CN100421685C - Chinese material medica preparation in use for treating infection of influenza virus, and preparation method - Google Patents
Chinese material medica preparation in use for treating infection of influenza virus, and preparation method Download PDFInfo
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- CN100421685C CN100421685C CNB2004100201045A CN200410020104A CN100421685C CN 100421685 C CN100421685 C CN 100421685C CN B2004100201045 A CNB2004100201045 A CN B2004100201045A CN 200410020104 A CN200410020104 A CN 200410020104A CN 100421685 C CN100421685 C CN 100421685C
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Abstract
The present invention relates to a technology and a method for preparing a preparation for treating influenza virus infection. The preparation comprises an oral preparation and an injection, wherein the oral preparation comprises 10 to 60% of barbat skullcap herb extract and 40 to 90% of pharmaceutic auxiliary material; the injection comprises 0.5 to 30% of barbat skullcap herb extract and 70 to 99.5% of pharmaceutic auxiliary material; the barbat skullcap herb extract comprises flavone, alkaloid, steride, saccharide, and the like (the total content of the flavone is from 20 to 90%). The barbat skullcap herb is extracted, separated and enrichened by water and ethanol with different concentration to obtain the barbat skullcap herb extract. The technology is simple, economic and practical, the solvent can be circularly used, and the present invention is suitable for industrial production. The preparation is prepared from single traditional Chinese medicine, and has the advantages of stable quality, less medicine taking dosage, outstanding curative effect and high safety. The present invention is extremely meaningful when developed into Chinese medical preparation for preventing and treating influenza virus infection.
Description
Technical field
The present invention relates to the preparation method of Chinese medicine preparation technology and preparation, the Herba Scutellariae Barbatae extract of a kind of prevention and treatment influenza infection and preparation method thereof of saying so more specifically, reaching with this extract is the various Chinese medicine preparation that main component is made.
Background technology
Influenza claims influenza again, is the acute respiratory infectious disease that is caused by influenza virus.All want every year the eruption and prevalence sexuality to emit in China, and constantly variation, current do not have an ideal medicine.The Chinese medicine preparation of existing various treatment influenza viruss mostly is compound preparation, and as SHUANGHUANLIAN, YINQIAO, Saigae Tataricae, Sang Ju Yin etc., though have certain curative effect, many compositions cause difficult quality to repeat the production poor controllability.Therefore press for sure, quality controllable prevention of curative effect and the Chinese medicine preparation for the treatment of influenza infection on the market, to satisfy the demand of extensive patients.
The Herba Scutellariae Barbatae that the present invention adopts is the herb of labiate Herba Scutellariae Barbatae Scutellaria barbata D.Don.Compositions such as herb contains alkaloid, is rich in flavonoid, phenols, terpenoid, steroidal, polysaccharide, Chinese Pharmacopoeia records Herba Scutellariae Barbatae for 2000 editions one one 89 pages, Herba Scutellariae Barbatae has a lot of pharmacodynamic features, have antibiotic, antiinflammatory, antiviral isoreactivity, cellular immunization to body has facilitation, cancerous cell there is certain inhibitory action, heat clearing away is arranged, detoxifies, invigorate blood circulation, effect such as blood stasis dispelling, detumescence, pain relieving.
The above-mentioned effect of Herba Scutellariae Barbatae has caused people's great attention in recent years, and therefore, often the form with compound recipe is used to prevent or treat the various infection that influenza virus causes.And the Herba Scutellariae Barbatae total flavones extract is as an effective site, and in its antiviral research and the Herba Scutellariae Barbatae extract, total flavones, total alkaloids main component Study on content are not seen bibliographical information.We have obtained the effective site of Herba Scutellariae Barbatae through screening and separating, and the most of composition of product is more clearly, and quality is controlled easily, acts on more sure.
Summary of the invention
Technical problem to be solved by this invention is to overcome on the existing insufficient basis of medicine, provide a kind of and can obviously prevent and suppress influenza infection, and mass ratio is easier to control, and the Herba Scutellariae Barbatae extract that general flavone content is high to reduce impurity, improves curative effect.
Another object of the present invention is, the preparation technology of Herba Scutellariae Barbatae extract effective site is provided, and except that adopting some known methods, has also adopted some important steps to improve content of total flavone in the Herba Scutellariae Barbatae extract.
A further object of the present invention is that it is the various Chinese medicine preparation that main active is made that a kind of effective site with Herba Scutellariae Barbatae extract is provided.
