CN102093379A - Preparation method of high-purity bergapten and psoralen - Google Patents
Preparation method of high-purity bergapten and psoralen Download PDFInfo
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- CN102093379A CN102093379A CN2010106142120A CN201010614212A CN102093379A CN 102093379 A CN102093379 A CN 102093379A CN 2010106142120 A CN2010106142120 A CN 2010106142120A CN 201010614212 A CN201010614212 A CN 201010614212A CN 102093379 A CN102093379 A CN 102093379A
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- BGEBZHIAGXMEMV-UHFFFAOYSA-N COc1c(C=CC(O2)=O)c2cc2c1cc[o]2 Chemical compound COc1c(C=CC(O2)=O)c2cc2c1cc[o]2 BGEBZHIAGXMEMV-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention relates to a preparation method for separating high-purity bergapten and psoralen from ficus carica by using a high speed countercurrent chromatography method. The method comprises the following steps of: (1) preparing a proper solvent system, and standing still for layering to obtain an upper phase and a lower phase; (2) selecting the upper phase as a fixed phase and the lower phase as a flowing phase; filling a countercurrent chromatograph column with the fixed phase, and regulating the rotating speed of a host to be 600-1,000rpm; pumping the flowing phase into the column with a flowing speed of 0.5-5.0ml/min, and after dynamic balance of the whole system is established, introducing the sample through a sample introduction valve; and (3) receiving a target ingredient according to an ultraviolet spectrum of a detector, and then concentrating and crystallizing to obtain the finished product. The method is suitable for the preparation of various types of high speed countercurrent chromatographs as well as bergapten and psoralen of various contents and has the characteristics of large separation quantity, high recovery rate and simpleness and convenience for operation.
Description
Technical field
The invention belongs to the preparation field of coumarins composition, particularly relate to the preparation method of a kind of high purity bergapton and psoralene.
Background technology
Fructus Fici is Moraceae fig (Ficus Carica L), contains the amino acid of multiple needed by human body in the fruit of Fructus Fici, and contains multivitamins such as abundant VA and VC, and not only taste is sweet and refreshing, and has great pharmaceutical use.On the traditional Chinese medical science, Fructus Fici is mainly used in " strengthening the stomach and promoting bowel movement, subduing swelling and detoxicating " and treatment enteritis, dysentery, hemorrhoid etc.Leaf of Fig except that can treat hemorrhoid, pyogenic infections, pained, also have certain hypertension and antitumous effect.Fig leaf extract has extremely strong bacteriostatic activity, can be used as natural antiseptic agent and is used for food.Psoralene and bergapten are the main antipathogenic compositions in the fig leaf extract.Psoralene also can cause photosensitization, and injection or these materials for oral administration again with long wave ultraviolet or sun exposure, the red swelling of the skin at exposure place, pigment are increased, even epidermis thicken; Also can be used to treat vitiligo.
The structural formula of bergapton is as follows:
The structural formula of psoralene 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 bergapton and psoralene.This method overcomes the defective of traditional isolation technique, adopts high-speed countercurrent chromatography (HSCCC) highly purified bergapton of preparation and psoralene, 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 bergapton of the present invention and psoralene comprises:
(1) 1-5: 0.5-1.5: 1-5: the 1-10 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 bergapton and psoralene.
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: Fructus Fici 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: 1.5: 1: 1; 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 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: 3: 0.5: 1: 8; Engine speed 650rpm 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: 2: 0.5: 4: 2; Engine speed 600rpm 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: 1: 5: 9; Engine speed 700rpm 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: 5: 0.7: 1: 10; Engine speed 800rpm 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: 1.5: 3: 5; Engine speed 1000rpm 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 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.
High purity is meant purity 〉=98%, obtains bergapton and the pure product of psoralene through flash liberation, and purity is more than 98%.
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.
The target component that separates and collect is concentrated to and 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 bergapton and psoralene (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 bergapton and psoralene (reaching more than 98%) from the Fructus Fici 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 bergapton and psoralene 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 that 300mg Fructus Fici study is dissolved in that 10ml goes up mutually and stand-by in the solution of phase composite under the 10ml.Before the sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 950rpm, 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 bergapton and psoralene flow point, carries out crystallization after concentrated freeze-dried, and its HPLC purity reaches 98.5%.
