CN102030733A - Method for preparing high-purity costuslactone and dehydrocostus lactone - Google Patents
Method for preparing high-purity costuslactone and dehydrocostus lactone Download PDFInfo
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- CN102030733A CN102030733A CN2010106142008A CN201010614200A CN102030733A CN 102030733 A CN102030733 A CN 102030733A CN 2010106142008 A CN2010106142008 A CN 2010106142008A CN 201010614200 A CN201010614200 A CN 201010614200A CN 102030733 A CN102030733 A CN 102030733A
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Abstract
The invention relates to a method for preparing high-purity costuslactone and dehydrocostus lactone through high-speed countercurrent chromatography, which comprises the following steps of: (1) preparing a proper solvent system, standing and demixing to obtain an upper phase and a lower phase; (2) selecting the upper phase as a fixed phase and the lower phase as a mobile phase, filling the fixed phase in a column of a countercurrent chromatograph, regulating the rotating speed of a main machine to be 600-1,000rpm, pumping the mobile phase into the column at a flow rate of 0.5-5.0ml/min, and sampling through a sampling valve after the whole system is dynamically balanced; and (3) receiving a target component according to an ultraviolet spectrum of a detector, concentrating, and crystallizing. The method is suitable for preparing the costuslactone and dehydrocostus lactone in various contents through various high-speed countercurrent chromatographs, and has the characteristics of large separation amount, high recovery rate, and simplicity and convenience of operation.
Description
Technical field
The invention belongs to the preparation field of the contained lactone of the banksia rose, the preparation method of particularly a kind of high purity costuslactone and dehydro-.
Background technology
The banksia rose is the dry root of the composite family Saussurea lappa Clarke platymiscium banksia rose (Auckland ia lappaDecne), and the effect of tool promoting the circulation of QI to relieve pain, strengthening the spleen to promote digestion is mainly used in treatment of diseases such as Peptic Ulcers, biliary colic, bronchial asthma clinically.The banksia rose mainly contains volatile oil, and its main component is Costunolide and dehydro-, and the two has relaxing smooth muscle and spasmolysis, is the main active ingredient of the banksia rose, also is the important indicator of banksia rose quality control.Lactone compositions such as costuslactone and the bronchoconstriction effect of going lactone volatile oil all can cause antihistamine, vagusstoff and bariumchloride, wherein stronger with the dihydrocostulactone effect.
The structural formula of costuslactone is as follows:
The structural formula of Costunolide is as follows:
High-speed countercurrent chromatography (High-SpeedCountercurrent Chromatography, HSCCC) be that a kind of successive that grew up in nearly 30 years need not the efficient of any solid support, liquid liquid distribution chromatography isolation technique fast, its principle is the centrifugal force that utilizes borded pile to produce when planetary motion, immiscible two-phase is constantly mixed, keep a phase (stationary phase) wherein simultaneously, utilize constant flow pump to import another phase (moving phase) continuously, the solute that enters borded pile with moving phase distributes between two-phase repeatedly, press the order of partition ratio, quilt is wash-out successively.The elder generation that allocation proportion is big in moving phase is by wash-out, otherwise, big back of allocation proportion in stationary phase by wash-out.When the traditional liquid chromatography technology amount of being prepared was separated, allocative efficiency was low, and solvent-oil ratio is big, and problems such as solid state adhesion body or carrier can bring that sample is adsorbed, loss and sex change.And HSCCC can guarantee higher peak type resolving power, have easy and simple to handle, fractional dose is big, sample is lossless, the separation efficiency height, the theoretical rate of recovery is 100%, and advantages such as favorable reproducibility and isolating environment mitigation now have been widely used in the preparation separation and the purifying of field chemical substances such as biology, medicine, environmental protection.
Summary of the invention
Technical problem to be solved by this invention provides the preparation method of a kind of high purity costuslactone and dehydro-.This method overcomes the defective of traditional isolation technique, adopts high-speed countercurrent chromatography (HSCCC) to prepare the method for high purity banksia rose ester and dehydro-, and this method is easy and simple to handle, rate of recovery height, and fractional dose is big.
