CN1969999A - Antivirus compound formulation, preparation process, quality control method and use thereof - Google Patents
Antivirus compound formulation, preparation process, quality control method and use thereof Download PDFInfo
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Abstract
The invention discloses a compound preparation which comprises two or more of extracts of scutellaria root flavones, barren wort flavones and houttuynia cordata, and can be prepared into and can be prepared into injections, capsules, tablets, dispersible tablets, sublingual tablets, granules, oral liquid preparations, drop pills and other pharmacologically allowable dose forms. The preparation has the advantages of definite curative effects, better stability, lower toxic and side effects, The preparation can be used for treating pneumonia, respiratory tract infection, influenza, avian Influenza, SARS, asthma, and low body immunity.
Description
Technical field
The present invention is a kind of antivirus compound formulation and preparation method thereof, quality control method and application, belongs to technical field of Chinese medicine.
Technical background
Flu is the upper respiratory tract infection that is caused by multiple virus, is commonly called as " cold ", is all generable common respiratory tract diseases of the four seasons.Viral influenza is a upper respiratory tract infection, is called for short again and goes up sense, and be the common respiratory infectious disease that causes by multiple virus.Though it is a lot of to be used for the treatment of the medicine of flu on the market, but the problem that the side effect of Western medicine ubiquity is big, and Chinese patent medicine is according to the different causes of disease, in conjunction with the medicine of theory of Chinese medical science in order to the treatment disease, for example anemofrigid cold, anemopyretic cold etc. all are to need to select different medicines to treat.And at present Western medicine class coldrex exists dizzy, drowsiness, myasthenia of limbs etc. allow the not drawback of fast response of people on the market; And pure Chinese medicine coldrex exists onset to wait shortcoming slowly.Better prevent and treat purpose in order to reach, a large amount of research has been done by many inventors and medicine enterprise, and some outstanding treatment products also are provided; As: number of patent application is: 200410048399.7, name is called the patent application of " a kind of antiviral oral cavity disintegration tablet and preparation method thereof ", and the disease that it is used for the flu aspect has rapid-action effect; But in further investigation, find, adopt the many big prescriptions of flavour of a drug, the complicated component of its preparation, and make patient's dosage big, the applicant has adopted the effective site compatibility of Radix Scutellariae, Herba Epimedii, Herba Houttuyniae can not only reduce patient's dose on this basis, removes the strong composition of some toxic and side effects in the medicinal substances extract, has improved the safety of preparation and the controllability of quality, greatly improve curative effect, and more help the molding of preparation.
Summary of the invention
The objective of the invention is to: a kind of antiviral Chinese medicine preparation and its production and application is provided; The present invention is directed to prior art, under Chinese medical theory instructs, on the basis of experiment screening, adopt Radix Scutellariae total flavones, Herba Epimedii total flavones, Herba Houttuyniae extract compatibility to make preparation, optimize best prescription and technology; The product that obtains, particularly ejection preparation and sublingual lozenge formulation products can play the effect of the first pass effect that absorption is fast, bioavailability is high, rapid-action, avoid liver.
The present invention constitutes like this: calculate according to percentage by weight, it is to be made one or both in X=Herba Epimedii total flavones and the Herba Houttuyniae extract by Radix Scutellariae total flavones 1～99% and X99～1% and suitable adjuvant.Be preferably: calculate according to percentage by weight, it is to be made one or both in X=Herba Epimedii total flavones and the Herba Houttuyniae extract by Radix Scutellariae total flavones 20～80% and X80～20% and suitable adjuvant.Say accurately: calculate according to percentage by weight, it is to be made one or both in X=Herba Epimedii total flavones and the Herba Houttuyniae extract by Radix Scutellariae total flavones 60～40%, X40～60% and suitable adjuvant.
Described preparation be directly used in the injection of drug administration by injection, directly for the venous transfusion of intravenous drip, need to be used for after the dilution all acceptable dosage forms on the concentrated solution for injection of intravenous drip and the injectable sterile powder that makes with freeze-drying or spray drying method and aseptic block and the pharmaceuticss such as tablet, capsule, granule, drop pill, pill, soft capsule, oral liquid, oral cavity disintegration tablet or dispersible tablet.Described preparation can be various injections, drop pill, sublingual lozenge, oral cavity disintegration tablet, dispersible tablet, soft capsule, capsule, ordinary tablet.
Described preparation can make on the basis that in Radix Scutellariae total flavones, Herba Epimedii total flavones and the Herba Houttuyniae extract one or more is prepared into liposome or pro-liposome.
Contain the flavonoid constituents in the described preparation, calculate by weight percentage, wherein 70% of total flavones in the injection and the volatile oil contents total solid after greater than deduction adjuvant amount and water quantities in the preparation, flavonoid in the oral formulations and the volatile oil total solid after greater than deduction adjuvant amount and water quantities in the preparation 50% ";
Described drug effective region can be commercially available or adopt following method preparation:
A, Radix Scutellariae total flavones effective site are preparations like this: get radix scutellariae medicinal materials, adding entry or alcoholic solution after the pulverizing extracts, merge extractive liquid,, filter, concentrate the Radix Scutellariae total flavones crude extract, adopt in ethanol precipitation, column chromatography, extraction, the flocculent precipitation one or more to unite on this basis to use carry out suitably refining, Radix Scutellariae total flavones;
B, Herba Epimedii total flavones effective site are preparations like this: get epimedium herb, adding entry or alcoholic solution after the pulverizing extracts, merge extractive liquid,, filter, concentrate the Herba Epimedii total flavones crude extract, adopt in ethanol precipitation, column chromatography, extraction, the flocculent precipitation one or more to unite on this basis to use carry out suitably refining, Herba Epimedii total flavones;
C, Herba Houttuyniae extract effective site are preparations like this: get the Herba Houttuyniae medical material, add entry, soak into, unite to use with in decocting method, ethanol refluxing process, steam distillation, organic solvent extractionprocess, the supercritical extraction one or more and extract, or carry out on this basis further making with extra care, get Herba Houttuyniae extract.