For addressing the above problem, the present invention has studied and defined following technical scheme:
A kind of Herba Scutellariae Barbatae extract that is used for the treatment of influenza infection is characterized in that Herba Scutellariae Barbatae extract is grouped into by one-tenth such as total flavones, alkaloid, steroidal, saccharides, and wherein general flavone content is 20%-90%, total alkaloid content 0.5-10%.
Total flavones, contain carthamin carthamidin, 5,7,4 ' trihydroxy-8 methoxy flavone (5,7,4 '-trihydroxy-8-methoxyflavanone), isocarthamidin isocarthamidin, scutellarein scutellarein, scutellarin scutellarin; Wherein 5,7,4 ' trihydroxy-8 methoxy flavone (4 '-hydroxyl wogonin) 0.1mg/Kg-400mg/Kg has inhibitory action to influenza virus.
The preparation method of Herba Scutellariae Barbatae extract is characterized in that:
A solvent extraction: the Herba Scutellariae Barbatae herb is pulverized with solvent orange 2 A (heating or percolation) extraction, got crude extract;
B separated from solvent purification: carry thing and adopt the B solvent to get mixture through separation and purification, enrichment, recording general flavone content is 20%-90%, total alkaloid content 0.5-10%; Method comprises:
A. liquid-liquid extraction method: crude extract adopts counter-current distribution method to extract continuously with solvent B must extract extract in 6 hours;
B. acid precipitation method: crude extract is transferred PH6-9 through diluted alkaline, uses the B solvent extraction, and water layer is transferred PH2-5 with diluted acid, the acidic precipitation thing, water layer reuse B solvent extraction, extract, with acidic precipitation thing and extract merge mixture;
C. absorb-elute method: crude extract, is collected each component evaporate to dryness and is got extract with solvent B eluting through macroporous resin column or silica gel column chromatography or polyamide column method.
In the preparation method, the extraction solvent orange 2 A is water, 30-90% ethanol, methanol, ethyl acetate, acetone;
Separation and purification solvent B is dichloromethane, chloroform, butanols, isopropyl alcohol, n-butyl alcohol, petroleum ether, ether, water-ethyl acetate, water-n-butyl alcohol, 0.1-20% dilute acid soln, 0.1-20% dilute alkaline soln, ethyl acetate.
Described dilute acid soln is hydrochloric acid, sulphuric acid, phosphoric acid, oxalic acid, acetic acid; Dilute alkaline soln is sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate.
Described macroporous resin model is D-101, AB-8 type, NK-9.
Concrete extracting method is as follows:
(1), the Herba Scutellariae Barbatae herb is pulverized, use water extraction, the crude extract of Herba Scutellariae Barbatae, last macroporous resin column separation.Water and Different concentrations of alcohol (30-90%) eluting.Collect each several part, survey flavone, the highest 1.5-60% of 30-60% ethanol elution part scutellarin content.Ethanol (30-90%) eluate gets mixture general flavone content 20-90%.
(2), the Herba Scutellariae Barbatae herb is pulverized, extract with ethanol 30-90%, the crude extract of Herba Scutellariae Barbatae.Crude extract adds alkali liquor and regulates pH to 7-8, (alkali NaOH, KOH, Na
2CO
3, NaHCO
3), get alkaline medicinal liquid, use organic solvent extraction, tell the solvent layer, pH to 2-4 is transferred in the acid of water layer reuse, (acid HCl, H
2SO
4, H
3PO
4, HAC), solution organic solvent extraction, extract concentrate mixture, general flavone content 20-90%.
(3), the Herba Scutellariae Barbatae herb is pulverized, extract with diluted alkaline 0.1-20% solution, crude extract carries out silica gel column chromatography, separates, and gets extract with the solvent eluting.
(4), the Herba Scutellariae Barbatae herb is pulverized, use water extraction, the crude extract of Herba Scutellariae Barbatae, crude extract carries out silica gel column chromatography, separation gets extract with the solvent eluting.
(5), the Herba Scutellariae Barbatae herb is pulverized, extract with diluted alkaline 0.1-20% solution, the crude extract of Herba Scutellariae Barbatae, transfer pH to 2-5 with acid, the solution organic solvent extraction, extract concentrated mixture, general flavone content 20-90%.