The preparation method of a kind of high purity costuslactone of the present invention and dehydro-comprises:
(1) 1-5: 0.5-1: 1-5: the 5-10 mixing by volume of A component, B component, C component and D component is placed in the separating funnel, shakes up standing demix, after ready to balance 20-40 minute, upper and lower phase is separated, promptly get this solvent system; Wherein the A component is methyl acetate, ethyl acetate or butylacetate; The B component is n-propyl alcohol or propyl carbinol; The C component is ethanol or methyl alcohol; The D component is a water;
(2) in the selection being stationary phase mutually, is moving phase down mutually, is full of the counter current chromatograph pillar with stationary phase earlier, the adjusting engine speed is 600-1000rpm, the flow velocity of moving phase with 0.5-5.0ml/min pumped in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction;
(3) according to detector uv-spectrogram receiving target composition, with flow point concentrate, crystallization, obtain costuslactone and dehydro-.
Above-mentioned solvent system is preferably ethyl acetate-propyl carbinol-ethanol-water system.
The preparation method of the sample that is advanced in the described step (2) is: Radix Aucklandiae extract is dissolved in the upper and lower phase.
Solvent system in the described step (1) is ethyl acetate-n-propyl alcohol-methanol-water, and the volume ratio of this four component is followed successively by: 1: 1: 1: 7; Engine speed 850rpm in the described step (2), the flow velocity that moving phase pumps in the post is 5.0ml/min.
Solvent system in the described step (1) is methyl acetate-n-propyl alcohol-alcohol-water, and the volume ratio of this four component is followed successively by: 4: 0.8: 2: 6; Engine speed 950rpm in the described step (2), the flow velocity that moving phase pumps in the post is 0.5ml/min.
Solvent system in the described step (1) is ethyl acetate-propyl carbinol-alcohol-water, and the volume ratio of this four component is followed successively by: 3: 0.5: 1: 8; Engine speed 650rpm in the described step (2), the flow velocity that moving phase pumps in the post is 3.0ml/min.
Solvent system in the described step (1) is ethyl acetate-propyl carbinol-alcohol-water, and the volume ratio of this four component is followed successively by: 1: 0.7: 2: 9; Engine speed 600rpm in the described step (2), the flow velocity that moving phase pumps in the post is 1.0ml/min.
Solvent system in the described step (1) is ethyl acetate-propyl carbinol-alcohol-water, and the volume ratio of this four component is followed successively by: 2: 0.8: 3: 1; Engine speed 700rpm in the described step (2), the flow velocity that moving phase pumps in the post is 2.0ml/min.
Solvent system in the described step (1) is ethyl acetate-propyl carbinol-alcohol-water, and the volume ratio of this four component is followed successively by: 5: 0.5: 4: 7; Engine speed 800rpm in the described step (2), the flow velocity that moving phase pumps in the post is 3.0ml/min.Solvent system in the described step (1) is ethyl acetate-propyl carbinol-alcohol-water, and the volume ratio of this four component is followed successively by: 4: 1: 4: 5; Engine speed 1000rpm in the described step (2), the flow velocity that moving phase pumps in the post is 4.0ml/min.
Solvent system in the described step (1) is butylacetate-n-propyl alcohol-alcohol-water, and the volume ratio of this four component is followed successively by: 4: 1: 1: 6; Engine speed 750rpm in the described step (2), the flow velocity that moving phase pumps in the post is 4.0ml/min.
According to solubility constant, do not destroying under the system equilibrated situation, regulate A, B, C, the volume ratio of D four components.
Experiment condition is fit to temperature 20-40 ℃, and in the said temperature scope, when temperature was higher, appearance time slightly shifted to an earlier date, and separating effect changes little, and peak shape is not had much influences.
Engine speed and flow velocity need be controlled within the specific limits, by volume solvent system are placed separating funnel, shake up standing demix.Behind the ready to balance certain hour, upper and lower phase is separated, adopt the TBE-300B high-speed counter-current chromatograph, this type column volume is 300ml, and the sample introduction circle is 20ml, is furnished with the TBP-50A pump, TBD-23 detector and N2000 chromatographic working station.Before the sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 600-1000rpm, with the flow velocity of 0.5-5.0ml/min moving phase is pumped in the post.
High purity is meant purity 〉=98%; The target component that separates and collect is concentrated to and will carries out crystallization again after the certain purity and obtain monomer.