Injectable sterile block in the described preparation prepares like this: get Herba Houttuyniae extract, after enclose is handled, add Radix Scutellariae total flavones, Herba Epimedii total flavones, add 1800ml water for injection, press medicine and added mannitol than 1: 2.5,, add the injection water to 2000ml with saturated sodium hydroxide solution adjust pH to 6.0～7.0 with supplementary product consumption, mixing, the needle-use activated carbon of adding 0.4% boiled coarse filtration 35 minutes, reuse 0.45 μ m and 0.22 μ m microporous filter membrane filter, the filtrate packing, every bottle of 2.0ml, lyophilization, equilibration time when the balance solidification point of phase I is 0 ℃ is 3 hours, i.e. the time of shelf temperature and product temperature basically identical; The second stage solidification point is from 0 ℃ during to minimum eutectic temperature-15 ℃, and shelf temperature and product temperature equilibration time are 3 hours; Phase III continues to be cooled to-30 ℃, needs 4 hours approximately, keeps this temperature 3 hours, freeze the jail fully until product, promptly begin evacuation, enter drying program, evacuation under-30 ℃ of constant temperature slowly heats up 3～6 ℃/h, to the lowest total of the melting point temperature, the time is about 10 hours, after sublimation drying is finished, continuation is under the low pressure condition, and it is dry to remove residual moisture to heat up, and the time is about 5～8 hours, kept more than 40 ℃ dry 3 hours, gland, promptly.
Described sublingual lozenge is such preparation: get Radix Scutellariae total flavones, Herba Epimedii total flavones, Herba Houttuyniae extract mixing, add 5% lactose, 15% mannitol, 25% polyvinylpyrrolidone K30, cross 30 mesh sieves, add an amount of Pulvis Talci, micropowder silica gel, evenly mixed, tabletting promptly gets sublingual lozenge.The adjuvant of sublingual lozenge can be following one or more: lactose, mannitol, corn starch, polyvinylpyrrolidone K30, citric acid, sodium citrate, magnesium stearate, xanthein, acetoacetate derivative, sweeting agent, lemon flavouring.
The adjuvant of described preparation can be one or more in lactose, galactose, mannitol, corn starch, polyvinylpyrrolidone K30, citric acid, sodium citrate, magnesium stearate, pigment, acetoacetate derivative, sweeting agent, spice, glycine, glucose, sodium chloride, dextran, glycerol, ethanol, propylene glycol, Polyethylene Glycol, sorbitol, tween, HP-, the poloxamer.
Pro-liposome in the described preparation prepares like this: get Radix Scutellariae total flavones, Herba Epimedii total flavones, Herba Houttuyniae extract, add the phosphate buffer dissolving, add in the fused solution of fabaceous lecithin, cholesterol and 18-amine. mixing, stir supersound process, freezing, the dry powder that obtains sieves, promptly.
Described method of quality control comprise in the following method partly or entirely:
(1) finger printing of anti-viral pharmaceutical compositions test comprises based on the finger printing of Radix Scutellariae total flavones composition characteristics with based in the finger printing of Herba Epimedii total flavones and Herba Houttuyniae extract composition characteristics one or more;
(2) baicalin, noroxylin, chrysin, icariin, icariside I, Herba Epimedii glycosides A, B, C, precious icariin I, II, the differential test method of all or part of composition in VI, Quercetin, methylnonanone, decanoylacetaldehyde or its sodium salt, the lauryl aldehyde;
(3) baicalin, noroxylin, chrysin, icariin, icariside I, Herba Epimedii glycosides A, B, C, precious icariin I, II, the content test method of all or part of composition in VI, Quercetin, methylnonanone, decanoylacetaldehyde or its sodium salt, lauryl aldehyde, total flavones, the volatile oil.
Described preparation is used to prepare the medicine of treatment pneumonia, respiratory tract infection, influenza, bird flu, SARS, asthma, the low inferior disease of immunity of organisms.
For proving that medicine provided by the invention has effective effect, the applicant has carried out a series of experiments;
Experimental example 1: to the comparative study of different proportioning pharmacodynamics
By the experiment of Diplococcus pneumoniae infecting mouse protective effect, the prescription of different proportion has been carried out the screening test of system, wherein: get 18～22gKM kind mice random packet, 21 every group, 1. the male and female dual-purpose fills a prescription 1: blank group equivalent normal saline; 2. fill a prescription 2: model control group, equivalent normal saline; 3. fill a prescription 3: Radix Scutellariae total flavones/Herba Epimedii total flavones, Herba Houttuyniae extract=99/1; 4. fill a prescription 4: Radix Scutellariae total flavones/Herba Epimedii total flavones, Herba Houttuyniae extract=80/20; 5. fill a prescription 5: Radix Scutellariae total flavones/Herba Epimedii total flavones, Herba Houttuyniae extract=40/60; 6. fill a prescription 6: Radix Scutellariae total flavones/Herba Epimedii total flavones, Herba Houttuyniae extract=60/40; 7. fill a prescription 7: Radix Scutellariae total flavones/Herba Epimedii total flavones, Herba Houttuyniae extract=20/80; 8. fill a prescription 8: Radix Scutellariae total flavones/Herba Epimedii total flavones, Herba Houttuyniae extract=1/99.Each organizes mice by administration in 1 time/day * 6 days, and administration in the 3rd day is after 1 hour, and 0.5ml/ Mus of lumbar injection Diplococcus pneumoniae bacterium liquid (except that the blank group) continues administration 3 days, observes death condition in each treated animal 7 days.The results are shown in Table 1:
Table 1 prescription research conclusion
| Formula number | Number of animals (only) | Death toll (only) | Survival rate (%) |
| 1 2 3 4 5 6 7 8 | 21 21 21 21 21 21 21 21 | 0 19 14 13 10 11 15 16 | 100 9.5 33.3 38.1 52.4 47.6 28.6 23.8 |
By experimental result as can be known, Radix Scutellariae total flavones: best compatibility scope=40～60%: 60～40% of Herba Epimedii total flavones, Herba Houttuyniae extract.
