/ml approximately, uses petroleum ether extraction three times, keeps water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% an ethanol elution 2-4 volume, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless to be eluted to eluent with a large amount of distilled water, with 5 volumes of 10% ethanol elution, collects 10% alcoholic acid eluent, concentrates and evaporate to dryness, gets Ainsliaea fragrans Champ. purification thing, and general flavone content is about 55%.
Embodiment 2:
Get Ainsliaea fragrans Champ. medical material 1kg, pulverize, cross 20 mesh sieves, in addition the 12000ml pH value is that the volume fraction of 8 aqua calcis preparation is 10% alcoholic solution, and reflux, extract, 2 hours is filtered also preservation filtrate, repetitive operation 3 times.Merge three times filtrate, filtrate is concentrated into and contains flavone 2mg/ml approximately, uses petroleum ether extraction three times, keeps water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% an ethanol elution 2-4 volume, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless to be eluted to eluent with a large amount of distilled water, with 5 volumes of 30% ethanol elution, collects 30% alcoholic acid eluent, concentrates and evaporate to dryness, gets Ainsliaea fragrans Champ. purification thing, and general flavone content is about 67%.
Embodiment 3:
Get Ainsliaea fragrans Champ. medical material 1kg, pulverize, cross 20 mesh sieves, in addition the 12000ml pH value is that 8 ammonia dose volume mark is 30% alcoholic solution, and reflux, extract, 2 hours is filtered also preservation filtrate repetitive operation 3 times.Merge three times filtrate, filtrate is concentrated into and contains flavone 2mg/ml approximately, uses petroleum ether extraction three times, keeps water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% an ethanol elution 2-4 volume, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless to be eluted to eluent with a large amount of distilled water, with 5 volumes of 30% ethanol elution, collects 30% alcoholic acid eluent, concentrates and evaporate to dryness, gets Ainsliaea fragrans Champ. purification thing, and general flavone content is about 69%.
Embodiment 4:
Get Ainsliaea fragrans Champ. medical material 1kg, pulverize, cross 20 mesh sieves, in addition the 12000ml pH value is that 9 ammonia dose volume mark is 50% alcoholic solution, and reflux, extract, 2 hours is filtered also preservation filtrate, repetitive operation 3 times.Merge three times filtrate, filtrate is concentrated into and contains flavone 2mg/ml approximately, uses the petroleum ether extraction secondary, keeps water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% an ethanol elution 2-4 volume, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless that alcoholic solution with 5% is eluted to eluent, with 5 volumes of 50% ethanol elution, collects 50% alcoholic acid eluent, concentrates and evaporate to dryness, gets Ainsliaea fragrans Champ. purification thing, and general flavone content is about 79%.
Embodiment 5:
Get Ainsliaea fragrans Champ. medical material 1kg, pulverize, cross 20 mesh sieves, in addition the 12000ml pH value is that 9 sodium carbonate dose volume mark is 70% alcoholic solution, and reflux, extract, 2 hours is filtered also preservation filtrate, repetitive operation 3 times.Merge three times filtrate, filtrate is concentrated into and contains flavone 2mg/ml approximately, uses the petroleum ether extraction secondary, keeps water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% an ethanol elution 2-4 volume, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless that alcoholic solution with 10% is eluted to eluent, with 5 volumes of 70% ethanol elution, collects 70% alcoholic acid eluent, concentrates and evaporate to dryness, gets Ainsliaea fragrans Champ. purification thing, and general flavone content is about 84%.
Embodiment 6:
Get Ainsliaea fragrans Champ. medical material 1kg, pulverize, cross 20 mesh sieves, in addition the 12000ml pH value is that 8 sodium carbonate dose volume mark is 95% alcoholic solution, and reflux, extract, 2 hours is filtered also preservation filtrate, repetitive operation 3 times.Merge three times filtrate, filtrate is concentrated into and contains flavone 2mg/ml approximately, uses the petroleum ether extraction secondary, keeps water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% an ethanol elution 2-4 volume, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless that alcoholic solution with 15% is eluted to eluent, with 5 volumes of 95% ethanol elution, collects 95% alcoholic acid eluent, concentrates and evaporate to dryness, gets Ainsliaea fragrans Champ. purification thing, and general flavone content is about 90%.
Embodiment 7: the screening of ainsliaea fragrans champ-extract anti-inflammatory activity
Adopt water extraction method to obtain that extract F1 (the 1g extract is equivalent to raw medicinal herbs 6.7g), alkaline alcohol solution extraction method obtain extract F2 (the 1g extract is equivalent to raw medicinal herbs 4.2g), macroporous resin separation and purification method obtains purification thing F3 (the 1g extract is equivalent to raw medicinal herbs 18.2g).Adopt carrageenin to cause the rat paw edema test model it is carried out the pharmacologically active screening.