The effective site of Herba Scutellariae Barbatae extract is the various Chinese medicine preparation that main active is made, and it is characterized in that:
(1), the oral formulations of the Herba Scutellariae Barbatae herb extract of 10%-60% and 40%-90% pharmaceutic adjuvant composition;
(2), the injection of the Herba Scutellariae Barbatae herb extract of 0.5%-30% and 70%-99.5% pharmaceutic adjuvant composition;
Wherein, the Herba Scutellariae Barbatae herb extract is grouped into by one-tenth such as total flavones, alkaloid, steroidal, saccharides, and general flavone content is 20%-90%, total alkaloid content 0.5-10%.
Oral formulations of the present invention can be tablet, capsule, granule, drop pill, and being used for clinical dosage is to take every day by raw medicinal herbs 6-50 to restrain; Injection can be aqueous injection or injectable powder, and being used for clinical dosage is that injection every day restrains by raw medicinal herbs 3-30.
Pharmaceutic adjuvant of the present invention comprises that filler is (as mannitol, lactose, Polyethylene Glycol), binding agent (starch, microcrystalline Cellulose), disintegrating agent is (as carboxymethyl cellulose, the low hydroxypropyl cellulose that replaces), lubricant is (as Pulvis Talci, magnesium stearate), wetting agent is (as propylene glycol, ethanol), antioxidant is (as sodium pyrosulfite, sodium thiosulfate), antiseptic (benzyl alcohol) etc., they can be common doses, mix with the Herba Scutellariae Barbatae herb extract with proportioning commonly used, after Herba Scutellariae Barbatae herb extract consumption was determined, the proportioning between each pharmaceutic adjuvant can suitably be regulated as required.
The preparation concrete operations of various pharmaceutical preparatioies are as follows:
(1), takes by weighing and contain 10-60% Herba Scutellariae Barbatae herb extract by the configuration total amount, the filler of adding 40-90%, binding agent, disintegrating agent, lubricant, correctives etc., fully mix and make granule, compacting in 60-70 ℃ of dry 2-4 hour in flakes, make every to contain Herba Scutellariae Barbatae herb extract 40-240mg; Maybe with the wet granular made directly at 60-70 ℃ of dry 2-4 hour, be filled into then in the hungry area shell, make every capsules contain Herba Scutellariae Barbatae herb extract 30-180mg.
(2), take by weighing and contain 0.5-30% Herba Scutellariae Barbatae herb extract by the configuration total amount, the solvent, the antiseptic that add 70-99.5%, fully mix, add activated carbon decolorizing, filter, use less than 0.45 μ m microvoid membrane filtration, embedding after ultrafiltration, sterilized 30-60 minute, and made every ml contain Herba Scutellariae Barbatae herb extract 5-300mg for 100 ℃; Or with gained filtrate by after the standard packing, lyophilized injectable powder is made in lyophilization under vacuum condition.
(3), take by weighing and contain 10%-60% Herba Scutellariae Barbatae herb extract, add the filler, disintegrating agent, correctives of 40%-90% etc., fully mix with the 12-14 mesh sieve and make granule by the configuration total amount.At 60-70 ℃ of dry 2-4 hour, make every gram granule contain Herba Scutellariae Barbatae herb extract 100-600mg.
(4), take by weighing and contain 10%-60% Herba Scutellariae Barbatae herb extract by the configuration total amount, the filler of adding 40%-90%, antioxidant etc., heating and melting temperature (40-90 ℃) makes raw material and adjuvant fully miscible, drip and make ball, make every drop pill contain Herba Scutellariae Barbatae herb extract 4-30mg.
Can adopt water, ethanol 30-90% in the preparation method of the present invention is extraction solvent, extracting solution separates again, organic solvent extraction, enrichment, effective ingredient, like this can be, be rich in compositions such as flavonoid, steroidal, polysaccharide and fully extract with the alkaloid that contains in the Herba Scutellariae Barbatae herb.Carry out the Herba Scutellariae Barbatae ultraviolet determination routinely (referring to 2000 editions one one 89 pages of Chinese Pharmacopoeias, 33 pages of appendix) record and contain total flavones (20-90%), steroidal (1-10%), alkaloid (0.5-10%), polysaccharide (10-20%), carrying out Herba Scutellariae Barbatae HPLC routinely measures (referring to 2000 editions one one 89 pages of Chinese Pharmacopoeias, 38 pages of appendix), record scutellarin 1.5-60% etc.
The invention has the advantages that:
(1), this product is that the effective ingredient of single medicinal material is formed, and can be used for preventing or treating the various infection that influenza virus causes, as bronchitis, pneumonia etc., evident in efficacy, taking dose is little, toxic and side effects is little, steady quality is safe.