Experimental example 2: Study on Forming
2.1 the selection of injection filler kind and consumption
The applicant finds that in development suitable filler, filler loading are powder injection formulation molding and stable key factor, and in order to improve the quality of this powder injection formulation, at first, the applicant investigates the kind of filler.The results are shown in following table.
2.1.1 different filler kind screenings
The different filler lyophilizing of table 2 effect relatively
| Filler | Mannitol | Glucose | Lactose | Sodium chloride | HP-β-CD |
| Medicine: adjuvant mouldability | 1: 2.5 good | Not molding in 1: 2.5 | Not molding in 1: 2.5 | Not molding in 1: 2.5 | Not molding in 1: 2.5 |
As seen, because the eutectic point height of mannitol, good water solubility be beneficial to the lyophilizing and the molding of this product, and other filler all is not suitable for this product, so selection mannitol is filler.
2.1.2 the screening of mannitol consumption
The applicant investigates the weight ratio of mannitol and effective ingredient then, the results are shown in following table.
The different filler proportionings of table 3 are to the influence of lyophilizing effect
| Medicine: mannitol | Color | Mouldability | Water solublity | Clarity |
| 1∶1 1∶1.5 1∶2.0 1∶2.5 1∶3.0 | Yellow faint yellow yellowish white | The difference difference is good carefully | The difference difference is good carefully | Difference difference good job is poor |
As seen, medicine: mannitol=1: 2.5 o'clock, formed product is effective, considers from economic angle, determines medicine: mannitol=1: 2.5.
2.2 the selection of sublingual lozenge filler kind and consumption
2.2.1 different filler kind screenings
Sublingual lozenge then is directly to be absorbed and the tablet medicine of performance general action by the Sublingual mucosa.Sublingual lozenge can prevent that gastrointestinal tract from destroying the active ingredient of medicine, also can avoid the drug influence liver function.It is poor to have solved former dosage form disintegrative, and stripping is shortcoming slowly.
Investigation factor and level: pass through preliminary experiment, the rapid release absorption and the curative effect of the viral prescription of antagonism are had the clearly factor of influence: lactose powder (A) mannitol (B) and polyvinylpyrrolidone K30 (C) and consumption are investigated as variable factor, and each factor is fetched water to put down and seen the following form.Select L9 (4 for use
3) orthogonal table experimentizes.
Table 4 orthogonal test factor level table
| Lactose | Mannitol | Polyvinylpyrrolidone K30 | |
| 1 2 3 | 20％ 10％ 5％ | 15％ 25％ 35％ | 5％ 15％ 25％ |
With to the survival rate of infection of staphylococcus aureus mice as index, concrete experiment is: get 18～22g, KM kind mice random packet, every group 21, the male and female dual-purpose, each organized administration 1 time/day * 6 days, administration was after 1 hour in the 3rd day, 0.5ml/ Mus of lumbar injection staphylococcus aureus bacterium liquid continued administration 3 days, observed death condition in each treated animal 7 days.Experiment is divided into groups and be the results are shown in following table
Arrangement of table 5 orthogonal test and result
| The factor group number | Lactose | Mannitol | Polyvinylpyrrolidone K30 | Survival rate (%) |
| 1 2 3 4 5 6 7 8 9 | 1 1 1 2 2 2 3 3 3 | 1 2 3 1 2 3 1 2 3 | 1 2 3 2 3 1 3 1 2 | 14.3 38.1 28.6 28.6 33.3 19.0 42.9 14.3 23.8 |
As seen, adjuvant is selected 5% lactose, 15% mannitol, 25% polyvinylpyrrolidone K30, product good drug efficacy for use.
Experimental example 3: preparation pharmacodynamic experiment
3.1 vivo bacteria corrosion action
Protective effect to the infection of staphylococcus aureus mice: get 18～22g, KM kind mice random packet, 21 every group, male and female dual-purpose, 1. blank group equivalent normal saline; 2. model control group, the equivalent normal saline; 3. antiviral granule 3g/kg; 4. injection group 3g/kg of the present invention; 5. sublingual lozenge group 3g/kg of the present invention.Below respectively organize administration 1 time/day * 6 days, administration in the 3rd day is after 1 hour, and 0.5ml/ Mus of lumbar injection staphylococcus aureus bacterium liquid (except that the blank group) continues administration 3 days, observes death condition in each treated animal 7 days, the results are shown in Table.
Table 6 anti-virus formulation is to the protective effect of infection of staphylococcus aureus mice
| Group | Dosage (g/kg) | Number of animals (only) | Death toll (only) | Survival rate (%) |
| Blank group model matched group antiviral granule injection group of the present invention sublingual lozenge group of the present invention | - - 3.00 3.00 3.00 | 21 21 21 21 21 | 0 18 15 11 13 | 100 14.3 28.6 47.6 38.1 |
By experimental result as can be known, than the antiviral granule height, pharmaceutical preparation of the present invention has inhibitory action to staphylococcus aureus to the survival rate of infection of staphylococcus aureus mice in pharmaceutical preparation of the present invention.
3.2 interior resisting virus experiment
The interior resisting virus effect: virus infected mice median lethal dose(LD 50) (LD50) is measured and is got 49 of KM kind mices, body weight 11～13g, the male and female dual-purpose is divided into 7 groups at random, every group 7, get and increase 3 times viral allantoic fluid of poison, with 10 times of dilutions, every group drips a virus concentration, each organize mice under the ether light anaesthesia with viral allantoic fluid 30ul collunarium, observe death toll in 14 days, press Reed Muench method and calculate, LD50 is 2.88.