The present invention has adopted the high speed adverse current chromatogram isolation technique to overcome solid-state upholder or carrier irreversible adsorption, loss and sex change, make the high theory of the separated object rate of recovery reach 100%, the present invention is actual to be reached more than 95%, again because adopt preferred solvent system, the processing condition of control experiment condition temperature, adjustment engine speed and flow velocity, can high efficiencyly separate, obtain highly purified costuslactone and dehydro-(reaching more than 98%).
Beneficial effect
1, the present invention has adopted the high speed adverse current chromatogram isolation technique, guarantees higher peak shape resolution, and fractional dose is big, the rate of recovery is high, isolating environment relaxes, save solvent, easy and simple to handle.
2, the present invention is fit to obtain highly purified costuslactone and dehydro-(reaching more than 98%) from the Radix Aucklandiae extract of various technology approach preparations.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Choose methyl acetate-n-propyl alcohol-ethanol-water system separation and purification costuslactone constituents on half preparation type counter current chromatograph.It is 25 ℃ that experiment condition is fit to temperature, and earlier by 4: 0.8: 2: 6 volume ratios are disposed at above-mentioned solvent composition branch in the separating funnel, standing demix after the jolting.Ready to balance after for some time separates upper and lower phase.Adopt half preparation type counter current chromatograph, be furnished with the tetrafluoroethylene post, the 20ml sampling valve, column volume is 300ml, is furnished with the TBP-50A pump, TBD-23 detector and N2000 chromatographic working station.Take by weighing 100mg banksia rose study be dissolved in 10ml go up mutually with 10ml under stand-by in the solution of solution composition mutually.Before the sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 950rpm, with the flow velocity of 0.5ml/min moving phase is pumped in the post; After treating that whole system is set up running balance, by the sampling valve sample introduction, then according to the detector uv-spectrogram, the receiving target composition obtains costuslactone and dehydro-flow point, carries out crystallization after concentrated freeze-dried, and its HPLC purity reaches 98.8%.
Embodiment 2
Choose ethyl acetate-propyl carbinol-ethanol-water system separation and purification costuslactone constituents on half preparation type counter current chromatograph.It is 30 ℃ that experiment condition is fit to temperature, and earlier by 3: 0.5: 1: 8 volume ratios are disposed at above-mentioned solvent composition branch in the separating funnel, standing demix after the jolting.Ready to balance after for some time separates upper and lower phase.Adopt half preparation type counter current chromatograph, be furnished with the tetrafluoroethylene post, the 20ml sampling valve, column volume is 300ml, is furnished with the TBP-50A pump, TBD-23 detector and N2000 chromatographic working station.Take by weighing 150mg banksia rose study be dissolved in 10ml go up mutually with 10ml under stand-by in the solution mutually.Before the sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 650rpm, with the flow velocity of 3.0ml/min moving phase is pumped in the post; After treating that whole system is set up running balance, by the sampling valve sample introduction, then according to the detector uv-spectrogram, the receiving target composition obtains costuslactone and dehydro-flow point, carries out crystallization after concentrating, and its HPLC purity reaches 98.5%.
Embodiment 3
Choose butylacetate-n-propyl alcohol-ethanol-water system separation and purification costuslactone constituents on half preparation type counter current chromatograph.It is 22 ℃ that experiment condition is fit to temperature, and earlier by 4: 1: 1: 6 volume ratios are disposed at above-mentioned solvent composition branch in the separating funnel, standing demix after the jolting.Ready to balance after for some time separates upper and lower phase.Adopt half preparation type counter current chromatograph, be furnished with the tetrafluoroethylene post, the 20ml sampling valve, column volume is 300ml, is furnished with the TBP-50A pump, TBD-23 detector and N2000 chromatographic working station.Take by weighing 150mg banksia rose study be dissolved in 10ml go up mutually with 10ml under stand-by in the solution mutually.Before the sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 750rpm, with the flow velocity of 4.0ml/min moving phase is pumped in the post; After treating that whole system is set up running balance, by the sampling valve sample introduction, then according to the detector uv-spectrogram, the receiving target composition obtains costuslactone and dehydro-flow point, carries out crystallization after concentrated freeze-dried, and its HPLC purity reaches 98.9%.
