CN1723955A - Extractive of rhizome belamcandae, prepn. method and use thereof - Google Patents
Extractive of rhizome belamcandae, prepn. method and use thereof Download PDFInfo
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- CN1723955A CN1723955A CN 200510085620 CN200510085620A CN1723955A CN 1723955 A CN1723955 A CN 1723955A CN 200510085620 CN200510085620 CN 200510085620 CN 200510085620 A CN200510085620 A CN 200510085620A CN 1723955 A CN1723955 A CN 1723955A
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Abstract
A extract series of belamcanda rhizome, including the flavone, flvonoside and flavone aglycon of belamcanda, its extracting process and its application in preparing the medicines for preventing and treating the diseases in respiratory system are disclosed.
Description
Technical field
The present invention relates to Rhizoma Belamcandae extract, relate to general flavone from blackberry lily (forming) extract, general flavone from blackberry lily glucoside extract, general flavone from blackberry lily aglycon extract particularly by flavonoid glycoside and flavone aglycone, preparation method, reach iridin (iridin), irigenine (irigenin), general flavone from blackberry lily glucoside extract, general flavone from blackberry lily aglycon extract, the application of extractive of general flavone from blackberry lily in the medicine of preparation treatment or prevention respiratory system disease, treat or prevent the application in the medicine aspect acute and chronic pharyngolaryngitis, tonsillitis, the pneumonia in preparation particularly.
Background technology
Rhizoma Belamcandae, the dry rhizome of irides Rhizoma Belamcandae Belamcanda chinensis (L.) DC. is for pharmacopeia is recorded kind, beginning is stated from Shennong's Herbal, and it is cold in nature, bitter in the mouth, the effect of tool heat-clearing and toxic substances removing, sore-throat relieving expectorant, the blood detumescence of loosing cures mainly laryngopharynx swelling and pain, productive cough asthma.Rhizoma Belamcandae is called the key medicine of pharyngalgia " treatment sore throat " by Compendium of Material Medica, in the many classic prescriptions monographs of China, have as " Shengji Zonglu ", " hospital's great achievement opinion ", " prescriptions worth thousand gold " etc. more and to record.The compound recipe of treatment throat illness that with the Rhizoma Belamcandae is monarch drug is more, in the treatment throat illness side that " successive dynasties well-known doctor good recipe note " book is included, has in 1/4th the square medicine and contains Rhizoma Belamcandae.Rhizoma Belamcandae is at home as Chinese medicine, modern times are mainly used in the treatment diseases in respiratory system clinically, for example upper respiratory tract infection, acute/chronic pharyngitis, tonsillitis, chronic sinusitis, bronchitis, asthma, emphysema, pulmonary heart disease, laryngopharynx swelling and pain and abundant expectoration cough with asthma person etc.
The modern pharmacology result of study of Rhizoma Belamcandae shows that Rhizoma Belamcandae has effects such as antiinflammatory, antiviral, antifungal, antiallergic, excited pharyngolaryngeal mucosa and promotion salivation, and it mainly contains isoflavonoid.Rhizoma Belamcandae 70% ethanol extract has the obvious suppression effect to inflammatory.Rhizoma Belamcandae can significantly suppress the increasing of mouse skin capillary permeability due to the histamine, can obviously suppress the development of rat hyaluronidase foot edema.Rhizoma Belamcandae decoct or preserved material have inhibitory action external to common pathogenic dermatophytes.Rhizoma Belamcandae water decoction or injection suppress influenza virus in Embryo Gallus domesticus, suppress or delay the cytopathic effect of influenza virus, parainfluenza virus, rhinovirus, adenovirus, Coxsackie virus, echovirus and herpesvirus in tissue culture.The irigenine cytopathy activity that resisiting influenza virus, delay Coxsackie virus, echovirus cause in tissue culture.
The inventor is by a large amount of experimentatioies, the effective site and the effective ingredient of Rhizoma Belamcandae have been found, and then general flavone from blackberry lily (forming) extract, general flavone from blackberry lily glucoside extract, general flavone from blackberry lily aglycon extract are provided by flavonoid glycoside and flavone aglycone, and iridin (iridin), irigenine (irigenin) and the application of above-mentioned three kinds of extracts in the medicine of preparation treatment or prevention respiratory system disease, especially treating or preventing application aspect acute and chronic pharyngolaryngitis, tonsillitis, the pneumonia.