Protective effect to the influenza a virus infection mice: get KM kind mice, body weight 11～13g, male and female half and half are divided in groups 21 every group (1) blank groups, equivalent normal saline at random; (2) model control group, the equivalent normal saline; (3) ribavirin group 75mg/kg; (4) injection group 3g/kg of the present invention; (5) sublingual lozenge group 3g/kg of the present invention.Below respectively organize mice administration 1 time/* 6 days; in administration respectively organized in the day mice (except that the blank group) under the ether light anaesthesia to increase the viral allantois drop nose infecting mouse of poison 3 times; every Mus 30ul (20 LD50 challenging doses) observes zoogenetic infection sequela symptom; record infects death toll after 14 days; and calculate protective rate and average survival natural law, the results are shown in Table
Table 7 anti-virus formulation is to the protective effect of influenza a virus infection mice
| Group | Dosage (g/kg) | Number of animals (only) | Death toll (only) | Survival rate (%) |
| Blank group model matched group ribavirin group injection group of the present invention sublingual lozenge group of the present invention | - - 0.75 3.00 3.00 | 21 21 21 21 21 | 0 19 7 9 10 | 100 9.5 66.7 57.1 52.4 |
By experimental result as can be known, pharmaceutical preparation of the present invention has obvious protective effect to the influenza a virus infection mice, and pharmaceutical preparation of the present invention has inhibitory action better to influenza A virus.
Concrete embodiment
Embodiments of the invention 1: Radix Scutellariae total flavones 50g Herba Epimedii total flavones 25g Herba Houttuyniae extract 25g
Get Herba Houttuyniae extract, carry out after enclose handles with Tween 80, add residue two herbal medicines, add 1800ml water for injection, press medicine and added mannitol than 1: 2.5,, add the injection water to 2000ml with saturated sodium hydroxide solution adjust pH to 6.0～7.0 with supplementary product consumption, mixing, the needle-use activated carbon of adding 0.4% boiled coarse filtration 35 minutes, reuse 0.45 μ m and 0.22 μ m microporous filter membrane filter, the filtrate packing, every bottle of 2.0ml, lyophilization, equilibration time when the balance solidification point of phase I is 0 ℃ is 3 hours, i.e. the time of shelf temperature and product temperature basically identical; The second stage solidification point is from 0 ℃ during to minimum eutectic temperature-15 ℃, and shelf temperature and product temperature equilibration time are 3 hours; Phase III continues to be cooled to-30 ℃, needs 4 hours approximately, keeps this temperature 3 hours, freeze the jail fully until product, promptly begin evacuation, enter drying program, evacuation under-30 ℃ of constant temperature slowly heats up 3～6 ℃/h, to the lowest total of the melting point temperature, the time is about 10 hours, after sublimation drying is finished, continuation is under the low pressure condition, and it is dry to remove residual moisture to heat up, and the time is about 5～8 hours, kept more than 40 ℃ dry 3 hours, gland promptly gets the Injectable sterile block.One time 2,1 time on the one, with using behind the 250ml0.9% physiological saline solution.Calculate by weight percentage, in the injection flavones ingredient, volatile oil content sum be deduction adjuvant amount and water quantities in the preparation total solid 25%.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water flushings, reuse 60% alcohol desorption, collect stripping liquid, decompression recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 55%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed polyamide column, earlier with 8 times of volume water washings, discard eluent, 8 times of volume 70% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 55%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 2: Radix Scutellariae total flavones 50g Herba Epimedii total flavones 25g Herba Houttuyniae extract 25g
Get Herba Houttuyniae extract and mix with Radix Scutellariae total flavones, Herba Epimedii total flavones, add 5% lactose, 15% mannitol, 25% polyvinylpyrrolidone K30, cross 30 mesh sieves, add an amount of Pulvis Talci, micropowder silica gel, evenly mixed, tabletting promptly gets sublingual lozenge.
Calculate by weight percentage, all the content sums that can survey composition of the flavones ingredient in the preparation and other be deduction adjuvant amount and water quantities in the preparation total solid 52%.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water flushings, reuse 60% alcohol desorption, collect stripping liquid, decompression recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 55%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed polyamide column, earlier with 8 times of volume water washings, discard eluent, 8 times of volume 70% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 55%)
Wherein Herba Houttuyniae extract derives from commercially available or is made by following method: get Herba Houttuyniae, add 10 times of volume 70% alcohol reflux 3 times, each 1.5 hours, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed macroporous adsorptive resins, earlier with 8 times of volume water washings, discard eluent, 8 times of volume 60% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying must promptly get Herba Houttuyniae extract.(about general flavone content 60%)
Embodiments of the invention 3: Radix Scutellariae total flavones 40g Herba Epimedii total flavones 60g
Get above medicine and add 1800ml water for injection, press medicine and added mannitol than 1: 2.5 with supplementary product consumption, with saturated sodium hydroxide solution adjust pH to 6.0～7.0, add the injection water to 2000ml, mixing, the needle-use activated carbon of adding 0.4%, boiled 35 minutes, coarse filtration, reuse 0.45 μ m and 0.22 μ m microporous filter membrane filter, the filtrate packing, every bottle of 2.0ml, lyophilization, the equilibration time when the balance solidification point of phase I is 0 ℃ is 3 hours, i.e. the time of shelf temperature and product temperature basically identical; The second stage solidification point is from 0 ℃ during to minimum eutectic temperature-15 ℃, and shelf temperature and product temperature equilibration time are 3 hours; Phase III continues to be cooled to-30 ℃, needs 4 hours approximately, keeps this temperature 3 hours, freeze the jail fully until product, promptly begin evacuation, enter drying program, evacuation under-30 ℃ of constant temperature slowly heats up 3～6 ℃/h, to the lowest total of the melting point temperature, the time is about 10 hours, after sublimation drying is finished, continuation is under the low pressure condition, and it is dry to remove residual moisture to heat up, and the time is about 5～8 hours, kept more than 40 ℃ dry 3 hours, gland promptly gets the Injectable sterile block.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water flushings, reuse 60% alcohol desorption, collect stripping liquid, decompression recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 55%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed polyamide column, earlier with 8 times of volume water washings, discard eluent, 8 times of volume 70% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 55%)
Embodiments of the invention 4: Radix Scutellariae total flavones 40g Herba Houttuyniae extract 60g
Get Herba Houttuyniae extract, carry out adding Radix Scutellariae total flavones and mixing after enclose handles with Tween 80, add 5% lactose, 15% mannitol, 25% polyvinylpyrrolidone K30, cross 30 mesh sieves, add an amount of Pulvis Talci, micropowder silica gel, evenly mixed, tabletting promptly gets sublingual lozenge.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water flushings, reuse 60% alcohol desorption, collect stripping liquid, decompression recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 55%)
Wherein Herba Houttuyniae extract derives from commercially available.
