CN1817351A - Production of variolaria amra medicinal extract and its medicinal preparation - Google Patents
Production of variolaria amra medicinal extract and its medicinal preparation Download PDFInfo
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- CN1817351A CN1817351A CN 200510023904 CN200510023904A CN1817351A CN 1817351 A CN1817351 A CN 1817351A CN 200510023904 CN200510023904 CN 200510023904 CN 200510023904 A CN200510023904 A CN 200510023904A CN 1817351 A CN1817351 A CN 1817351A
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- herba ixeritis
- ixeritis sonchifoliae
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Abstract
A process for preparing the medicinal extract of ixeris herb includes such steps as adding alcohol, reflux extracting, decocting dregs, filtering, concentrating, depositing in alcohol, filtering, concentrating, adsorbing by macroreticular resin, eluting with water and alcohol, and vacuum concentrating. It can be used to prepare injection, tablet, capsule, oral liquid, or particles.
Description
Technical field
The present invention relates to the preparation method and the pharmaceutical preparation thereof of Herba Ixeritis Sonchifoliae medicinal extract.Have and relate to based on the preparation method of the medicinal extract of flavone compound and adenosine and be the Herba Ixeritis Sonchifoliae pharmaceutical preparation of active component with the medicinal extract that this method obtains.
Background technology
Herba Ixeritis Sonchifoliae, have another name called Herba Ixeritis Sonchifoliae, have promoting blood circulation and stopping pain, heat clearing away blood stasis dispelling, expansion coronary vasodilator, improve effects such as myocardium blood oxygen is supplied, increase fibrinoclase activity, inhibition thrombosis, its main medicinal ingredient is flavone and adenosine, wherein the highest with flavonoid content especially, the Herba Ixeritis Sonchifoliae pharmaceutical preparation of report is to be raw material with the Herba Ixeritis Sonchifoliae at present, carry out the simple preliminary various pharmaceutical preparatioies such as prepared aqueous injection in back and tablet of extracting, be mainly used in treatment cerebral thrombosis, coronary heart disease, angina pectoris, optic atrophy and fundus oculi disease.In the existing Herba Ixeritis Sonchifoliae pharmaceutical preparation production technology, exist the low and defectives such as extraction process is complicated, impurity content height of Herba Ixeritis Sonchifoliae medicinal ingredient extraction ratio.For example the preparation method of the disclosed Herba Ixeritis Sonchifoliae aqueous extract of Chinese patent application CN 1346648A is: decoct with water → collecting decoction → concentrate → add calcium oxide, centrifugal, precipitate → add ethanol, suspension, centrifugal → as to add the sulphuric acid neutralization, wave alcohol → add injection dilute with water → autoclaving → freezing → membrane separation technique ultrafiltration → dilution → embedding → sterilization.This extraction process complexity, though wherein doughnut membrance separation hyperfiltration technique can remove macromole impurity and antibacterial, the ultrafilter membrane price is expensive; and it is easily blocked; some medicine can also make the character of film change, and influences the protection and the regeneration of ultrafiltration, is not suitable for industrialized great production.Preparation technology's flow process of the Herba Ixeritis Sonchifoliae water extract that Chinese patent CN 1377689A introduces is: decoct with water → coarse filtration, microfiltration → concentrate → add calcium oxide, filtration → add ethanol, suspension → add sulphuric acid and neutralize, filter → add injection dilute with water →-8 a ℃ cold preservation filtration → active carbon and boil → embedding → sterilization, this extraction process and CN 1346648A basically identical, just adopt the active carbon boiling method to filter with the ultrafiltration of alternative membrane isolation technics, its shortcoming is an active carbon in absorption antibacterial and impurity, has also adsorbed effective medicinal ingredient.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Herba Ixeritis Sonchifoliae medicinal extract, this extracting method technology is simple, and extraction process is quality controllable, medicinal ingredient extraction ratio height and good stabilities such as flavone, adenosine.
Another object of the present invention is to provide Herba Ixeritis Sonchifoliae pharmaceutical preparation, and said preparation is an active component to utilize the prepared Herba Ixeritis Sonchifoliae medicinal extract of the inventive method.