(2), preparation technology's simple economy, practicality, solvent can recycle, and is more suitable for suitability for industrialized production.Gained Herba Scutellariae Barbatae herb extract can be made various dosage forms commonly used simultaneously.
(3), owing to be that pure Chinese medicinal preparation has been avoided vaccinate or taken anaphylaxis and some toxic and side effects that Western medicine brings, can satisfy the demand of different patients' preventions and treatment influenza virus.
The Herba Scutellariae Barbatae extract that the present invention makes has therapeutical effect to influenza infection, is described as follows by pharmacodynamics test: sample code name wherein derives from the content that embodiment 1-3 is explained respectively.
Get the sample that embodiment 1-3 obtains, be determined at intravital antiviral activity.
Influenza virus Mus lung adapted strain (A/PR/8/34) (purchase in the Chinese Academy of Sciences virus institute) is repeated to go down to posterity and detect the blood clotting titre, select the above allantoic fluid of titre 1:640 to make experiment seed culture of viruses stock solution, treating excess syndrome is tested virus and is planted stock solution, is 1/20,1/50,1/,100 three dilution factor with the dilution of 1460 culture fluid.Aseptic subpackaged freezing preservation.Choose 24 of 19-23g Kunming mouses, be divided into 3 groups at random, 8 every group.With mice with etherization after, respectively collunarium infective virus kind stock solution and four dilution viral liquid, every Mus 50ul.The time of symptoms of pneumonia and the natural law of infection back dead mouse appear in the record mouse infection time, and selection causes that the viral liquid of mice 60-90% death is used for formal test and infects, and determines that 1/50 virus sample infecting mouse is as the viral infection model.
100 of body weight 15～19g Kunming mouses, male and female half and half are divided into 10 groups at random, are respectively blank group, model control group, A, B, C, D, E, F group.Except that the blank group, each organizes the viral dilution drop nose infection of mice with selected concentration, every Mus 0.05ml.The 5th day began to continue administration 7 days behind the self-infection, and dosage is 10g crude drug/kg body weight, observed mouse invasion rate and survival state, and the survival rate and the time-to-live of each treated animal are compared, and the results are shown in following table.
Annotate: * compares with model control group, and card side is probabilistic method assay p＜0.05 accurately;
Composite score, Herba Scutellariae Barbatae extract C, B, D, H are obvious to influenza virus mice infected therapeutical effect, can obviously improve survival rate.
The specific embodiment
Among the embodiment, used ethanol is pharmaceutical grade, and sodium hydroxide, sulphuric acid are analytical pure, and other organic solvent is a technical grade.The Herba Scutellariae Barbatae medical material place of production is Henan, Hebei, macroporous resin is available from Chemical Plant of Nankai Univ., the Herba Scutellariae Barbatae ultraviolet determination is (referring to 2000 editions one one 89 pages of Chinese Pharmacopoeias, 33 pages of appendix) record and contain total flavones, Herba Scutellariae Barbatae HPLC measures (referring to 2000 editions one one 89 pages of Chinese Pharmacopoeias, 38 pages of appendix), record scutellarin etc.
Below in conjunction with preferred embodiment, the present invention will be further described, to being described in detail as follows according to the specific embodiment provided by the invention; For simple and purpose clearly, hereinafter appropriate omission the description of known technology, in order to avoid those unnecessary details influences are to the description of the technical program.
Embodiment 1:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram, with 18 times of water gaging heating extraction 2 times, crude extract (A) that must Herba Scutellariae Barbatae.Last macroporous resin column (D101 type or AB8) is separated, and receives the not medicinal liquid of absorption, concentrate 12g, water and Different concentrations of alcohol (30-90%) eluting.Collect each several part, after the washing part drying 26g, the 30-60% ethanol 67g that partly gets dry extract, 80-90% ethanol part ethanol part 8g.Survey total flavones, 30-60% ethanol elution part scutellarin content the highest (4.2%).Get mixture, mixture contains total flavones 33.8%, total alkaloid content 1.5%, steroidal content 1.8%, contents of saccharide 10.2%.
Embodiment 2:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram,, get the crude extract (B) of Herba Scutellariae Barbatae with 18 times of amount 50% ethanol extractions 2 times (heating or percolation).Last macroporous resin column (D101 type or AB8) is separated, and receives the not medicinal liquid of absorption, concentrate 15g (F), water and Different concentrations of alcohol (30-90%) eluting.Collect each several part, after the washing part drying 35g (G), the 30-60% ethanol 79g (H) that partly gets dry extract, 80-90% ethanol part ethanol part 14g.Survey total flavones, 30-60% ethanol elution part scutellarin content the highest (10.5%).Get mixture 35g, mixture contains total flavones 63.1%, total alkaloid content 2.1%, steroidal content 1.0%, contents of saccharide 5.2%.