Embodiments of the invention 5: Radix Scutellariae total flavones 40g Herba Epimedii total flavones 30g Herba Houttuyniae extract 30g
Get above medicament mixed, in adding lactose, mannitol, corn starch, polyvinylpyrrolidone K30, citric acid, sodium citrate, magnesium stearate, xanthein, acetoacetate derivative, sweeting agent, the lemon flavouring one or more, cross 30 mesh sieves, add an amount of Pulvis Talci, micropowder silica gel, evenly mixed, tabletting promptly gets sublingual lozenge.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water flushings, reuse 60% alcohol desorption, collect stripping liquid, decompression recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 55%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed polyamide column, earlier with 8 times of volume water washings, discard eluent, 8 times of volume 70% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 55%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil promptly.
Embodiments of the invention 6: Radix Scutellariae total flavones 60g Herba Epimedii total flavones 40g
Above medicament mixed is even, the dextrin of adding equivalent, mix homogeneously is granulated, and is encapsulated, promptly gets capsule.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, and adds 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid, filters decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filters, filtrate stirs with hydrochloric acid adjust pH to 2, and placement is spent the night, filter, precipitation washes with water, drains, and drying under reduced pressure gets Radix Scutellariae extract.(about general flavone content 30%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed polyamide column, earlier with 8 times of volume water and 5 times of volume 10% washing with alcohol, discard eluent, 8 times of volume 60% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 75%)
Embodiments of the invention 7: Radix Scutellariae total flavones 60g Herba Houttuyniae extract 40g
Above medicament mixed is even, add 2.5 times of amount dextrin, 0.4% stevioside, 1.5% microcrystalline Cellulose with an amount of alcoholic solution system soft material, is granulated, and 65 ℃ of forced air dryings are granulated, and granulate promptly gets granule.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water flushings, reuse 60% alcohol desorption, collect stripping liquid, decompression recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 55%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 8: Radix Scutellariae 60 total flavones g Herba Epimedii total flavones 20g Herba Houttuyniae extract 20g
Above medicament mixed is even, add distilled water, filter repeatedly, till the filtrate clarification., filter with absorbent cotton after the stirring and dissolving in filtrate with sucrose, it is an amount of to add distilled water on filter, shakes up, and promptly gets syrup.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water and 5 times of 15% alcohol flushing, discards eluent; Reuse 60% alcohol desorption is collected stripping liquid, decompression recycling ethanol, and measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 75%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed the D-101 macroporous resin column, earlier with 8 times of volume water and 5 times of volume 25% washing with alcohol, discard eluent, 6 times of volume 50% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 85%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 9: Radix Scutellariae total flavones 20g Herba Epimedii total flavones 80g
Above medicament mixed is even, and in principal agent: the ratio of adjuvant=1.5: 1 adds calcium phosphate, by principal agent: the ratio adding micropowder cellulose of adjuvant=1.0: 1, and press principal agent: the crospolyvinylpyrrolidone of adjuvant=2.5: 1, evenly mixed, make soft material in right amount with 70% ethanol, cross 30 mesh sieve system granules, 60 ℃ of dryings are taken out, and cross 30 mesh sieve granulate, add an amount of Pulvis Talci, micropowder silica gel, evenly mixed, tabletting promptly gets dispersible tablet.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, and adds 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid, filters decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filters, filtrate stirs with hydrochloric acid adjust pH to 2, and placement is spent the night, filter, precipitation washes with water, drains, and drying under reduced pressure gets Radix Scutellariae extract.(about general flavone content 30%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid, filters, and measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, add 4 times of volume water stirring and dissolving, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 30%)
Embodiments of the invention 10: Radix Scutellariae total flavones 20g Herba Houttuyniae extract 80g
Get above medicine and add an amount of water for injection dissolving, add the glucose or the sodium chloride of ormal weight, by volume add 0.5% active carbon behind the mixed dissolution, boil, keep little 30min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, boil the saturated sodium hydroxide solution of reuse adjust pH to 6.0～6.5, and 4 ℃ of cold preservations are spent the night, coarse filtration, fine straining, add the injection water, packing, sterilization promptly gets glucose or sodium chloride intravenous infusion.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, and adds 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid, filters decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filters, filtrate stirs with hydrochloric acid adjust pH to 2, and placement is spent the night, filter, precipitation washes with water, drains, and drying under reduced pressure gets Radix Scutellariae extract.(about general flavone content 30%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 11: Radix Scutellariae total flavones 20g Herba Epimedii total flavones 40g Herba Houttuyniae extract 40g
Above medicament mixed is even, will be that 1.8: 1 sodium stearate is put in the rustless steel container with the principal agent ratio, add extract, mix homogeneously is heated to 80-85 ℃, treat whole fusions after, 70-75 ℃ of insulation, mechanical high-speed are stirred 15min to evenly, are transferred in the reservoir, the dropping liquid valve is regulated in 70～75 ℃ of insulations, splashes in 30～35 ℃ the kerosene, drip apart from 5～6cm, drip 40～45 droplets/minute of speed, to the greatest extent and wipe kerosene the drop pill drop that forms, packing promptly gets drop pill.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water flushings, reuse 60% alcohol desorption, collect stripping liquid, decompression recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 55%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed polyamide column, earlier with 8 times of volume water and 5 times of volume 10% washing with alcohol, discard eluent, 8 times of volume 60% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 75%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 12: Radix Scutellariae total flavones 80g Herba Epimedii total flavones 20g
Above medicament mixed is even, add 2.5 times of amount dextrin, 0.4% stevioside, 1.5% microcrystalline Cellulose with an amount of alcoholic solution system soft material, is granulated, and 65 ℃ of forced air dryings are granulated, and granulate promptly gets granule.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, and adds 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid, filters decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filters, filtrate stirs with hydrochloric acid adjust pH to 2, and placement is spent the night, filter, precipitation washes with water, drains, and drying under reduced pressure gets Radix Scutellariae extract.(about general flavone content 30%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed the D-101 macroporous resin column, earlier with 8 times of volume water and 5 times of volume 25% washing with alcohol, discard eluent, 6 times of volume 50% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 85%)
Embodiments of the invention 13: Radix Scutellariae total flavones 80g Herba Houttuyniae extract 20g