Summary of the invention
The invention provides general flavone from blackberry lily (forming) extract by flavonoid glycoside and aglycon, wherein, in iridin, 100%＞Rhizoma Belamcandae isoflavone weight 〉=50%, be preferably 100%＞Rhizoma Belamcandae isoflavone weight 〉=80%, the ratio between iridin, the irigenine is 1: (0.1-1).
The invention provides the general flavone from blackberry lily glucoside extract, wherein, in iridin, 100%＞Rhizoma Belamcandae isoflavone weight 〉=50% is preferably 100%＞Rhizoma Belamcandae isoflavone weight 〉=80%; The weight of 100%＞iridin is 〉=10%, and the weight that is preferably 100%＞iridin is 〉=25.
The invention provides the general flavone from blackberry lily aglycon extract, wherein, in irigenine, 100%＞Rhizoma Belamcandae isoflavone weight 〉=50% is preferably 100%＞Rhizoma Belamcandae isoflavone weight 〉=80%; The weight of 100%＞irigenine is 〉=10%, is preferably 100%＞irigenine weight 〉=25%.
The invention provides above-mentioned three kinds of preparation method of extract.
The invention provides the application of above-mentioned three kinds of extracts in the medicine of preparation treatment or prevention respiratory system disease, especially in treatment or prevent application aspect acute and chronic pharyngolaryngitis, tonsillitis, the pneumonia.
The pharmaceutical composition that to the invention provides with above-mentioned any extract be active component.
The invention provides the application in the medicine of preparation treatment or prevention respiratory system disease of iridin or irigenine, especially in treatment or prevent application aspect acute and chronic pharyngolaryngitis, tonsillitis, the pneumonia.
The invention provides with iridin or irigenine is the pharmaceutical composition of active component.
The preparation method of extractive of general flavone from blackberry lily provided by the invention is:
Rhizoma Belamcandae medical material water extraction concentrates the back and adds ethanol precipitation, and supernatant reclaims ethanol, goes up polyamide column again, and first water eluting again with the finite concentration ethanol elution, is collected alcohol eluen, reclaims solvent, drying, promptly.
Extracting method of the present invention is preferably: get water extraction 2-4 time of dry Rhizoma Belamcandae, water consumption is 5-30 times, and each time of extracting is 30-120 minute, it is 1.00-1.25 that merging filtrate, filtrate decompression are concentrated into density, and adding ethanol to determining alcohol is 60-90%, precipitate 24 hours down in 4 ℃, filter; Decompression filtrate recycling ethanol, behind thin up to the 10 times volume, on the polyamide column handled well, applied sample amount (being equivalent to the crude drug amount) with the ratio of polyamide consumption is: (1-4): 1 (w/v), 2-10 column volume of first water eluting discards; Continue to collect eluent with 2-10 column volume of 70-100% ethanol elution, decompression recycling ethanol is drying to obtain.
Extracting method of the present invention is more preferably: get dry Rhizoma Belamcandae water reflux, extract, 3 times, water consumption is 10 times, each time of extracting is 60-120 minute, merging filtrate, it is 1.08 (100 ℃) that filtrate decompression is concentrated into density, adding ethanol to determining alcohol is 80%, precipitates 24 hours down in 4 ℃, filters; Decompression filtrate recycling ethanol, behind thin up to the 10 times volume, on the polyamide column handled well, applied sample amount (being equivalent to the crude drug amount) with the ratio of polyamide consumption is: 2: 1 (w/v), 10 column volumes of first water eluting discard; Continue to collect eluent with 5 column volumes of 95% ethanol elution, decompression recycling ethanol is drying to obtain.
The preparation method of general flavone from blackberry lily glucoside extract provided by the invention is:
The certain density ethanol extraction of Rhizoma Belamcandae medical material, extracting solution reclaims ethanol, last macroporous resin column, first water, low-concentration ethanol eluting again with the high concentration ethanol eluting, are collected alcohol eluen, reclaim solvent, last polyamide column decolouring or convection drying, promptly.
Extracting method of the present invention is preferably: get dry Rhizoma Belamcandae with the ethanol extraction of 50%-100% 2-4 time, solvent load be 5-30 doubly, each time of extracting is 30-120 minute, filtration; Decompression filtrate recycling ethanol, behind thin up to the 10 times volume, on the macroporous resin column handled well, applied sample amount (being equivalent to the crude drug amount) with the ratio of macroporous resin consumption is: (1-10): 1 (w/v), 1-10 column volume of first water eluting, 1-10 column volume of reuse low-concentration ethanol eluting, again with the ethanol elution 1-10 column volume of high concentration, collect high concentration ethanol eluent decompression recycling ethanol, dry or go up the polyamide column decolouring, promptly get content more than or equal to 50% general flavone from blackberry lily glycosides.