Embodiment 3:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram,, merge 2 times extracting solution with 18 times of amount 50% ethanol extractions (heating or percolation) 2 times, decompression recycling ethanol, crude extract that must Herba Scutellariae Barbatae, medicinal residues discard.Crude extract is regulated pH to 7-8 with 5%NaOH liquid, gets alkaline medicinal liquid, with chloroform (or petroleum ether) extraction.Tell the solvent layer, discard, water layer reuse 5% sulphuric acid is transferred pH to 2-4, place, centrifugal, acidic precipitation is standby, get 30g (C) after the drying, solution extracts with chloroform (or petroleum ether), layering, water layer, concentrate 86g (E), the solvent layer concentrate extract, after the drying 40g (D), with the acidic precipitation mix homogeneously, get mixture 70g.Mixture contains total flavones 59.7%, total alkaloid content 3.8%, steroidal content 2.0%, contents of saccharide 4.2% etc.
Embodiment 4:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram,, merge 2 times extracting solution with 18 times of amount 50% ethanol extractions (heating or percolation) 2 times, decompression recycling ethanol, crude extract that must Herba Scutellariae Barbatae, medicinal residues discard.Crude extract is regulated pH to 7-8 with 1%NaOH liquid, gets alkaline medicinal liquid, with ethyl acetate (or n-butyl alcohol) extraction.Tell the solvent layer, discard, water layer reuse 1% sulphuric acid is transferred pH to 2-4, place, centrifugal, acidic precipitation is standby, get 24g after the drying, solution extracts with ethyl acetate (or n-butyl alcohol), layering, water layer discarded, the solvent layer concentrate extract, get 48g after the drying,, get mixture 72g with the acidic precipitation mix homogeneously.Mixture contains total flavones 61.8%, total alkaloid content 2.5%, steroidal content 2.4%, contents of saccharide 3.9% etc.
Embodiment 5:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram,, merge 2 times extracting solution with 18 times of amount 50% ethanol extractions (heating or percolation) 2 times, decompression recycling ethanol, crude extract that must Herba Scutellariae Barbatae, medicinal residues discard.Crude extract is regulated pH to 7-8 with 3%NaOH liquid, gets alkaline medicinal liquid, with petroleum ether (or ethyl acetate) extraction.Tell the solvent layer, discard, water layer reuse 3% sulphuric acid is transferred pH to 2-4, place, centrifugal, acidic precipitation is standby, get 26g after the drying, solution extracts with n-butyl alcohol (or ethyl acetate), layering, water layer discarded, the solvent layer concentrate extract, get 47g after the drying,, get mixture 73g with the acidic precipitation mix homogeneously.Mixture contains total flavones 58.8%, total alkaloid content 2.8%, steroidal content 2.4%, contents of saccharide 3.5% etc.
Embodiment 6:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram,, merge 2 times extracting solution with 18 times of amount 50% ethanol extractions (heating or percolation) 2 times, decompression recycling ethanol, crude extract that must Herba Scutellariae Barbatae, medicinal residues discard.Crude extract is regulated pH to 7-8 with 5%NaOH liquid, gets alkaline medicinal liquid, with chloroform (or ethyl acetate) extraction.Tell the solvent layer, discard, water layer reuse 5% sulphuric acid is transferred pH to 2-4, place, centrifugal, acidic precipitation is standby, get 33g after the drying, solution extracts with petroleum ether (or n-butyl alcohol), layering, water layer discarded, the solvent layer concentrate extract, get 32g after the drying,, get mixture 65g with the acidic precipitation mix homogeneously.Mixture contains total flavones 60.9%, total alkaloid content 3.6%, steroidal content 2.8%, contents of saccharide 3.1% etc.
Embodiment 7:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram,, merge 2 times extracting solution with 18 times of amount 50% ethanol extractions 2 times, decompression recycling ethanol, crude extract that must Herba Scutellariae Barbatae, medicinal residues discard.Crude extract is regulated pH to 7-8 with 5%NaOH liquid, gets alkaline medicinal liquid, with petroleum ether (or ethyl acetate) extraction.Tell the solvent layer, discard, water layer reuse 5% sulphuric acid is transferred pH to 2-4, places, and is centrifugal, acidic precipitation is standby, gets 22g after the drying, and solution extracts with ether (or n-butyl alcohol), layering, water layer discarded, the solvent layer concentrate extract, after the drying 43g, with the acidic precipitation mix homogeneously, mixture 65g.Mixture contains total flavones 60.2%, total alkaloid content 1.6%, steroidal content 1.4%, contents of saccharide 4.7% etc.