Above medicament mixed is even, and in principal agent: the ratio of adjuvant=1.4: 1 adds calcium phosphate, by principal agent: the ratio adding micropowder cellulose of adjuvant=1.2: 1, and press principal agent: the crospolyvinylpyrrolidone of adjuvant=3: 1, evenly mixed, make soft material in right amount with 70% ethanol, cross 20 mesh sieve system granules, 55 ℃ of dryings are taken out, and cross 30 mesh sieve granulate, add an amount of Pulvis Talci, micropowder silica gel, evenly mixed, tabletting promptly gets dispersible tablet.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water flushings, reuse 60% alcohol desorption, collect stripping liquid, decompression recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 55%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 14: 80 parts of Herba Epimedii total flavones 10g of Radix Scutellariae total flavones Herba Houttuyniae extract 10g
Get the low-substituted hydroxypropyl cellulose and 1.5% sorbitol of above medicine adding 5%, compacting promptly gets oral cavity disintegration tablet in flakes.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water flushings, reuse 60% alcohol desorption, collect stripping liquid, decompression recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 55%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed the D-101 macroporous resin column, earlier with 8 times of volume water and 5 times of volume 25% washing with alcohol, discard eluent, 6 times of volume 50% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 85%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 15: Radix Scutellariae total flavones 99g Herba Epimedii total flavones 1g
Above medicine is added suitable adjuvant, evenly mixed, make soft material in right amount with 70% ethanol, cross 20 mesh sieve system granules, 60 ℃ of dryings are taken out, and cross 30 mesh sieve granulate, add an amount of Pulvis Talci, micropowder silica gel, and evenly mixed, tabletting promptly gets tablet.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water and 5 times of 15% alcohol flushing, discards eluent; Reuse 60% alcohol desorption is collected stripping liquid, decompression recycling ethanol, and measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, vacuum drying gets Radix Scutellariae extract.(about general flavone content 75%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid, filters, and measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, add 4 times of volume water stirring and dissolving, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 30%)
Embodiments of the invention 16: Radix Scutellariae total flavones 99g Herba Houttuyniae extract 1g
Get above medicine mixing, add an amount of water for injection dissolving, by volume add 0.3% active carbon, boil, keep little 30min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, with saturated sodium hydroxide solution adjust pH to 6.0～7.0, to boil, 5 ℃ of cold preservations are spent the night, coarse filtration, fine straining, in inlet temperature is 135 ℃, and leaving air temp is 60 ℃, and air velocity is 20ms
-1Condition under spray drying get powder, packing promptly gets injectable sterile powder.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water and 5 times of 20% alcohol flushing, discards eluent; Reuse 60% alcohol desorption is collected stripping liquid, decompression recycling ethanol, and measuring relative density when being concentrated into 60 ℃ is 1.0～1.05, with hydrochloric acid adjust pH to 2, stirs, and placement is spent the night, and filters, and precipitation washes with water, drains, and vacuum drying gets Radix Scutellariae extract.(about general flavone content 85%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 17: Radix Scutellariae total flavones 99g Herba Epimedii total flavones 0.5g Herba Houttuyniae extract 0.5g
Above medicament mixed is even, add 2 times of amount dextrin, 0.5% stevioside, 1.2% microcrystalline Cellulose with an amount of alcoholic solution system soft material, is granulated, and 60 ℃ of forced air dryings are granulated, and granulate promptly gets granule.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, and adds 5 times of volume 30% alcohol reflux 1 time, each 0.1 hour, merge extractive liquid, filters decompression filtrate recycling ethanol, concentrate, add 1 times of volume water dissolution, filter, filtrate is crossed macroporous resin column, earlier with 3 times of water flushings, reuse 30% alcohol desorption, collect stripping liquid, decompression recycling ethanol concentrates, and vacuum drying gets Radix Scutellariae total flavones; (about general flavone content 55%);
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, adds 2 times of volume 20% alcohol reflux 1 time, each 0.1 hour, merge extractive liquid, filters, and filtrate concentrates, add 1 times of water gaging, stirring and dissolving filters, filtrate is crossed polyamide column, earlier with 1 times of volume water washing, discards eluent, 1 times of volume 30% ethanol elution of reuse is collected eluent, decompression recycling ethanol, concentrate, vacuum drying gets Herba Epimedii total flavones; (about general flavone content 55%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 18: Radix Scutellariae total flavones 1g Herba Epimedii total flavones 99g
Above medicament mixed is even, the dextrin of adding equivalent, mix homogeneously is granulated, and is encapsulated, promptly gets capsule.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water and 5 times of 20% alcohol flushing, discards eluent; Reuse 60% alcohol desorption is collected stripping liquid, decompression recycling ethanol, and measuring relative density when being concentrated into 60 ℃ is 1.0～1.05, with hydrochloric acid adjust pH to 2, stirs, and placement is spent the night, and filters, and precipitation washes with water, drains, and vacuum drying gets Radix Scutellariae extract.(about general flavone content 85%)
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, add 10 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, measuring relative density when filtrate is condensed into 50 ℃ is 1.05～1.15, adds 3 times of water gagings, stirring and dissolving, filter, filtrate is crossed polyamide column, earlier with 8 times of volume water and 5 times of volume 10% washing with alcohol, discard eluent, 8 times of volume 60% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, measuring relative density when being condensed into 50 ℃ is 1.10～1.20, and vacuum drying gets Herba Epimedii extract.(about general flavone content 75%)
Embodiments of the invention 19: Radix Scutellariae total flavones 1g Herba Houttuyniae extract 99g
Get above medicine and add an amount of water for injection dissolving, add the glucose or the sodium chloride of ormal weight, by volume add 0.5% active carbon behind the mixed dissolution, boil, keep little 30min that boils, cold slightly filtration, filtrate adds the injection water to ormal weight, boil the saturated sodium hydroxide solution of reuse adjust pH to 6.0～6.5, and 4 ℃ of cold preservations are spent the night, coarse filtration, fine straining, add the injection water, packing, sterilization promptly gets glucose or sodium chloride intravenous infusion.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, add 8 times of volume 70% alcohol reflux 3 times, each 1 hour, merge extractive liquid,, filter, decompression filtrate recycling ethanol, measuring relative density when being concentrated into 60 ℃ is 1.05～1.15, adds 3 times of volume water dissolutioies, filter, filtrate is crossed the AB-8 macroporous resin column, earlier with 6 times of water and 5 times of 20% alcohol flushing, discards eluent; Reuse 60% alcohol desorption is collected stripping liquid, decompression recycling ethanol, and measuring relative density when being concentrated into 60 ℃ is 1.0～1.05, with hydrochloric acid adjust pH to 2, stirs, and placement is spent the night, and filters, and precipitation washes with water, drains, and vacuum drying gets Radix Scutellariae extract.(about general flavone content 85%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 20: Radix Scutellariae total flavones 1g Herba Epimedii total flavones 50g Herba Houttuyniae extract 49g
Above medicament mixed is even, be dissolved in the phosphate buffer (0.15M) standby, a certain proportion of fabaceous lecithin, cholesterol are dissolved in the 18-amine. solution, add in the phosphate-buffered liquor of said medicine, the water-bath type Ultrasound Instrument is handled 10min, gets liposome turbid liquor, behind the frozen drying, cross 180 mesh sieves, aseptic subpackaged, promptly get the pro-liposome injectable powder.