The Herba Ixeritis Sonchifoliae medicinal extract that the characteristics of Herba Ixeritis Sonchifoliae medicinal extract preparation method of the present invention have been to adopt macroporous adsorbent resin to come separating and purifying flavone compounds, adenosine etc. to form; macroporous resin is a kind of chromatography method that adsorptivity and screening property combine; the influence that has the physical and chemical stability height, not existed by inorganic matter; it is easy to regenerate; life cycle is long; be suitable for the formation closed cycle, plurality of advantages such as cost saving are fit to the large-scale production of enterprise.The inventive method comprises the steps:
Herba Ixeritis Sonchifoliae adds alcohol reflux → medicinal residues decocting and boils → filter → concentrate → precipitate with ethanol → filtration concentrates → macroporous resin adsorption → water elution → ethanol elution → concentrating under reduced pressure → Herba Ixeritis Sonchifoliae medicinal extract.
Its concrete operation method is: get clean Herba Ixeritis Sonchifoliae, measure alcohol reflux 2～4 times, each 2～4 hours with 20～40 times; The Herba Ixeritis Sonchifoliae medicinal residues that to cross through alcohol reflux boil each 2～4 hours 2～4 times with 20～50 times decocting again; Filter, filtrate is carried out precipitate with ethanol 2～3 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 50%～75% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 36～48 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last macroporous resin, the control flow velocity is 3～5ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 3～5ml/min; After eluting is complete, collect ethanol elution, decompression, concentrated promptly gets the Herba Ixeritis Sonchifoliae medicinal extract.
Among the present invention, 4 ℃ of conventional cold preservation preservations are adopted in cold preservation, check that with thin layer chromatography the total flavones in the effluent comes to judge whether eluting is complete in the ethanol elution process, the developing solvent that thin layer chromatography adopted is chloroform-methanol (8: 2, V/V), under the 365nm fluorescent lamp, inspect,, show that promptly eluting is complete if there is not the fluorescent spot point to detect.
The method of quality control of Herba Ixeritis Sonchifoliae medicinal extract is as follows:
Herba Ixeritis Sonchifoliae flavone compound, adenosine are the main effective ingredient of Herba Ixeritis Sonchifoliae medicinal extract, and wherein the Herba Ixeritis Sonchifoliae flavonoid content is the highest, and general flavone content can be used as the index of quality control.By weight percentage, content of total flavone should reach more than 50%, adopts ultraviolet spectrophotometry to analyze, and is reference substance with the rutin, measures the light absorption value at 500nm wavelength place.
Add excipient or other adjuvant of acceptable pharmaceutically with the prepared Herba Ixeritis Sonchifoliae medicinal extract of the inventive method as active component, make various pharmaceutical preparatioies according to a conventional method, as oral formulations such as the injection that uses for injection or tablet, capsule, oral liquid, granules.
Among the present invention, the content of Herba Ixeritis Sonchifoliae total flavones should be more than or equal to 5mg/ml in the injection, and the content of adenosine should be more than or equal to 30 μ g/ml; Content of total flavone should restrain more than or equal to 5mg/ in the oral formulations, and the content of adenosine should restrain more than or equal to 30 μ g/.Herba Ixeritis Sonchifoliae pharmaceutical preparation of the present invention has good stable.
Below by comparative experiments the extraction effect of the inventive method to the Herba Ixeritis Sonchifoliae medicinal extract is described:
(1) Herba Ixeritis Sonchifoliae medicinal extract preparation method:
1, the inventive method: get clean Herba Ixeritis Sonchifoliae 25kg, with the alcohol reflux of 30 times of amounts 3 times, each 3 hours; The Herba Ixeritis Sonchifoliae medicinal residues of again alcohol reflux being crossed boil 3 times with the decocting of 40 times of amounts, each 3 hours; Filter, filtrate is carried out precipitate with ethanol 2 times after concentrating, and makes to contain the alcohol amount and reach 60% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 48 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last AB-8 type macroporous resin, the control flow velocity is 4ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 4ml/min; Check total flavones in the effluent with thin layer chromatography in the elution process, to judge eluting whether complete [developing solvent: chloroform-methanol (8: 2) inspect, must not have the fluorescence speckle under the 365nm fluorescent lamp]; Collect ethanol elution, decompression, concentrated promptly gets the Herba Ixeritis Sonchifoliae medicinal extract.
