CN102180933A - Preparation method of skunk bugbane monomer components - Google Patents
Preparation method of skunk bugbane monomer components Download PDFInfo
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- CN102180933A CN102180933A CN2011100748273A CN201110074827A CN102180933A CN 102180933 A CN102180933 A CN 102180933A CN 2011100748273 A CN2011100748273 A CN 2011100748273A CN 201110074827 A CN201110074827 A CN 201110074827A CN 102180933 A CN102180933 A CN 102180933A
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- rattletop
- cimicifugoside
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- chloroform
- methanol
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Abstract
The invention relates to a preparation method of skunk bugbane monomer components, which comprises the following steps: extracting drug skunk bugbane with a 60-80% alcoholic solution, concentrating the extracting solution, adding alkali to the concentrated solution to regulate the pH value to 8-11, extracting with an organic solvent, carrying out silicagel column chromatography on the extract, eluting with chloroform-methanol, collecting the fraction crude extract, and separating the crude extract by a high-speed countercurrent chromatography to obtain the monomers skunk bugbane glycoside A, skunk bugbane glycoside B, skunk bugbane glycoside C, skunk bugbane glycoside D and cimigenol xyloside. The purity of the products obtained by the method provided by the invention is higher than 98%.
Description
Technical field:
The present invention relates to a kind of preparation method of rattletop monomer component, relate in particular to a kind of high-speed countercurrent chromatography of using and from the rattletop crude extract, separate the method for preparing the rattletop monomer component.
Background technology:
Rattletop is Ranunculaceae Rattleroot (Cimicifugeae S.I.) plant, comprises big three leaf rattletops (Cimicifugaheracleifolia Kom.), Xingan's rattletop (Cimicifuga dahurica (Turcz.) Maxim.) and rattletop (Cimicifuga foetida L.).Rattletop family plant is many is used as medicine with underground part.Rattletop has the promoting eruption of delivering, and is clearing heat and detoxicating, and the effect of elevate a turnable ladder yang-energy is used for headache due to pathogenic wind-heat, dentalgia, and aphtha, swelling and pain in the throat, measles without adequate eruption, the sun poison is sent out spot, prolapse of the anus, diseases such as uterine prolapse.The rattletop rhizome contains Cimiside (Cimi-cifugoside), Cimigenol xyloside (Cimigenol xyloside), Whitfield's ointment (Salicylic acid), tannin (Tannin), resin (Resin), coffic acid (Caffeic acid), forulic acid (Ferulic acid), isoferulic acid (Isoferulic acid), cimicifugine (Cimicifu-gine) etc.Xingan's rattletop rhizome contains macrotin (Cimitin), glucoside, alkaloid (Alkaloid), carbohydrate, resin, isoferulic acid, forulic acid and coffic acid, still emanate β-Gu Zaichun (β-Sitosterol), cimigenol (Cimigenol), Cimigenol xyloside.Big three leaf rattletops contain Cimiside, macrotin, Cimigenol xyloside, alkaloid, isoferulic acid etc.
Studies show that in recent years, main active ingredient is a saponins compound in the rattletop.The total saponins of rattletop can improve castrated rats serum estradiol level, and luteotropic hormone concentration is reduced, and can suppress the osteoporosis and the climacteric syndrome that cause owing to endocrine regulation, estrogen deficiency.The preparation of rattletop saponins monomer component has great importance for exploitation, the quality control of rattletop medicine series.
At present, mostly the separation method of existing rattletop monomer component is that silicagel column and gel column combine, and method is loaded down with trivial details, poor reproducibility, and preparation amount is less, and specificity is low.As " chemical ingredients of Chinese medicine rattletop ", adopt the preparation of silicagel column and Sephardex LH-20 column purification, preparation amount is less, operates complicated.
High-speed countercurrent chromatography (HSCCC) is that a kind of liquid liquid of any carrier that do not need distributes isolation technique, utilize one-way fluid kinetic balance principle, based on sample relatively moving and the difference of partition ratio and realize separating in the immiscible two-phase in the rotating screw pipe, its separation efficiency and speed can compare favourably with HPLC.HSCCC separation efficiency height, there be not absorption and the pollution of carrier to sample in the product purity height, and preparation amount is big and solvent consumption is few, simple to operate, can isolate specific component from extremely complicated mixture.It is different with general stratographic separate mode, is particularly useful for making the separation of level, has been widely used in the separation and purification process of Chinese medicine and natural product.
Summary of the invention:
The technical problem to be solved in the present invention provides a kind of preparation method of rattletop monomer component.