Wherein Radix Scutellariae total flavones derives from commercially available or made by following method: Radix Scutellariae is pulverized, and adds 10 times of volume 90% alcohol reflux 7 times, each 5 hours, merge extractive liquid, filters decompression filtrate recycling ethanol, concentrate, add 6 times of volume water dissolutioies, filter, filtrate is crossed macroporous resin column, earlier with 8 times of water flushings, reuse 90% alcohol desorption, collect stripping liquid, decompression recycling ethanol concentrates, and vacuum drying gets Radix Scutellariae total flavones; (about general flavone content 55%);
Wherein Herba Epimedii total flavones derives from commercially available or made by following method: Herba Epimedii is cut into 1cm left and right sides segment, adds 16 times of volume 90% alcohol reflux 8 times, each 5 hours, merge extractive liquid, filters, and filtrate concentrates, add 8 times of water gagings, stirring and dissolving filters, filtrate is crossed polyamide column, earlier with 12 times of volume water washings, discards eluent, 12 times of volume 90% ethanol elutions of reuse are collected eluent, decompression recycling ethanol, concentrate, vacuum drying gets Herba Epimedii total flavones; (about general flavone content 55%)
Wherein Herba Houttuyniae extract derives from commercially available or made by following method: get Herba Houttuyniae, add 10 times of volume water, soak into half an hour, reheat distillation 8 hours is collected volatile oil and is promptly got Herba Houttuyniae extract.
Embodiments of the invention 21: the quality control method of preparation of the present invention adopts following method:
(1) finger printing of anti-viral pharmaceutical compositions test comprises based on the finger printing of Radix Scutellariae total flavones composition characteristics with based in the finger printing of Herba Epimedii total flavones and Herba Houttuyniae extract composition characteristics one or more;
(2) baicalin, noroxylin, chrysin, icariin, icariside I, Herba Epimedii glycosides A, B, C, precious icariin I, II, the differential test method of all or part of composition in VI, Quercetin, methylnonanone, decanoylacetaldehyde or its sodium salt, the lauryl aldehyde;
(3) baicalin, noroxylin, chrysin, icariin, icariside I, Herba Epimedii glycosides A, B, C, precious icariin I, II, the content test method of all or part of composition in VI, Quercetin, methylnonanone, decanoylacetaldehyde or its sodium salt, lauryl aldehyde, total flavones, the volatile oil.
Claims (14)
1, a kind of antivirus compound formulation is characterized in that: calculate according to percentage by weight, it is to be made one or both in X=Herba Epimedii total flavones and the Herba Houttuyniae extract by Radix Scutellariae total flavones 1～99% and X99～1% and suitable adjuvant.
2, according to the described a kind of antivirus compound formulation of claim 1, it is characterized in that: calculate according to percentage by weight, it is to be made one or both in X=Herba Epimedii total flavones and the Herba Houttuyniae extract by Radix Scutellariae total flavones 20～80% and X80～20% and suitable adjuvant.
3, according to claim 1 or 2 described a kind of antivirus compound formulations, it is characterized in that: calculate according to percentage by weight, it is to be made one or both in X=Herba Epimedii total flavones and the Herba Houttuyniae extract by Radix Scutellariae total flavones 60～40%, X40～60% and suitable adjuvant.
4, according to any described antivirus compound formulation of claim 1～3, it is characterized in that: described preparation can be any acceptable dosage form on the pharmaceutics, comprising: be directly used in the injection of drug administration by injection, directly supply the venous transfusion of intravenous drip, need be used for the concentrated solution for injection of intravenous drip and injectable sterile powder and aseptic block and tablet, capsule, granule, drop pill, pill, soft capsule, oral liquid, oral cavity disintegration tablet and the dispersible tablet etc. that make with freeze-drying or spray drying method after diluting.
5, according to the described a kind of antivirus compound formulation of claim 4, it is characterized in that: described preparation can be various injections, drop pill, sublingual lozenge, oral cavity disintegration tablet, dispersible tablet, soft capsule, capsule, ordinary tablet.
6, according to claim 4,5 described a kind of antivirus compound formulations, it is characterized in that: described preparation can make on the basis that in Radix Scutellariae total flavones and Herba Epimedii total flavones, the Herba Houttuyniae extract one or more is prepared into liposome or pro-liposome.