Extracting method of the present invention is more preferably: get dry Rhizoma Belamcandae with 80% ethanol extraction 3 times, solvent load is 10 times, and each time of extracting is 60-120 minute, filters; Decompression filtrate recycling ethanol, behind thin up to the 10 times volume, on the AB-8 macroporous resin column handled well, applied sample amount (being equivalent to the crude drug amount) with the ratio of macroporous resin consumption is: (3-6): 1 (w/v), 3 column volumes of elder generation's water eluting, 3 column volumes of reuse 10%-30% ethanol elution, last 5 column volumes of ethanol elution with 40%-60%, collect a part of eluent in back, decompression recycling ethanol, the polyamide column of handling well on the aqueous solution (consumption: the 1-10 of crude drug amount doubly), 2-3 column volume of elder generation's water eluting, the ethanol elution 3-5 column volume of reuse 30%-40% is collected alcohol eluen, reclaim solvent, be drying to obtain content more than or equal to 80% general flavone from blackberry lily glycosides.
The preparation method of general flavone from blackberry lily aglycon extract provided by the invention is:
The certain density ethanol extraction of Rhizoma Belamcandae medical material, extracting solution reclaims ethanol, and direct (or through hydrolysis) goes up polyamide column, the ethanol elution of first water, low concentration, the ethanol elution of reuse high concentration is collected the high concentration ethanol eluent, reclaims solvent, drying, promptly.
Extracting method of the present invention is preferably: get dry Rhizoma Belamcandae with the ethanol extraction of 50%-100% 2-4 time, solvent load be 5-30 doubly, each time of extracting is 30-120 minute, filtration; Decompression filtrate recycling ethanol, behind the thin up, with acid or enzyme hydrolysis, on the polyamide column handled well, applied sample amount (being equivalent to the crude drug amount) with the ratio of polyamide consumption is: (1-4): 1 (w/v), 2-10 column volume of first water eluting, 2-10 column volume of reuse 20-40% ethanol elution, with the ethanol elution 2-10 column volume of 50%-95%, collect 50%-95% ethanol elution decompression recycling ethanol at last, be drying to obtain.
Extracting method of the present invention most preferably is: get dry Rhizoma Belamcandae with 80% ethanol extraction 3 times, solvent load is 10 times, and each time of extracting is 60-120 minute, filters; Decompression filtrate recycling ethanol, behind thin up to the 10 times volume, add Snailase (being equivalent to the heavy 0.001-0.5 of medical material doubly), in 37 ℃ of following hydrolysis 24 hours, hydrolyzed solution filters, the polyamide column of handling well on the precipitate, applied sample amount (being equivalent to the crude drug amount) with the ratio of polyamide consumption is: (1-4): 1 (w/v), 3 column volumes of elder generation's water eluting, 3 column volumes of reuse 20-40% ethanol elution, with 5 column volumes of ethanol elution of 50%-95%, collect 50%-95% ethanol elution decompression recycling ethanol at last, be drying to obtain.
The preparation method of iridin of the present invention is: general flavone from blackberry lily extracts with systematic solvent extraction, gets its n-butanol extraction partly, separates and purification with silica gel column chromatography.
The preparation method of irigenine of the present invention is: general flavone from blackberry lily extracts with systematic solvent extraction, gets its ethyl acetate extraction partly, separates and purification with silica gel column chromatography.
Iridin provided by the invention or irigenine are when being used for respiratory system disease, and using dosage is 1-1000mg/ days, are preferably 5-500mg/ days, more preferably 20-200mg/ days.
Above-mentioned three kinds of extracts provided by the invention are when being used for respiratory system disease, and using dosage is 1-1000mg/ days, is preferably 5-500mg/ days, more preferably 20-200mg/ days.
Pharmaceutical composition provided by the invention, can prepare by this area conventional method also can be by oral, Sublingual, percutaneous, muscle or administrations such as subcutaneous, mucocutaneous or vein.Oral formulations can be made as tablet, capsule, granule, chewing agent, pill, suspension, solution etc., non-intestinal drug delivery agent can be made dosage forms such as injection, freeze-dried powder, and topical can be made as cream, ointment, patch, spray etc.But be not limited to this.