Embodiment 8:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram,, merge 2 times extracting solution with 18 times of amount 50% ethanol extractions 2 times, decompression recycling ethanol, crude extract that must Herba Scutellariae Barbatae, medicinal residues discard.Crude extract is regulated pH to 7-8 with 3%NaOH liquid, gets alkaline medicinal liquid, filters, discard precipitate, supernatant is transferred pH to 2-4 with 3% sulphuric acid, places, centrifugal, acidic precipitation is standby, gets 25g after the drying, solution extracts with chloroform (or petroleum ether), layering, water layer discarded, the solvent layer concentrate extract, get 46g after the drying,, get mixture 71g with the acidic precipitation mix homogeneously.Mixture contains total flavones 58.6%, total alkaloid content 1.7%, steroidal content 2.0%, contents of saccharide 4.4% etc.
Embodiment 9:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram,, merge 2 times extracting solution with 18 times of amount 50% ethanol extractions 2 times, decompression recycling ethanol, crude extract that must Herba Scutellariae Barbatae, medicinal residues discard.Crude extract is regulated pH to 7-8 with 5%NaOH liquid, gets alkaline medicinal liquid, filters, discard precipitate, supernatant is transferred pH to 2-4 with 5% sulphuric acid, places, centrifugal, acidic precipitation is standby, gets 34g after the drying, solution extracts with ethyl acetate (or n-butyl alcohol), layering, water layer discarded, the solvent layer concentrate extract, get 45g after the drying,, get mixture 79g with the acidic precipitation mix homogeneously.Mixture contains total flavones 56.2%, total alkaloid content 1.3%, steroidal content 1.8%, contents of saccharide 4.9% etc.
Embodiment 10:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram,, merge 2 times extracting solution with 18 times of amount 50% ethanol extractions 2 times, decompression recycling ethanol, crude extract that must Herba Scutellariae Barbatae, medicinal residues discard.Crude extract is regulated pH to 7-8 with 7%NaOH liquid, gets alkaline medicinal liquid, filters, discard precipitate, supernatant is transferred pH to 2-4 with 7% sulphuric acid, places, centrifugal, acidic precipitation is standby, gets 32g after the drying, solution extracts with isopropyl alcohol (or ether), layering, water layer discarded, the solvent layer concentrate extract, get 43g after the drying,, get mixture 75g with the acidic precipitation mix homogeneously.Mixture contains total flavones 54.3%, total alkaloid content 1.8%, steroidal content 2.0%, contents of saccharide 5.0% etc.
Embodiment 11:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram, extract 2 times, merge 2 times extracting solution with 18 times of amount 1% sodium hydroxide (or sodium carbonate) solution, concentrating under reduced pressure, crude extract that must Herba Scutellariae Barbatae, medicinal residues discard.Silicagel column on the crude extract with chloroform (or ethyl acetate, methanol) eluting, is collected each several part, carries out qualitative identification with magnesium powder-hydrochloric acid, merges positive part, and concentrating under reduced pressure must mixture 30g.Mixture contains total flavones 85%, steroidal content 1.6% etc.
Embodiment 12:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram, extract with 18 times of water gagings, get the crude extract of Herba Scutellariae Barbatae, polyamide column on the crude extract, water and Different concentrations of alcohol eluting, collect each several part, carry out qualitative identification with magnesium powder-hydrochloric acid, merge positive part, concentrating under reduced pressure, get mixture 50g, mixture contains total flavones 65.7%, total alkaloid content 1.3%, contents of saccharide 5.3% etc.
Embodiment 13:
The Herba Scutellariae Barbatae herb is pulverized, taken by weighing 1 kilogram, extract with 18 times of amount 50% ethanol (heating or percolation), get the crude extract of Herba Scutellariae Barbatae, polyamide column on the crude extract, water and Different concentrations of alcohol eluting, collect each several part, carry out qualitative identification with magnesium powder-hydrochloric acid, merge positive part, concentrating under reduced pressure, get mixture 57g, mixture contains total flavones 68.2%, total alkaloid content 1.8%, steroidal content 1.3%, contents of saccharide 4.5% etc.