7, according to any described a kind of antivirus compound formulation in the claim 1～6, it is characterized in that: contain flavones ingredient in the preparation, calculate by weight percentage, wherein the flavones ingredient content in the injection and other all can survey 70% of the total solid of component content sum after greater than deduction adjuvant amount and water quantities in the preparation, all can survey 50% of the total solid of component content sum after greater than deduction adjuvant amount and water quantities in the preparation flavones ingredient content in the oral formulations and other.
8,, it is characterized in that described drug effective region can be commercially available or adopt following method preparation as any described a kind of antivirus compound formulation in the claim 1～7:
A, Radix Scutellariae total flavones effective site are preparations like this: get radix scutellariae medicinal materials, adding entry or alcoholic solution after the pulverizing extracts, merge extractive liquid,, filter, concentrate the Radix Scutellariae total flavones crude extract, adopt in ethanol precipitation, column chromatography, extraction, the flocculent precipitation one or more to unite on this basis to use carry out suitably refining, Radix Scutellariae total flavones;
B, Herba Epimedii total flavones effective site are preparations like this: get epimedium herb, adding entry or alcoholic solution after the pulverizing extracts, merge extractive liquid,, filter, concentrate the Herba Epimedii total flavones crude extract, adopt in ethanol precipitation, column chromatography, extraction, the flocculent precipitation one or more to unite on this basis to use carry out suitably refining, Herba Epimedii total flavones;
C, Herba Houttuyniae extract effective site are preparations like this: get the Herba Houttuyniae medical material, add entry, soak into, unite to use with in decocting method, ethanol refluxing process, steam distillation, organic solvent extractionprocess, the supercritical extraction one or more and extract, or carry out on this basis further making with extra care, get Herba Houttuyniae extract.
9, preparation method according to any described a kind of antivirus compound formulation in the claim 1～8, it is characterized in that: the Injectable sterile block in the described preparation prepares like this: get Herba Houttuyniae extract, Radix Scutellariae total flavones, Herba Epimedii total flavones, add 1800ml water for injection, press medicine and added mannitol than 1: 2.5 with supplementary product consumption, with saturated sodium hydroxide solution adjust pH to 6.0～7.0, add the injection water to 2000ml, mixing, the needle-use activated carbon of adding 0.4%, boiled 35 minutes, coarse filtration, reuse 0.45 μ m and 0.22 μ m microporous filter membrane filter, the filtrate packing, every bottle of 2.0ml, lyophilization, the equilibration time when the balance solidification point of phase I is 0 ℃ is 3 hours, i.e. the time of shelf temperature and product temperature basically identical; The second stage solidification point is from 0 ℃ during to minimum eutectic temperature-15 ℃, and shelf temperature and product temperature equilibration time are 3 hours; Phase III continues to be cooled to-30 ℃, needs 4 hours approximately, keeps this temperature 3 hours, freeze the jail fully until product, promptly begin evacuation, enter drying program, evacuation under-30 ℃ of constant temperature slowly heats up 3～6 ℃/h, to the lowest total of the melting point temperature, the time is about 10 hours, after sublimation drying is finished, continuation is under the low pressure condition, and it is dry to remove residual moisture to heat up, and the time is about 5～8 hours, kept more than 40 ℃ dry 3 hours, gland, promptly.
10, according to the preparation method of any described antivirus compound formulation in the claim 1～8, it is characterized in that: described sublingual lozenge is such preparation: get Radix Scutellariae total flavones, Herba Epimedii total flavones, Herba Houttuyniae extract mixing, add 5% lactose, 15% mannitol, 25% polyvinylpyrrolidone K30, cross 30 mesh sieves, add an amount of Pulvis Talci, micropowder silica gel, evenly mixed, tabletting promptly gets sublingual lozenge.
11, according to any described antivirus compound formulation in the claim 1～6,8, it is characterized in that: adjuvant can be one or more in lactose, galactose, mannitol, corn starch, polyvinylpyrrolidone K30, citric acid, sodium citrate, magnesium stearate, pigment, acetoacetate derivative, sweeting agent, spice, glycine, glucose, sodium chloride, dextran, glycerol, ethanol, propylene glycol, Polyethylene Glycol, sorbitol, tween, HP-, the poloxamer.
12, according to the preparation method of the Chinese medicine preparation of the described treatment cardiovascular and cerebrovascular disease of claim 6, it is characterized in that: the pro-liposome in the described preparation prepares like this: get Radix Scutellariae total flavones, Herba Epimedii total flavones, Herba Houttuyniae extract, add the phosphate buffer dissolving, add in the fused solution of fabaceous lecithin, cholesterol and 18-amine. mixing, stir supersound process, freezing, the dry powder that obtains sieves, promptly.
13, as the application of any described antivirus compound formulation in the claim 1～10, it is characterized in that: described method of quality control comprise in the following method partly or entirely:
(1) finger printing of anti-viral pharmaceutical compositions test comprises based on the finger printing of Radix Scutellariae total flavones composition characteristics with based in the finger printing of Herba Epimedii total flavones and Herba Houttuyniae extract composition characteristics one or more;
(2) baicalin, noroxylin, chrysin, icariin, icariside I, Herba Epimedii glycosides A, B, C, precious icariin I, II, the differential test method of all or part of composition in VI, Quercetin, methylnonanone, decanoylacetaldehyde or its sodium salt, the lauryl aldehyde;
(3) baicalin, noroxylin, chrysin, icariin, icariside I, Herba Epimedii glycosides A, B, C, precious icariin I, II, the content test method of all or part of composition in VI, Quercetin, methylnonanone, decanoylacetaldehyde or its sodium salt, lauryl aldehyde, total flavones, the volatile oil.
14, as the application of any described antivirus compound formulation in the claim 1～3, it is characterized in that: described preparation is used to prepare the medicine of treatment pneumonia, respiratory tract infection, influenza, bird flu, SARS, asthma, the low inferior disease of immunity of organisms.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2018020984A (en) * | 2016-08-05 | 2018-02-08 | 三栄源エフ・エフ・アイ株式会社 | Long acting quercetin glycoside formulation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2018020984A (en) * | 2016-08-05 | 2018-02-08 | 三栄源エフ・エフ・アイ株式会社 | Long acting quercetin glycoside formulation |
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