2, Chinese patent application CN 1346648A method: take by weighing clean Herba Ixeritis Sonchifoliae 25kg, decoct with water 2 times, add 12～15 times of water gagings for the first time and decocted 1 hour, adding for the second time 8～10 times of water gagings decocted 0.5 hour, merge decoction liquor, be concentrated into every 1ml and be equivalent to crude drug in whole 0.5g, be cooled to below 40 ℃, the limit adds 10% calcium oxide breast limit and stirs, regulate pH value to 10, placed 12 hours, centrifugal, precipitate is weighed, be suspended in 5.0～5.5 times the ethanol, add 50% sulfuric acid solution and regulate pH value 3～4, fully stir, centrifugal, clear and bright liquid adds 40% sodium hydroxide solution and regulates pH value to 7～8, filters, and filtrate recycling ethanol is also waved most ethanol, adding injection is diluted with water to every 1ml and is equivalent to crude drug in whole 4.0g, 115 ℃～120 ℃ added autoclaving 15 minutes, put coldly, transferred more than 24 hours in-5 ℃ again, naturally melt, with 50,000 molecular weight Hollow Fiber Ultrafiltrations, transfer pH7.6～7.8, with 10,000 molecular weight Hollow Fiber Ultrafiltrations, microporous filter membrane filters, and promptly gets the Herba Ixeritis Sonchifoliae medicinal extract.
More than every kind of processing method all repeat 3 times.
(2) general flavone content and the adenosine content in the above resulting extract of each processing method of mensuration.The content assaying method of total flavones and adenosine is as follows:
Content of total flavone adopts determined by ultraviolet spectrophotometry, is reference substance with the rutin, measures the light absorption value at 500nm wavelength place.
The content of adenosine adopts high effective liquid chromatography for measuring, and condition determination is as follows:
Chromatographic column: Dimonsil
TMC18 post (46mm * 250mm, 5 μ m), mobile phase is methanol acetonitrile water (volume ratio 5: 4: 91); Flow velocity 1mLmin-1; Sample size 20 μ L; Detect wavelength 259nm.
(3) experimental result:
Table 1 flavone total amount and adenosine content
| The inventive method | CN 1346648A method | |
| General flavone content (gram) adenosine content (gram) | 272 2.2 | 134 0.7 |
From the experimental result shown in the table 1 as can be seen, the inventive method has good extraction effect, and the extracted amount of effective ingredient such as Herba Ixeritis Sonchifoliae flavone compound, adenosine obviously is better than art methods.
Beneficial effect
1, to have extraction process simple for the inventive method, advantage such as cost is low, extraction process is quality controllable.
2, the inventive method adopts macroporous adsorbent resin to come separating and purifying flavone, in the leaching process loss of Herba Ixeritis Sonchifoliae medicinal ingredient little, extraction ratio height, effective ingredient Herba Ixeritis Sonchifoliae flavone compound and adenosine content height in the resulting Herba Ixeritis Sonchifoliae medicinal extract.
3, pharmaceutical preparation of the present invention has good stability.
The specific embodiment
The present invention is further elaborated below in conjunction with specific embodiment, but do not limit the present invention.
Embodiment 1 preparation Herba Ixeritis Sonchifoliae medicinal extract
Get clean Herba Ixeritis Sonchifoliae 30kg, measure alcohol reflux 4 times, each 3 hours with 20 times; The Herba Ixeritis Sonchifoliae medicinal residues of again alcohol reflux being crossed boil 4 times with the decocting of 35 times of amounts, each 4 hours; Filter, filtrate is carried out precipitate with ethanol 2 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 75% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 48 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last AB-6 type macroporous resin, the control flow velocity is 5ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 3ml/min; Check total flavones in the effluent with thin layer chromatography in the elution process, to judge eluting whether complete [developing solvent: chloroform-methanol (8: 2) inspect, must not have the fluorescence speckle under the 365nm fluorescent lamp]; Collect ethanol elution, decompression, concentrated promptly gets the Herba Ixeritis Sonchifoliae medicinal extract.