Embodiment 14:
The Herba Scutellariae Barbatae herb is pulverized, take by weighing 1 kilogram, extract with 18 times of amount 1% sodium hydroxide (or sodium carbonate) solution, get the crude extract of Herba Scutellariae Barbatae, transfer pH to 2-4 with 5% sulphuric acid, solution is with organic solvent chloroform (ethyl acetate or butanols) extraction, extract concentrate mixture 58g, mixture contains total flavones 64.8%, steroidal content 1.1%, contents of saccharide 4.2% etc.
Embodiment 15:
The Herba Scutellariae Barbatae herb is pulverized, take by weighing 1 kilogram, extract, get the crude extract of Herba Scutellariae Barbatae with 18 times of amount 30% ethanol (heating or percolation), be dissolved in water, solution organic solvent petroleum ether extraction, petroleum ether layer discards, and water layer adds ethanol, make the alcohol amount of containing reach 75% ethanol precipitate with ethanol, filter, discard precipitate, supernatant, concentrate and receive alcohol, get extractum, be dissolved in water, with counter-current distribution method continuous extraction 6 hours, aqueous solvent-ethyl acetate, extract concentrate mixture 52g, mixture contains total flavones 63.5%, steroidal content 1.2%, contents of saccharide 4.5% etc.
Embodiment 16:
The Herba Scutellariae Barbatae herb is pulverized, take by weighing 1 kilogram, extract, get the crude extract of Herba Scutellariae Barbatae with 18 times of amount 30% ethanol (heating or percolation), be dissolved in water, solution organic solvent petroleum ether extraction, petroleum ether layer discards, and water layer adds ethanol, make the alcohol amount of containing reach 75% ethanol precipitate with ethanol, filter, discard precipitate, supernatant, concentrate and receive alcohol, get extractum, be dissolved in water, with counter-current distribution method continuous extraction 6 hours, aqueous solvent-n-butyl alcohol, extract concentrate mixture 55g, mixture contains total flavones 64.6%, steroidal content 1.5%, contents of saccharide 4.7% etc.
Embodiment 17: preparation process, dosage form: tablet
Prescription:
Herba Scutellariae Barbatae mixture 200g
Microcrystalline Cellulose (PH-301) 120g
Low-substituted hydroxypropyl cellulose 12g
Citric acid 4g
Mannitol 20g
Micropowder silica gel 10g
Stearic acid 4g
Pulvis Talci 30g
Fructus Citri tangerinae essence is an amount of
Make 1000
Above-mentioned raw materials fully mixed make granule, compacting in 60-70 ℃ of dry 2-4 hour in flakes, make every to contain Herba Scutellariae Barbatae herb extract 40-240mg.
Embodiment 18: preparation process, dosage form: capsule
Prescription:
Herba Scutellariae Barbatae mixture 150g
Microcrystalline Cellulose 90g
Micropowder silica gel 23g
Starch 25g
Stearic acid 2g
Pulvis Talci 10g
Make 1000 capsules
The wet granular made directly at 60-70 ℃ of dry 2-4 hour, is filled in the hungry area shell then, makes every capsules contain Herba Scutellariae Barbatae herb extract 30-180mg.
Embodiment 19: preparation process, dosage form: granule
Prescription:
Herba Scutellariae Barbatae mixture 500g
Lactose 350g
Carboxymethyl starch sodium 135g
Protein sugar 5g
Citric acid 10g
Fructus Citri tangerinae essence is an amount of
Make the 1000g granule
Mix with the 12-14 mesh sieve and make granule.At 60-70 ℃ of dry 2-4 hour, make every gram granule contain Herba Scutellariae Barbatae herb extract 100-600mg.
Embodiment 20: preparation process, dosage form: drop pill
Prescription:
Herba Scutellariae Barbatae mixture 20g
Macrogol 4000 10g
Polyethylene glycol 6000 30g
Sodium pyrosulfite is an amount of
Make 1000 drop pill
Heating and melting temperature (40-90 ℃) makes raw material and adjuvant fully miscible, drips to make ball, makes every drop pill contain Herba Scutellariae Barbatae herb extract 4-30mg.
Embodiment 21: preparation process, dosage form: water preparation
Prescription:
Herba Scutellariae Barbatae mixture 10g
2 milliliters of benzyl alcohol
300 milliliters of propylene glycol
Sodium carbonate is an amount of
Water for injection is an amount of
Make 1000 milliliters (liquid drugs injections)
Above-mentioned raw materials is fully mixed, add activated carbon decolorizing, filter, use less than 0.45um microvoid membrane filtration, embedding after ultrafiltration was sterilized 30-60 minute, and was made every ml contain Herba Scutellariae Barbatae herb extract 5-300mg for 100 ℃.