With iridin or irigenine is the pharmaceutical composition of active component, and dosage unit is 1-1000mg, is preferably 5-500mg, more preferably 20-200mg.
With general flavone from blackberry lily glucoside extract, general flavone from blackberry lily aglycon extract, extractive of general flavone from blackberry lily is the pharmaceutical composition of active component, and dosage unit is 1-1000mg, is preferably 5-500mg, more preferably 20-200mg.
The inventor has confirmed that by following test above-mentioned three kinds of extracts, iridin, irigenines have the effect of treatment or prevention respiratory system disease, especially in treatment or prevent effect aspect acute and chronic pharyngolaryngitis, tonsillitis, the pneumonia, but be not limited to this test.
The specific embodiment
The preparation of preparation example 1. general flavone from blackberry lily
Get Rhizoma Belamcandae medical material 20kg, extract 3 times with 10 times of water gagings, the time of extracting is 90 minutes at every turn, filters merging filtrate, and it is 1.04 (100 ℃) that filtrate decompression is concentrated into density, and adding ethanol to determining alcohol is 70%, precipitates 24 hours down in 4 ℃, filters; Decompression filtrate recycling ethanol, behind thin up to the 10 times volume, last polyamide column (120L), earlier with 10 bed volumes of water elution (1200L), again with about 5 bed volumes of 95% ethanol elution (600L), collect this part eluent, concentrate drying obtains belamcanda chinensis total isoflavone 498g (yield: 2.5%).After testing, isoflavone levels is 73% (in iridin) in this extract, wherein contains iridin 15.4%.Irigenine content is 4.6%.
The preparation of preparation example 2. general flavone from blackberry lily
Get Rhizoma Belamcandae medical material 20kg, extract 3 times with 10 times of water gagings, the time of extracting is 120 minutes at every turn, filters merging filtrate, and it is 1.08 (100 ℃) that filtrate decompression is concentrated into density, and adding ethanol to determining alcohol is 80%, precipitates 24 hours down in 4 ℃, filters; Decompression filtrate recycling ethanol, behind thin up to the 10 times volume, last polyamide column (120L), earlier with 10 bed volumes of water elution (1200L), again with about 5 bed volumes of 75% ethanol elution (600L), collect this part eluent, concentrate drying obtains belamcanda chinensis total isoflavone 498g (yield: 2.5%).After testing, isoflavone levels is 81% (in iridin) in this extract, wherein contains iridin 19.8%.Irigenine content is 5.1%.
The preparation of preparation example 3. general flavone from blackberry lily glycosides
Get Rhizoma Belamcandae medical material 20kg, the ethanol extraction with 80% 3 times, solvent load are 10 times, and each time of extracting is 120 minutes, filters; Decompression filtrate recycling ethanol, behind thin up to the 10 times volume, on the AB-8 macroporous resin column (120L) handled well, earlier with 3 bed volumes of water elution (360L), about 3 bed volumes of 25% ethanol elution (360L) are again with 5 column volumes of ethanol elution (600L) of 40%, collect this 40% ethanol part eluent, decompression recycling ethanol, concentrate drying obtains belamcanda chinensis total isoflavone glycosides 339g (yield: 1.7%).After testing, isoflavone levels is 64% (in iridin) in this extract, and wherein iridin content is 19.3%.
The preparation of preparation example 4. general flavone from blackberry lily glycosides
Get Rhizoma Belamcandae medical material 20kg, the ethanol extraction with 80% 3 times, solvent load are 10 times, and each time of extracting is 120 minutes, filters; Decompression filtrate recycling ethanol, behind thin up to the 10 times volume, on the AB-8 macroporous resin column (120L) handled well, earlier with 3 bed volumes of water elution (360L), about 3 bed volumes of 25% ethanol elution (360L), again with 5 column volumes of ethanol elution (600L) of 40%, collect this 40% ethanol part eluent, decompression recycling ethanol, the polyamide column of handling well on the aqueous solution (120L), elder generation's water 2 column volumes of eluting (240L), reuse 3 column volumes of 40% ethanol elution (360L) are collected alcohol eluen, reclaim solvent, concentrate drying obtains belamcanda chinensis total isoflavone glycosides 306g (yield: 1.5%).After testing, isoflavone levels is 83% (in iridin) in this extract, and wherein iridin content is 28.9%.