Embodiment 2 preparation Herba Ixeritis Sonchifoliae medicinal extracts
Get clean Herba Ixeritis Sonchifoliae 25kg, measure alcohol reflux 3 times, each 3 hours with 30 times; The Herba Ixeritis Sonchifoliae medicinal residues of again alcohol reflux being crossed boil 2 times with the decocting of 50 times of amounts, each 2 hours; Filter, filtrate is carried out precipitate with ethanol 3 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 65% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 36 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last AB-8 type macroporous resin, the control flow velocity is 4ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 4ml/min; Check total flavones in the effluent with thin layer chromatography in the elution process, to judge eluting whether complete [developing solvent: chloroform-methanol (8: 2) inspect, must not have the fluorescence speckle under the 365nm fluorescent lamp]; Collect ethanol elution, decompression, concentrated promptly gets the Herba Ixeritis Sonchifoliae medicinal extract.
Embodiment 3 Herba Ixeritis Sonchifoliae medicament freeze-drying injectable powder
Prescription is formed: Herba Ixeritis Sonchifoliae 30kg
Mannitol 1kg
Water for injection is an amount of
Make 10000ml
Preparation method:
Get clean bitter dish 30kg, measure alcohol reflux 2 times, each 3 hours with 40 times; The Herba Ixeritis Sonchifoliae medicinal residues of again alcohol reflux being crossed boil 2 times with the decocting of 50 times of amounts, each 2 hours; Filter, filtrate is carried out precipitate with ethanol 2 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 75% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 48 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last D
101The type macroporous resin, the control flow velocity is 5ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 5ml/min; Check total flavones in the effluent with thin layer chromatography in the elution process, to judge eluting whether complete [developing solvent: chloroform-methanol (8: 2) inspect, must not have the fluorescence speckle under the 365nm fluorescent lamp]; Collect ethanol elution, decompression, concentrated promptly gets the medicinal extracting solution of Herba Ixeritis Sonchifoliae; Add mannitol 1kg, stir, dissolving filters, and adds the injection water and make the aqueous solution that every 1ml contains the 7mg total flavones, and re-adjustment pH value to 8 promptly gets the used Herba Ixeritis Sonchifoliae medicinal extract of this injection lyophilizing solution;
With the used Herba Ixeritis Sonchifoliae medicinal extract of above-mentioned Herba Ixeritis Sonchifoliae injection lyophilizing solution by after every bottle of 10ml packing, do not seal and put into and freeze drying box size corresponding metal dish, freeze drying box is carried out sterilization treatment, and the temperature of its shelf is reduced to-30 ℃, the metal dish that preparation will be housed is put into freeze drying box rapidly, kept 2 hours, then freeze drying box is carried out application of vacuum, making the vacuum in the case is 0.2Pa, again shelf is heated up, and be strict controlled in below the eutectic point-2 ℃, kept 12 hours, be warming up to 40 ℃ at last, and the maintenance certain hour, formulation temperature is overlapped with shelf temperature, put into aseptic filtering gas, the water content of control preparation is sealed rapidly and is got final product 2%.General flavone content is 7mg/ml in this injectable powder, and adenosine content is 58 μ g/ml.