The present invention is achieved by the following technical solutions:
A kind of preparation method of rattletop monomer component is characterized in that may further comprise the steps:
(1) the rattletop pulverizing medicinal materials is extracted 1-3 time with the 60-80% alcoholic solution, each 1-2h, concentrating under reduced pressure obtains concentrated solution;
(2) concentrated solution is added adjusting PH with base to 8-11, use organic solvent extraction, the extract by adopting silica gel column chromatography is used the chloroform-methanol wash-out, collects the flow point concentrate drying and obtains crude extract;
(3) crude extract application high speed adverse current chromatogram separates, the solvent systems that hexane-chloroform-methanol-water is formed fully leaves standstill after the vibration in separating funnel, layering, on be stationary phase mutually, be moving phase mutually down, collect according to the detector ultraviolet spectrogram, merge identical component, obtain cimicifugoside A, cimicifugoside B, cimicifugoside C, cimicifugoside D and cimigenol xyloside monomer.
Optional ultrasonic extraction of extracting method or refluxing extraction in the described step (1), alcoholic solution is an ethanolic soln.
Organic solvent is a propyl carbinol in the described step (2), and the volume ratio of chloroform-methanol is 5-7: 2.
The volume ratio of hexane-chloroform-methanol in the described step (3)-water is 2-3: 4-7: 5-8: 1-4.
The invention has the advantages that:
1, step is few, weak point consuming time, and the yield height is easy to large-scale production;
2, operation is simple, is easy to control, and obtains multiple product simultaneously, raw material availability height, separation efficiency height;
3, the present invention adopts high-speed countercurrent chromatography, does not have reversible adsorption, the sample free of losses;
4, the highly purified monomer component for preparing of the present invention can be used as reference substance and uses.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1
With the rattletop pulverizing medicinal materials with 5 times of amounts (V/W), 60% ethanolic soln supersound extraction 2 times, each 1h, be evaporated to no alcohol and obtain concentrated solution, concentrated solution adds adjusting PH with base to 10, uses n-butanol extraction, reclaims propyl carbinol, the extract by adopting silica gel column chromatography, use the chloroform-methanol eluant solution, the volume ratio of chloroform-methanol is 7: 2, collects the flow point concentrate drying and obtains crude extract; With hexane, chloroform, methyl alcohol, water is 2: 5: 6 by volume: 2 configurations, place separating funnel fully to leave standstill after the vibration, layering, on be stationary phase mutually, be moving phase mutually down, be that sampling valve is in the sample introduction state, stationary phase is filled the chromatography column of counter current chromatograph with the flow velocity of 10ml/min, the opening speed controller, make the rotation of spiral tube clockwise direction, when the chromatographic instrument rotating speed is 850r/min, with the flow velocity is that 2.5ml/min pumps into moving phase, with crude extract phased soln down, and by the sampling valve sample introduction, each sample size is 150mg, collect according to the detector ultraviolet spectrogram, merge identical component, obtain cimicifugoside A, cimicifugoside B, cimicifugoside C, cimicifugoside D and cimigenol xyloside monomer, detect cimicifugoside A through HPLC, cimicifugoside B, cimicifugoside C, cimicifugoside D, the purity of cimigenol xyloside is respectively 98.2%, 98.0%, 98.3%, 98.4%, 98.5%.
Embodiment 2
With the rattletop pulverizing medicinal materials with 8 times of amounts (V/W), 80% ethanolic soln refluxing extraction 1 time, each 2h, be evaporated to no alcohol and obtain concentrated solution, concentrated solution adds adjusting PH with base to 8, uses n-butanol extraction, reclaims propyl carbinol, the extract by adopting silica gel column chromatography, use the chloroform-methanol eluant solution, the volume ratio of chloroform-methanol is 3: 1, collects the flow point concentrate drying and obtains crude extract; With hexane, chloroform, methyl alcohol, water is 2: 4: 5 by volume: 4 configurations, place separating funnel fully to leave standstill after the vibration, layering, on be stationary phase mutually, be moving phase mutually down, be that sampling valve is in the sample introduction state, stationary phase is filled the chromatography column of counter current chromatograph with the flow velocity of 10ml/min, the opening speed controller, make the rotation of spiral tube clockwise direction, when the chromatographic instrument rotating speed is 750r/min, with the flow velocity is that 2.5ml/min pumps into moving phase, with crude extract phased soln down, and by the sampling valve sample introduction, each sample size is 200mg, collect according to the detector ultraviolet spectrogram, merge identical component, obtain cimicifugoside A, cimicifugoside B, cimicifugoside C, cimicifugoside D and cimigenol xyloside monomer, detect cimicifugoside A through HPLC, cimicifugoside B, cimicifugoside C, cimicifugoside D, the purity of cimigenol xyloside is respectively 98.3%, 98.2%, 98.1%, 98.2%, 98.3%.