Get 50 of Wistar rats, random packet, the experimental group rat gives water extraction method respectively and obtains extract F1, and the alkaline alcohol solution extraction method obtains extract F2 and macroporous resin separation and purification method obtains purification thing F3, wherein F1330mgkg
-1, F2 540mgkg
-1, F3 120mgkg
-1Positive drug contrast and solvent control rats give aspirin 100mgkg respectively
-1With with volume distilled water, 10mlkg
-1The volume gastric infusion, 12 hours (± 2 hours) 1 time, continuous 4 times.
Be injected in the subcutaneous inflammation that causes of the right back sufficient sole of the foot of rat with 1% carrageenin 0.1ml immediately after the last administration; Measure rat cause scorching before and cause 1,2,4,6,8 hour the sufficient sole of the foot volume in scorching back, calculate rat paw edema rate (%) and inhibitory rate of intumesce (%).
Experimental data represents that with meansigma methods ± standard deviation significance test adopts one factor analysis of variance between the group of measurement data, relatively adopts the t check in twos, and P＜0.05 is for there being significant difference, and P＜0.01 is for there being significant differences.Experimental result sees Table 1.
Experimental result, positive control medicine aspirin has showed tangible anti-inflammatory activity under institute's amount of reagent, with the matched group comparing difference significance and highly significant (P＜0.01 or 0.05) were arranged in 1-8 hour behind the medicine, behind medicine 2-8 hour rush hour of effect.
Test, the different process of the clinical equivalent dosage that tries has all showed anti-inflammatory activity in various degree after extracting the administration of Ainsliaea fragrans Champ. composition, wherein F2 and F3 behind medicine 2-8 hour with the matched group comparing difference significance and highly significant (P＜0.01 or 0.05) are arranged, F1 behind medicine 4-8 hour with the matched group comparing difference significance (P＜0.05) is arranged.Result of the test, the used dosage of Ainsliaea fragrans Champ. F3 component testing is lower, and antiinflammatory action is strong and stable.
Claims (7)
1, Ainsliaea fragrans Champ total flavone extract is characterized in that: content of total flavone is between 50%-95% in this extract.
2, Ainsliaea fragrans Champ. extractive of general flavone according to claim 1 is characterized in that: this extractive of general flavone can be made acceptable clinically preparation with pharmaceutically acceptable carrier.
3, a kind of preparation method of Ainsliaea fragrans Champ. extractive of general flavone as claimed in claim 1, it is characterized in that: it comprises the steps:
1. get drying, the Ainsliaea fragrans Champ. medical material of pulverizing is doubly measured the alcoholic solution that concentration is 5%-90% with 6-15, and 30-100 ℃ of reflux, extract, 2-4 time filtered, and filtrate concentrates;
2. get extract concentrated solution, remove impurity such as chlorophyll with petroleum ether extraction for 2-4 time, keep macroporous resin column absorption on the water layer; Or directly get the extract concentrated solution upper prop;
3. use 0%-15% alcoholic solution eluting macroporous resin column colourless to eluent, eluent is collected with the ethanol elution of 10%-95% in the back, reclaims ethanol, and evaporate to dryness is to the extractum shape, and vacuum drying is pulverized, ainsliaea fragrans champ-extract.
4, preparation method as claimed in claim 3 is characterized in that: the 2. described macroporous resin of step hangs down polar macroporous resin in being.
5, preparation method as claimed in claim 3 is characterized in that: the preferred D-101 resin of described macroporous resin.
6, the preparation method of Ainsliaea fragrans Champ. extractive of general flavone as claimed in claim 3 is characterized in that: the alcoholic solution of step described in 1. is for being that the weak caustic solutions such as ammonia, calcium hydroxide, sodium carbonate of 7.5-10 are prepared with pH value.
7, Ainsliaea fragrans Champ. extractive of general flavone and its preparation application in the medicine of preparation treatment acute and chronic cervicitis.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008102280694A CN101380347A (en) | 2008-10-14 | 2008-10-14 | Ainsliaea fragrans Champ total flavone extract and extraction method and use thereof |
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| CNA2008102280694A CN101380347A (en) | 2008-10-14 | 2008-10-14 | Ainsliaea fragrans Champ total flavone extract and extraction method and use thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105125612A (en) * | 2015-10-23 | 2015-12-09 | 云南云龙制药股份有限公司 | Preparation method and application of frangrant ainsliaea herb soft capsule |
| CN108014157A (en) * | 2017-12-31 | 2018-05-11 | 长沙湘资生物科技有限公司 | Application of the Ainsliaea fragrans champ extract in antibacterial-anti-inflammatory drug |
-
2008
- 2008-10-14 CN CNA2008102280694A patent/CN101380347A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105125612A (en) * | 2015-10-23 | 2015-12-09 | 云南云龙制药股份有限公司 | Preparation method and application of frangrant ainsliaea herb soft capsule |
| CN105125612B (en) * | 2015-10-23 | 2017-09-05 | 云南云龙制药股份有限公司 | A kind of preparation method and application of Ainsliaea fragrans Champ soft capsule |
| CN108014157A (en) * | 2017-12-31 | 2018-05-11 | 长沙湘资生物科技有限公司 | Application of the Ainsliaea fragrans champ extract in antibacterial-anti-inflammatory drug |
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Application publication date: 20090311 |