Embodiment 4 Herba Ixeritis Sonchifoliae medicine injections
Prescription is formed: Herba Ixeritis Sonchifoliae 25kg
Sodium chloride 90g
Water for injection is an amount of
Make 10000ml
Preparation method:
Get clean Herba Ixeritis Sonchifoliae 25kg, measure alcohol reflux 4 times, each 2 hours with 20 times; The Herba Ixeritis Sonchifoliae medicinal residues of again alcohol reflux being crossed boil 4 times with the decocting of 20 times of amounts, each 2 hours; Filter, filtrate is carried out precipitate with ethanol 3 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 50% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 48 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last polyamide type macroporous resin, the control flow velocity is 3ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 3ml/min; Check total flavones in the effluent with thin layer chromatography in the elution process, to judge eluting whether complete [developing solvent: chloroform-methanol (8: 2) inspect, must not have the fluorescence speckle under the 365nm fluorescent lamp]; Collect ethanol elution, decompression, concentrated promptly gets Herba Ixeritis Sonchifoliae medicinal ingredient extracting solution; Add sodium chloride 90g, stir, dissolving filters, and adds the injection water and make the aqueous solution that every 1ml contains the 7.5mg total flavones, and re-adjustment pH value to 7.5 promptly gets the used Herba Ixeritis Sonchifoliae medicinal extract of this injection solution;
The used Herba Ixeritis Sonchifoliae medicinal extract of above-mentioned Herba Ixeritis Sonchifoliae injection solution by after every bottle of 10ml packing, is sealed rapidly, and sterilization gets final product.General flavone content is 7.5mg/ml in this injection, and adenosine content is 45 μ g/ml.
Embodiment 5 Herba Ixeritis Sonchifoliae medicament freeze-drying injectable powder
Prescription is formed: Herba Ixeritis Sonchifoliae 35kg
Gelatin hydrolysate 0.5kg
Glucose 0.5kg
Water for injection is an amount of
Make 10000ml
Preparation method:
Get clean Herba Ixeritis Sonchifoliae 35kg, measure alcohol reflux 3 times, each 3 hours with 30 times; The Herba Ixeritis Sonchifoliae medicinal residues of again alcohol reflux being crossed boil 3 times with the decocting of 40 times of amounts, each 3 hours; Filter, filtrate is carried out precipitate with ethanol 2 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 60% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 36 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last AB-8 type macroporous resin, the control flow velocity is 4ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 4ml/min; Check total flavones in the effluent with thin layer chromatography in the elution process, to judge eluting whether complete [developing solvent: chloroform-methanol (8: 2) inspect, must not have the fluorescence speckle under the 365nm fluorescent lamp]; Collect ethanol elution, decompression, concentrated promptly gets Herba Ixeritis Sonchifoliae medicinal ingredient extracting solution; Add gelatin hydrolysate and each 0.5kg of glucose, stir, dissolving filters, and adds the injection water and make the aqueous solution that every 1ml contains the 6mg total flavones, and re-adjustment pH value to 7 promptly gets the used Herba Ixeritis Sonchifoliae medicinal extract of this injection lyophilizing solution;
With the used Herba Ixeritis Sonchifoliae medicinal extract of above-mentioned Herba Ixeritis Sonchifoliae injection lyophilizing solution by after every bottle of 10ml packing, do not seal and put into and freeze drying box size corresponding metal dish, freeze drying box is carried out sterilization treatment, and the temperature of its shelf is reduced to-30 ℃, the metal dish that preparation will be housed is put into freeze drying box rapidly, kept 3 hours, then freeze drying box is carried out application of vacuum, making the vacuum in the case is 0.2Pa, again shelf is heated up, and be strict controlled in below the eutectic point-2 ℃, kept 11 hours, be warming up to 40 ℃ at last, and the maintenance certain hour, formulation temperature is overlapped with shelf temperature, put into aseptic filtering gas, the water content of control preparation is sealed rapidly and is got final product 2%.General flavone content is 6mg/ml in this injectable powder, and adenosine content is 37 μ g/ml.