Embodiment 4
Choose ethyl acetate-n-propyl alcohol-methanol-water system separation and purification costuslactone constituents on half preparation type counter current chromatograph.It is 40 ℃ that experiment condition is fit to temperature, and earlier by 1: 1: 1: 7 volume ratios are disposed at above-mentioned solvent composition branch in the separating funnel, standing demix after the jolting.Ready to balance after for some time separates upper and lower phase.Adopt half preparation type counter current chromatograph, be furnished with the tetrafluoroethylene post, the 20ml sampling valve, column volume is 300ml, is furnished with the TBP-50A pump, TBD-23 detector and N2000 chromatographic working station.Take by weighing 100mg banksia rose study be dissolved in 10ml go up mutually with 10ml under stand-by in the solution mutually.Before the sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 850rpm, with the flow velocity of 5.0ml/min moving phase is pumped in the post; After treating that whole system is set up running balance, by the sampling valve sample introduction, then according to the detector uv-spectrogram, the receiving target composition obtains costuslactone and dehydro-flow point, carries out crystallization after concentrating, and its HPLC purity reaches 98.2%.
Embodiment 5
Choose ethyl acetate-propyl carbinol-ethanol-water system separation and purification costuslactone constituents on half preparation type counter current chromatograph.It is 25 ℃ that experiment condition is fit to temperature, and earlier by 1: 0.7: 2: 9 volume ratios are disposed at above-mentioned solvent composition branch in the separating funnel, standing demix after the jolting.Ready to balance after for some time separates upper and lower phase.Adopt half preparation type counter current chromatograph, be furnished with the tetrafluoroethylene post, the 20ml sampling valve, column volume is 300ml, is furnished with the TBP-50A pump, TBD-23 detector and N2000 chromatographic working station.Take by weighing 150mg banksia rose study be dissolved in 10ml go up mutually with 10ml under stand-by in the solution mutually.Before the sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 600rpm, with the flow velocity of 1.0ml/min moving phase is pumped in the post; After treating that whole system is set up running balance, by the sampling valve sample introduction, then according to the detector uv-spectrogram, the receiving target composition obtains costuslactone and dehydro-flow point, carries out crystallization after concentrating, and its HPLC purity reaches more than 98%.
Embodiment 6
Choose ethyl acetate-propyl carbinol-ethanol-water system separation and purification costuslactone constituents on half preparation type counter current chromatograph.It is 28 ℃ that experiment condition is fit to temperature, and earlier by 2: 0.8: 3: 10 volume ratios are disposed at above-mentioned solvent composition branch in the separating funnel, standing demix after the jolting.Ready to balance after for some time separates upper and lower phase.Adopt half preparation type counter current chromatograph, be furnished with the tetrafluoroethylene post, the 20ml sampling valve, column volume is 300ml, is furnished with the TBP-50A pump, TBD-23 detector and N2000 chromatographic working station.Take by weighing 150mg banksia rose study be dissolved in 10ml go up mutually with 10ml under stand-by in the solution mutually.Before the sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 700rpm, with the flow velocity of 2.0ml/min moving phase is pumped in the post; After treating that whole system is set up running balance, by the sampling valve sample introduction, then according to the detector uv-spectrogram, the receiving target composition obtains costuslactone and dehydro-flow point, carries out crystallization after concentrating, and its HPLC purity reaches more than 98%.
Embodiment 7
Choose ethyl acetate-propyl carbinol-ethanol-water system separation and purification costuslactone constituents on half preparation type counter current chromatograph.It is 35 ℃ that experiment condition is fit to temperature, and earlier by 5: 0.5: 4: 7 volume ratios are disposed at above-mentioned solvent composition branch in the separating funnel, standing demix after the jolting.Ready to balance after for some time separates upper and lower phase.Adopt half preparation type counter current chromatograph, be furnished with the tetrafluoroethylene post, the 20ml sampling valve, column volume is 300ml, is furnished with the TBP-50A pump, TBD-23 detector and N2000 chromatographic working station.Take by weighing 150mg banksia rose study be dissolved in 10ml go up mutually with 10ml under stand-by in the solution mutually.Before the sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 800rpm, with the flow velocity of 3.0ml/min moving phase is pumped in the post; After treating that whole system is set up running balance, by the sampling valve sample introduction, then according to the detector uv-spectrogram, the receiving target composition obtains costuslactone and dehydro-flow point, carries out crystallization after concentrating, and its HPLC purity reaches more than 98%.