Embodiment 3
With the rattletop pulverizing medicinal materials with 6 times of amounts (V/W), 70% ethanolic soln refluxing extraction 3 times, each 1h, be evaporated to no alcohol and obtain concentrated solution, concentrated solution adds adjusting PH with base to 11, uses n-butanol extraction, reclaims propyl carbinol, the extract by adopting silica gel column chromatography, use the chloroform-methanol eluant solution, the volume ratio of chloroform-methanol is 5: 2, collects the flow point concentrate drying and obtains crude extract; With hexane, chloroform, methyl alcohol, water is 3: 7: 8 by volume: 2 configurations, place separating funnel fully to leave standstill after the vibration, layering, on be stationary phase mutually, be moving phase mutually down, be that sampling valve is in the sample introduction state, stationary phase is filled the chromatography column of counter current chromatograph with the flow velocity of 10ml/min, the opening speed controller, make the rotation of spiral tube clockwise direction, when the chromatographic instrument rotating speed is 950r/min, with the flow velocity is that 2.5ml/min pumps into moving phase, with crude extract phased soln down, and by the sampling valve sample introduction, each sample size is 200mg, collect according to the detector ultraviolet spectrogram, merge identical component, obtain cimicifugoside A, cimicifugoside B, cimicifugoside C, cimicifugoside D and cimigenol xyloside monomer, detect cimicifugoside A through HPLC, cimicifugoside B, cimicifugoside C, cimicifugoside D, the purity of cimigenol xyloside is respectively 98.0%, 98.2%, 98.4%, 98.4%, 98.3%.
Claims (4)
1. the preparation method of a rattletop monomer component is characterized in that may further comprise the steps:
(1) the rattletop pulverizing medicinal materials is extracted 1-3 time with the 60-80% alcoholic solution, each 1-2h, concentrating under reduced pressure obtains concentrated solution;
(2) concentrated solution is added adjusting PH with base to 8-11, use organic solvent extraction, the extract by adopting silica gel column chromatography is used the chloroform-methanol wash-out, collects the flow point concentrate drying and obtains crude extract;
(3) crude extract application high speed adverse current chromatogram separates, the solvent systems that hexane-chloroform-methanol-water is formed fully leaves standstill after the vibration in separating funnel, layering, on be stationary phase mutually, be moving phase mutually down, collect according to the detector ultraviolet spectrogram, merge identical component, obtain cimicifugoside A, cimicifugoside B, cimicifugoside C, cimicifugoside D and cimigenol xyloside monomer.
2. according to the preparation method of a kind of rattletop monomer component described in the claim 1, it is characterized in that optional ultrasonic extraction of extracting method or refluxing extraction in the described step (1), alcoholic solution is an ethanolic soln.
3. according to the preparation method of a kind of rattletop monomer component described in the claim 1, it is characterized in that organic solvent is a propyl carbinol in the described step (2), the volume ratio of chloroform-methanol is 5-7: 2.
4. according to the preparation method of a kind of rattletop monomer component described in the claim 1, it is characterized in that the volume ratio of hexane-chloroform-methanol in the described step (3)-water is 2-3: 4-7: 5-8: 1-4.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100748273A CN102180933A (en) | 2011-03-28 | 2011-03-28 | Preparation method of skunk bugbane monomer components |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100748273A CN102180933A (en) | 2011-03-28 | 2011-03-28 | Preparation method of skunk bugbane monomer components |
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| CN102180933A true CN102180933A (en) | 2011-09-14 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105497169A (en) * | 2016-01-06 | 2016-04-20 | 南京海源中药饮片有限公司 | Method for extracting phenolic acid effective constituents of rhizome cimicifugae |
| CN107281206A (en) * | 2016-03-30 | 2017-10-24 | 南京惠宝生物医药有限公司 | Black cohosh root glycosides is preparing the application in preventing and treating senile dementia medicine |
-
2011
- 2011-03-28 CN CN2011100748273A patent/CN102180933A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105497169A (en) * | 2016-01-06 | 2016-04-20 | 南京海源中药饮片有限公司 | Method for extracting phenolic acid effective constituents of rhizome cimicifugae |
| CN107281206A (en) * | 2016-03-30 | 2017-10-24 | 南京惠宝生物医药有限公司 | Black cohosh root glycosides is preparing the application in preventing and treating senile dementia medicine |
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Application publication date: 20110914 |