Embodiment 6 Herba Ixeritis Sonchifoliae medicinal tablets
Prescription is formed: Herba Ixeritis Sonchifoliae 40kg
Starch slurry is an amount of
Microcrystalline Cellulose 15kg
Water for injection is an amount of
Make 10000
Preparation method:
Get clean Herba Ixeritis Sonchifoliae 40kg, measure alcohol reflux 4 times, each 2.5 hours with 25 times; The Herba Ixeritis Sonchifoliae medicinal residues of again alcohol reflux being crossed boil 3 times with 30 times decocting, each 2.5 hours; Filter, filtrate is carried out precipitate with ethanol 3 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 70% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 48 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last D
201The type macroporous resin, the control flow velocity is 5ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 3ml/min; Check total flavones in the effluent with thin layer chromatography in the elution process, to judge eluting whether complete [developing solvent: chloroform-methanol (8: 2) inspect, must not have the fluorescence speckle under the 365nm fluorescent lamp]; Collect ethanol elution, decompression, concentrated promptly gets the medicinal extraction extracting solution of Herba Ixeritis Sonchifoliae.
Above-mentioned medicinal extraction extracting solution is mixed with starch, granulate with starch slurry, drying, granulate is surveyed content, contains 6mg total flavones tabletting by every, promptly.This tablet, the every heavy 200mg of sheet, every contains adenosine 20 micrograms.
The stability experiment of embodiment 7 Herba Ixeritis Sonchifoliae medicine injectable powder
Prepare Herba Ixeritis Sonchifoliae medicine injectable powder by embodiment 3 methods, Herba Ixeritis Sonchifoliae medicine injectable powder places 37 ℃ of climatic chambers to deposit.Timing sampling checks that 3 totally months, inspection item was as follows:
Visual examination: whether be out of shape atrophy, whether color deepens;
Clarity test: getting one bottle and add 10ml water for injection, observe dissolution time, is instant in 20 seconds, and it is qualified to be considered as,
Whether lamp inspection has precipitate to separate out;
The medicinal liquid pH value is checked: get one bottle add the 10ml dissolved in distilled water after, with 25 type pH meters mensuration medicinal liquid pH value;
The assay of main component adenosine and flavone.
Place 37 ℃ to investigate 3 months continuously Herba Ixeritis Sonchifoliae medicine injectable powder, experimental result sees Table 2.
37 ℃ of accelerated test results of table 2 Herba Ixeritis Sonchifoliae medicine injectable powder
| Time (moon) | |||||
| 0 | 1 | 2 | 3 | ||
| 01 batch | Color and luster pH value water solublity adenosine (μ g/ml) flavone (mg/ml) | Yellowish 7.70 instant 58 7.31 | Yellowish 7.69 instant 56 7.30 | Yellowish 7.65 instant 56 7.28 | Yellowish 7.61 instant 55 7.27 |
| 02 batch | Color and luster pH value water solublity adenosine (μ g/ml) flavone (mg/ml) | Yellowish 7.73 instant 63 7.29 | Yellowish 7.69 instant 59 7.25 | Yellowish 7.69 instant 60 7.24 | Yellowish 7.61 instant 58 7.24 |
| 03 batch | Color and luster pH value water solublity adenosine (μ g/ml) flavone (mg/ml) | Yellowish 7.73 instant 64 7.25 | Yellowish 7.69 instant 59 7.24 | Yellowish 7.67 instant 62 7.24 | Yellowish 7.65 instant 61 7.22 |
As shown in table 2, the content of the outward appearance of medicine injectable powder of the present invention, color and luster, water solublity, pH value and adenosine and flavone has no significant change, steady quality, and every batch of moisture determination in addition is all below 2%.