Embodiment 8
Choose ethyl acetate-propyl carbinol-ethanol-water system separation and purification costuslactone constituents on half preparation type counter current chromatograph.It is 38 ℃ that experiment condition is fit to temperature, and earlier by 4: 1: 4: 5 volume ratios are disposed at above-mentioned solvent composition branch in the separating funnel, standing demix after the jolting.Ready to balance after for some time separates upper and lower phase.Adopt half preparation type counter current chromatograph, be furnished with the tetrafluoroethylene post, the 20ml sampling valve, column volume is 300ml, is furnished with the TBP-50A pump, TBD-23 detector and N2000 chromatographic working station.Take by weighing 150mg banksia rose study be dissolved in 10ml go up mutually with 10ml under stand-by in the solution mutually.Before the sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 1000rpm, with the flow velocity of 4.0ml/min moving phase is pumped in the post; After treating that whole system is set up running balance, by the sampling valve sample introduction, then according to the detector uv-spectrogram, the receiving target composition obtains costuslactone and dehydro-flow point, carries out crystallization after concentrating, and its HPLC purity reaches more than 98%.
Claims (10)
1. the preparation method of high purity costuslactone and dehydro-comprises:
(1) 1-5: 0.5-1: 1-5: the 5-10 mixing by volume of A component, B component, C component and D component is placed in the separating funnel, shakes up standing demix, after ready to balance 20-40 minute, upper and lower phase is separated, promptly get solvent system; Wherein the A component is methyl acetate, ethyl acetate or butylacetate; The B component is n-propyl alcohol or propyl carbinol; The C component is ethanol or methyl alcohol; The D component is a water;
(2) in the selection being stationary phase mutually, is moving phase down mutually, is full of the counter current chromatograph pillar with stationary phase earlier, the adjusting engine speed is 600-1000rpm, the flow velocity of moving phase with 0.5-5.0ml/min pumped in the post, treat that whole system is set up running balance after, by the sampling valve sample introduction;
(3) according to detector uv-spectrogram receiving target composition, with flow point concentrate, crystallization, obtain costuslactone and dehydro-.
2. the preparation method of a kind of high purity costuslactone according to claim 1 and dehydro-is characterized in that: the preparation method of the sample that is advanced in the described step (2) is: Radix Aucklandiae extract is dissolved in the upper and lower phase.
3. the preparation method of a kind of high purity costuslactone according to claim 1 and dehydro-, it is characterized in that: the solvent system in the described step (1) is ethyl acetate-n-propyl alcohol-methanol-water, and the volume ratio of this four component is followed successively by: 1: 1: 1: 7; Engine speed 850rpm in the described step (2), the flow velocity that moving phase pumps in the post is 5.0ml/min.
4. the preparation method of a kind of high purity costuslactone according to claim 1 and dehydro-, it is characterized in that: the solvent system in the described step (1) is methyl acetate-n-propyl alcohol-alcohol-water, and the volume ratio of this four component is followed successively by: 4: 0.8: 2: 6; Engine speed 950rpm in the described step (2), the flow velocity that moving phase pumps in the post is 0.5ml/min.
5. the preparation method of a kind of high purity costuslactone according to claim 1 and dehydro-, it is characterized in that: the solvent system in the described step (1) is ethyl acetate-propyl carbinol-alcohol-water, and the volume ratio of this four component is followed successively by: 3: 0.5: 1: 8; Engine speed 650rpm in the described step (2), the flow velocity that moving phase pumps in the post is 3.0ml/min.
6. the preparation method of a kind of high purity costuslactone according to claim 1 and dehydro-, it is characterized in that: the solvent system in the described step (1) is ethyl acetate-propyl carbinol-alcohol-water, and the volume ratio of this four component is followed successively by: 1: 0.7: 2: 9; Engine speed 600rpm in the described step (2), the flow velocity that moving phase pumps in the post is 1.0ml/min.
7. the preparation method of a kind of high purity costuslactone according to claim 1 and dehydro-, it is characterized in that: the solvent system in the described step (1) is ethyl acetate-propyl carbinol-alcohol-water, and the volume ratio of this four component is followed successively by: 2: 0.8: 3: 1; Engine speed 700rpm in the described step (2), the flow velocity that moving phase pumps in the post is 2.0ml/min.