Embodiment 22: preparation process, dosage form: injectable powder
Prescription:
Herba Scutellariae Barbatae mixture 10g
2 milliliters of benzyl alcohol
Sodium carbonate is an amount of
Water for injection is an amount of
Make 50g (powder pin)
By after the standard packing, the dry powder injection is made in lyophilization under vacuum condition with gained filtrate.
Claims (8)
1. a Herba Scutellariae Barbatae extract that is used for the treatment of influenza infection is characterized in that Herba Scutellariae Barbatae extract comprises total flavones, total alkaloids, steroidal and saccharide, and wherein general flavone content is that 20%-90% and total alkaloid content are 0.5-10%.
2. by the described extract of claim 1, it is characterized in that described total flavones contains carthamin, 5,7,4 '-trihydroxy-8-methoxy flavone, isocarthamidin, scutellarein and scutellarin;
Wherein 5,7,4 '-trihydroxy-8-methoxy flavone 0.1mg/Kg-400mg/Kg has inhibitory action to influenza virus.
3. the preparation method of the described Herba Scutellariae Barbatae extract of claim 1 is characterized in that: the A solvent extraction: the Herba Scutellariae Barbatae herb is pulverized with solvent orange 2 A extracted under heating or percolation, get crude extract; The B solvent purification: crude extract adopts the B solvent to get mixture through separation and purification, enrichment, and recording general flavone content is that 20%-90% and total alkaloid content are 0.5-10%; Method comprises:
A. liquid-liquid extraction method: crude extract adopts counter-current distribution method to extract continuously with solvent B must extract extract in 6 hours;
B. acid precipitation method: crude extract is transferred pH6-9 through diluted alkaline, with or without the B solvent extraction, water layer is transferred pH2-5 with diluted acid, the acidic precipitation thing; Water layer reuse B solvent extraction, extract, with acidic precipitation thing and extract merge mixture; Or
C. absorb-elute method: crude extract, is collected each component evaporate to dryness and is got extract with solvent B eluting through macroporous resin column or silica gel column chromatography or polyamide column method,
Wherein, described solvent orange 2 A is selected from water, 0.1-20% dilute alkaline soln, 30-90% ethanol, methanol, ethyl acetate and acetone; Be selected from dichloromethane, chloroform, butanols, isopropyl alcohol, n-butyl alcohol, petroleum ether, ether, water-ethyl acetate, 0.1-20% dilute acid soln, 0.1-20% dilute alkaline soln, water-n-butyl alcohol and ethyl acetate with described solvent B.
4. preparation method according to claim 3 is characterized in that described diluted acid is selected from hydrochloric acid, sulphuric acid, phosphoric acid, oxalic acid and acetic acid; Be selected from sodium hydroxide, potassium hydroxide, sodium carbonate and sodium bicarbonate with described diluted alkaline.
5. preparation method according to claim 3 is characterized in that used macroporous resin model is selected from D-101, AB-8 type and NK-9.
6. comprise the Chinese medicine preparation of claim 1 or 2 described Herba Scutellariae Barbatae extracts, it is characterized in that, this Chinese medicine preparation is:
(1), the oral formulations of the Herba Scutellariae Barbatae extract of 10%-60% and 40%-90% pharmaceutic adjuvant composition; Or
(2), the injection of the Herba Scutellariae Barbatae extract of 0.5%-30% and 70%-99.5% pharmaceutic adjuvant composition.
7. Chinese medicine preparation as claimed in claim 6 is characterized in that described oral formulations is tablet, capsule, granule or drop pill; With described injection be aqueous injection or lyophilized injectable powder.
8. Chinese medicine preparation as claimed in claim 6 is characterized in that described pharmaceutic adjuvant is selected from filler, binding agent, disintegrating agent, lubricant and antioxidant.
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| CN102688291B (en) * | 2012-06-01 | 2014-07-09 | 康阳润和（北京）医药科技有限公司 | Sculellaria barbata general flavone compound, oral preparations prepared from Sculellaria barbata general flavone compound and preparation methods respectively for Sculellaria barbata general flavone compound and oral preparations |
| CN104277086B (en) * | 2013-07-12 | 2018-08-28 | 河北以岭医药研究院有限公司 | Scutellarin extracting method in a kind of Sculellaria barbata |
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