Embodiment 8 Herba Ixeritis Sonchifoliae medicine oral liquids
Prescription is formed: Herba Ixeritis Sonchifoliae 27kg
Water is an amount of
Make 10000ml
Preparation method:
Get clean Herba Ixeritis Sonchifoliae 27kg, measure alcohol reflux 4 times, each 2 hours with 25 times; The Herba Ixeritis Sonchifoliae medicinal residues of again alcohol reflux being crossed boil 4 times with the decocting of 20 times of amounts, each 2 hours; Filter, filtrate is carried out precipitate with ethanol 3 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 65% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 48 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last polyamide type macroporous resin, the control flow velocity is 3ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 3ml/min; Check total flavones in the effluent with thin layer chromatography in the elution process, to judge eluting whether complete [developing solvent: chloroform-methanol (8: 2) inspect, must not have the fluorescence speckle under the 365nm fluorescent lamp]; Collect ethanol elution, decompression, concentrated promptly gets Herba Ixeritis Sonchifoliae medicinal ingredient extracting solution; Add water and make the aqueous solution that every 1ml contains the 6.5mg total flavones, re-adjustment pH value to 7.0 promptly gets the used Herba Ixeritis Sonchifoliae medicinal extract of this oral liquid solution;
The used Herba Ixeritis Sonchifoliae medicinal extract of above-mentioned Herba Ixeritis Sonchifoliae oral liquid solution by after every bottle of 10ml packing, is sealed rapidly, and sterilization gets final product.General flavone content is 6.5mg/ml in this injection, and adenosine content is 55 μ g/ml.
Embodiment 9 Herba Ixeritis Sonchifoliae medicinal granules
Prescription is formed: Herba Ixeritis Sonchifoliae 30kg
Starch slurry is an amount of
Microcrystalline Cellulose 47kg
Make 10000 bags
Preparation method:
Get clean Herba Ixeritis Sonchifoliae 30kg, measure alcohol reflux 3 times, each 2 hours with 20 times; The Herba Ixeritis Sonchifoliae medicinal residues of again alcohol reflux being crossed boil 3 times with the decocting of 20 times of amounts, each 2 hours; Filter, filtrate is carried out precipitate with ethanol 3 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 60% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 48 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last polyamide type macroporous resin, the control flow velocity is 3ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 3ml/min; Check total flavones in the effluent with thin layer chromatography in the elution process, to judge eluting whether complete [developing solvent: chloroform-methanol (8: 2) inspect, must not have the fluorescence speckle under the 365nm fluorescent lamp]; Collect ethanol elution, decompression, concentrated promptly gets Herba Ixeritis Sonchifoliae medicinal ingredient extracting solution;
Above-mentioned Herba Ixeritis Sonchifoliae medicinal ingredient extracting solution is mixed with microcrystalline Cellulose, granulate with starch slurry, drying, granulate is surveyed content, packing, promptly.This granule, the heavy 5g of every bag contains adenosine 300 micrograms, total flavones 28mg.
Embodiment 10 Herba Ixeritis Sonchifoliae medicine capsules
Prescription is formed: Herba Ixeritis Sonchifoliae 30kg
Starch slurry is an amount of
Microcrystalline Cellulose 12kg
Make 10000
Preparation method: get clean Herba Ixeritis Sonchifoliae 30kg, measure alcohol reflux 3 times, each 2 hours with 20 times; The Herba Ixeritis Sonchifoliae medicinal residues of again alcohol reflux being crossed boil 3 times with the decocting of 20 times of amounts, each 2 hours; Filter, filtrate is carried out precipitate with ethanol 3 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 60% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 48 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last polyamide type macroporous resin, the control flow velocity is 3ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 3ml/min; Check total flavones in the effluent with thin layer chromatography in the elution process, to judge eluting whether complete [developing solvent: chloroform-methanol (8: 2) inspect, must not have the fluorescence speckle under the 365nm fluorescent lamp]; Collect ethanol elution, decompression, concentrated promptly gets Herba Ixeritis Sonchifoliae medicinal ingredient extracting solution;
Above-mentioned Herba Ixeritis Sonchifoliae medicinal ingredient extracting solution is mixed with microcrystalline Cellulose, granulate with starch slurry, drying, granulate is surveyed content, packing, promptly.This capsule, every heavy 150mg contains adenosine 70 micrograms, total flavones 6mg.
Claims (5)
1, a kind of preparation method of Herba Ixeritis Sonchifoliae medicinal extract, it is characterized in that adopting macroporous adsorbent resin to come separation and purification Herba Ixeritis Sonchifoliae medicinal extract, may further comprise the steps: Herba Ixeritis Sonchifoliae adds that alcohol reflux, medicinal residues decocting boil, filter, concentrate, precipitate with ethanol, filtration concentrate, macroporous resin adsorption, water elution, ethanol elution, concentrating under reduced pressure obtain medicinal extract.