8. the preparation method of a kind of high purity costuslactone according to claim 1 and dehydro-, it is characterized in that: the solvent system in the described step (1) is ethyl acetate-propyl carbinol-alcohol-water, and the volume ratio of this four component is followed successively by: 5: 0.5: 4: 7; Engine speed 800rpm in the described step (2), the flow velocity that moving phase pumps in the post is 3.0ml/min.
9. the preparation method of a kind of high purity costuslactone according to claim 1 and dehydro-, it is characterized in that: the solvent system in the described step (1) is ethyl acetate-propyl carbinol-alcohol-water, and the volume ratio of this four component is followed successively by: 4: 1: 4: 5; Engine speed 1000rpm in the described step (2), the flow velocity that moving phase pumps in the post is 4.0ml/min.
10. the preparation method of a kind of high purity costuslactone according to claim 1 and dehydro-, it is characterized in that: the solvent system in the described step (1) is butylacetate-n-propyl alcohol-alcohol-water, and the volume ratio of this four component is followed successively by: 4: 1: 1: 6; Engine speed 750rpm in the described step (2), the flow velocity that moving phase pumps in the post is 4.0ml/min.
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| CN201010614200.8A CN102030733B (en) | 2010-12-30 | 2010-12-30 | The preparation method of a kind of high purity costuslactone and dehydro-α-curcumene |
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| CN201010614200.8A CN102030733B (en) | 2010-12-30 | 2010-12-30 | The preparation method of a kind of high purity costuslactone and dehydro-α-curcumene |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327026A (en) * | 2014-10-15 | 2015-02-04 | 西南民族大学 | Method of extracting and separating costunolide and dehydrocostuslactone |
| CN104876900A (en) * | 2015-05-18 | 2015-09-02 | 徐州医学院 | Method for extracting, separating and purifying costunolide and dehydrocostus lactone from elecampane |
| CN105315246A (en) * | 2015-04-16 | 2016-02-10 | 霍秀菊 | Method for separating and purifying costunolide and dehydrocostus lactone from costustoot |
| CN106138060A (en) * | 2016-08-14 | 2016-11-23 | 武晓丹 | The pharmaceutical composition of a kind of moclobemide and medical usage thereof |
| CN106279087A (en) * | 2016-08-14 | 2017-01-04 | 武晓丹 | A kind of compound and preparation method thereof, medical applications |
| CN106317003A (en) * | 2016-08-14 | 2017-01-11 | 武晓丹 | Furazolidone pharmaceutical composition and biological and medicinal applications thereof |
| CN106317002A (en) * | 2016-08-14 | 2017-01-11 | 武晓丹 | Natural compound separated from sargentgloryvine stem, preparation method and application thereof |
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2010
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| 李躬行，等，: "高速逆流色谱法分离木香中的木香烃内酯和去氢木香内酯", 《华西药学杂志》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327026A (en) * | 2014-10-15 | 2015-02-04 | 西南民族大学 | Method of extracting and separating costunolide and dehydrocostuslactone |
| CN104327026B (en) * | 2014-10-15 | 2016-06-15 | 西南民族大学 | A kind of method extracting separation costunolide and Decahydro-3,6,9-tris(methylene)azuleno[4,5-b |
| CN105315246A (en) * | 2015-04-16 | 2016-02-10 | 霍秀菊 | Method for separating and purifying costunolide and dehydrocostus lactone from costustoot |
| CN104876900A (en) * | 2015-05-18 | 2015-09-02 | 徐州医学院 | Method for extracting, separating and purifying costunolide and dehydrocostus lactone from elecampane |
| CN106138060A (en) * | 2016-08-14 | 2016-11-23 | 武晓丹 | The pharmaceutical composition of a kind of moclobemide and medical usage thereof |
| CN106279087A (en) * | 2016-08-14 | 2017-01-04 | 武晓丹 | A kind of compound and preparation method thereof, medical applications |
| CN106317003A (en) * | 2016-08-14 | 2017-01-11 | 武晓丹 | Furazolidone pharmaceutical composition and biological and medicinal applications thereof |
| CN106317002A (en) * | 2016-08-14 | 2017-01-11 | 武晓丹 | Natural compound separated from sargentgloryvine stem, preparation method and application thereof |
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| CN102030733B (en) | 2015-08-05 |
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