Embodiment 2
Choose ethyl acetate-propyl carbinol-ethanol-water system separation and purification bergapton and psoralene 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 Fructus Fici 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 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 bergapton and psoralene flow point, carries out crystallization after concentrating, and its HPLC purity reaches 98.8%.
Embodiment 3
Choose butylacetate-n-propyl alcohol-ethanol-water system separation and purification bergapton and psoralene 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 Fructus Fici 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 bergapton and psoralene flow point, carries out crystallization after concentrated freeze-dried, and its HPLC purity reaches 98.2%.
Embodiment 4
Choose ethyl acetate-n-propyl alcohol-methanol-water system separation and purification bergapton and psoralene on half preparation type counter current chromatograph.It is 40 ℃ that experiment condition is fit to temperature, and earlier by 1: 1.5: 1: 1 volume ratio is 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 Fructus Fici 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 bergapton and psoralene flow point, carries out crystallization after concentrating, and its HPLC purity reaches 99.0%.
Embodiment 5
Choose ethyl acetate-propyl carbinol-ethanol-water system separation and purification bergapton and psoralene on half preparation type counter current chromatograph.It is 25 ℃ that experiment condition is fit to temperature, and earlier by 5: 0.5: 4: 2 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 Fructus Fici 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 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 bergapton and psoralene 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 bergapton and psoralene on half preparation type counter current chromatograph.It is 30 ℃ that experiment condition is fit to temperature, and earlier by 3: 1: 5: 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 Fructus Fici 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 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 bergapton and psoralene 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 bergapton and psoralene on half preparation type counter current chromatograph.It is 28 ℃ that experiment condition is fit to temperature, and earlier by 5: 0.7: 1: 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 Fructus Fici 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 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 bergapton and psoralene 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 bergapton and psoralene on half preparation type counter current chromatograph.It is 35 ℃ that experiment condition is fit to temperature, and earlier by 5: 1.5: 3: 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 Fructus Fici 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 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 bergapton and psoralene flow point, carries out crystallization after concentrating, and its HPLC purity reaches more than 98%.
Claims (10)
1. the preparation method of high purity bergapton and psoralene comprises:
(1) 1-5: 0.5-1.5: 1-5: the 1-10 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 bergapton and psoralene.
2. the preparation method of a kind of high purity bergapton according to claim 1 and psoralene is characterized in that: the preparation method of the sample that is advanced in the described step (2) is: Fructus Fici extract is dissolved in the upper and lower phase.
3. the preparation method of a kind of high purity bergapton according to claim 1 and psoralene, 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: 1.5: 1: 1; 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 bergapton according to claim 1 and psoralene, 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 3.0ml/min.
5. the preparation method of a kind of high purity bergapton according to claim 1 and psoralene, 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 0.5ml/min.
6. the preparation method of a kind of high purity bergapton according to claim 1 and psoralene, 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: 0.5: 4: 2; Engine speed 600rpm in the described step (2), the flow velocity that moving phase pumps in the post is 0.5ml/min.
7. the preparation method of a kind of high purity bergapton according to claim 1 and psoralene, 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: 1: 5: 9; Engine speed 700rpm in the described step (2), the flow velocity that moving phase pumps in the post is 1.0ml/min.
8. the preparation method of a kind of high purity bergapton according to claim 1 and psoralene, 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: 0.7: 1: 10; Engine speed 800rpm in the described step (2), the flow velocity that moving phase pumps in the post is 2.0ml/min.
9. the preparation method of a kind of high purity bergapton according to claim 1 and psoralene, 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: 1.5: 3: 5; Engine speed 1000rpm in the described step (2), the flow velocity that moving phase pumps in the post is 3.0ml/min.
10. the preparation method of a kind of high purity bergapton according to claim 1 and psoralene, 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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| CN112457324A (en) * | 2020-12-06 | 2021-03-09 | 淮安市厚沐医疗技术咨询中心 | Method for separating and purifying bergapten from clausena lansium |
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| CN112457324A (en) * | 2020-12-06 | 2021-03-09 | 淮安市厚沐医疗技术咨询中心 | Method for separating and purifying bergapten from clausena lansium |
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