2, the preparation method of Herba Ixeritis Sonchifoliae medicinal extract according to claim 1 is characterized in that may further comprise the steps: get clean Herba Ixeritis Sonchifoliae, measure alcohol reflux 2～4 times, each 2～4 hours with 20～40 times; The Herba Ixeritis Sonchifoliae medicinal residues that to cross through alcohol reflux boil each 2～4 hours 2～4 times with 20～50 times decocting again; Filter, filtrate is carried out precipitate with ethanol 2～3 times after being concentrated into the thick paste shape, makes to contain the alcohol amount and reach 50%～75% at every turn; Get supernatant then and filter merging filtrate and ethanol extract, cold preservation 36～48 hours; Get supernatant and filter, filtrate is concentrated into every 1ml and is equivalent to crude drug in whole 0.5g; Last macroporous resin, the control flow velocity is 3～5ml/min; After filtrate was all adsorbed, it was colourless to be eluted to effluent with distilled water, and elution speed is 3ml/min; Reuse 70% ethanol carries out eluting, and the control flow velocity is 3～5ml/min; After eluting is complete, collect ethanol elution, decompression, concentrated promptly gets the Herba Ixeritis Sonchifoliae medicinal extract.
3, the resulting Herba Ixeritis Sonchifoliae medicinal extract of the described preparation method of claim 1 pharmaceutical preparation of further making.
4, Herba Ixeritis Sonchifoliae pharmaceutical preparation according to claim 3 is characterized in that being injection or oral agents.
5, according to claim 3 or 4 described Herba Ixeritis Sonchifoliae pharmaceutical preparatioies, the content that it is characterized in that Herba Ixeritis Sonchifoliae total flavones in the described injection is more than or equal to 5mg/ml, and the content of adenosine is more than or equal to 30 μ g/ml; Content of total flavone restrains more than or equal to 5mg/ in the described oral formulations, and the content of adenosine restrains more than or equal to 30 μ g/.
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| CN 200510023904 CN1817351A (en) | 2005-02-07 | 2005-02-07 | Production of variolaria amra medicinal extract and its medicinal preparation |
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| CN 200510023904 CN1817351A (en) | 2005-02-07 | 2005-02-07 | Production of variolaria amra medicinal extract and its medicinal preparation |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102293805A (en) * | 2011-01-06 | 2011-12-28 | 沈阳双鼎制药有限公司 | Total phenolic acid of ixeris sonchifolia (Bunge) hance, and preparation method |
| CN102523862A (en) * | 2011-11-16 | 2012-07-04 | 沈阳双鼎制药有限公司 | Cultivation and quality control method for ixeris sonchifolia hance for Kudiezi injection |
| CN108420842A (en) * | 2018-04-28 | 2018-08-21 | 通化师范学院 | A kind of sowthistle-leaf ixeris seedling preparation of antigout effect |
-
2005
- 2005-02-07 CN CN 200510023904 patent/CN1817351A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102293805A (en) * | 2011-01-06 | 2011-12-28 | 沈阳双鼎制药有限公司 | Total phenolic acid of ixeris sonchifolia (Bunge) hance, and preparation method |
| CN102293805B (en) * | 2011-01-06 | 2013-04-17 | 沈阳双鼎制药有限公司 | Total phenolic acid of ixeris sonchifolia (Bunge) hance, and preparation method |
| CN102523862A (en) * | 2011-11-16 | 2012-07-04 | 沈阳双鼎制药有限公司 | Cultivation and quality control method for ixeris sonchifolia hance for Kudiezi injection |
| CN102523862B (en) * | 2011-11-16 | 2013-05-08 | 沈阳双鼎制药有限公司 | Cultivation and quality control method for ixeris sonchifolia hance for Kudiezi injection |
| CN108420842A (en) * | 2018-04-28 | 2018-08-21 | 通化师范学院 | A kind of sowthistle-leaf ixeris seedling preparation of antigout effect |
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