The preparation of preparation example 5. general flavone from blackberry lily aglycons
Get dry Rhizoma Belamcandae with 80% ethanol extraction 3 times, solvent load is 10 times, and each time of extracting is 120 minutes, filters; Decompression filtrate recycling ethanol, behind thin up to the 4 times volume, adding hydrochloric acid to concentration is hydrochloric acid 6%, heating hydrolysis 3 hours, hydrolyzed solution filters, the polyamide column of handling well on the precipitate (120L), 3 column volumes of first water eluting (360L), reuse 3 column volumes of 30% ethanol elution (360L), at last with 5 column volumes of ethanol elution (600L) of 95%, collect 95% ethanol elution, decompression recycling ethanol obtains belamcanda chinensis total isoflavone 252g (yield: 1.3%).After testing, isoflavone levels is 58% (in irigenine) in this extract, and wherein irigenine content is 14.6%.
The preparation of preparation example 6. general flavone from blackberry lily aglycons
Get dry Rhizoma Belamcandae with 80% ethanol extraction 3 times, solvent load is 10 times, and each time of extracting is 120 minutes, filters; Decompression filtrate recycling ethanol, behind thin up to the 10 times volume, add Snailase (be equivalent to medical material and weigh 0.1 times), in 37 ℃ of following hydrolysis 24 hours, hydrolyzed solution filters, the polyamide column of handling well on the precipitate (120L), 3 column volumes of first water eluting (360L), reuse 3 column volumes of 30% ethanol elution (360L), at last with 5 column volumes of ethanol elution (600L) of 95%, collect 95% ethanol elution, decompression recycling ethanol obtains belamcanda chinensis total isoflavone 207g (yield: 1.0%).After testing, isoflavone levels is 82% (in irigenine) in this extract, and wherein irigenine content is 26.3%.
The preparation of preparation example 7. iridins
Get the belamcanda chinensis total isoflavone 200g of preparation example 2 preparations, with 20 times of water gaging suspendibles, suspension is earlier with ethyl acetate extraction 3 times (each consumption is 3 times of suspendible), again with n-butanol extraction 3 times (each consumption is 3 times of suspendible).The combined ethyl acetate layer gets ethyl acetate extraction part 38g behind the recovery solvent; Merge n-butanol layer, get n-butanol extraction part 106g behind the recovery solvent.
Get partly 50g of n-butanol extraction, use an amount of dissolve with methanol, admix in about 150g silica gel, evaporate to dryness methanol in the silicagel column of the about 1500g silica gel of dress, is used chloroform, methanol gradient elution in packing into, collect the stream part that contains iridin respectively, reclaim solvent, the gained solid is the iridin crude product.Polyamide column on the crude product (about 1L), water-ethanol gradient elution is collected the stream part that contains iridin, concentrate the certain density ethyl alcohol recrystallization of concentrate reuse, the final iridin 3.1g that gets, detect [Huang Delin through HPLC, Liu Zhongyi, Wei Hao, the RP-HPLC method is measured the Rhizoma Belamcandae glycoside in Rhizoma Belamcandae and the Rhizoma Iridis Tectori, the content of Rhizoma Iridis Tectori glycoside, the West China pharmaceutical journal, 1997,12 (2): 115-116], content is respectively 91%., as follows through the physics and chemistry determination data, with pertinent literature [JP63030417; Phytochem, 1983,22 (9): 2061] the contrast basically identical, identify that it is an iridin.
The physical and chemical determination data of iridin:
Fusing point: 205-208 ℃ ESI-MS, m/z521 (M-1)
+UV
Max MeOHNm:256,320 IR (KBr, cm
-1): 3397,1658,1620,1587,1513
1H-NMR (DMSO-d
6, 400MHz): 12.89 (1H, s), 9.22 (1H, s), 8.48 (1H, s), 6.90 (1H, s), 6.73 (1H, d, J=1.88), 6.69 (1H, d, J=1.88), 5.38 (1H, d, J=5.04), 3.80 (3H, s), 3.78 (3H, s), 3.70 (3H, s)
13C-NMR (DMSO-d
6, 100MHz): 180.5,156.6,155.3,152.9,152.8,152.3,150.2,136.4,132.5,125.8,122.0,110.3,106.4,104.6,100.1,94.0,77.3,76.7,73.1,69.6,60.6,60.2,59.9,55.8
The preparation of preparation example 8. irigenines
Get test example 7 described ethyl acetate extraction part 30g, use an amount of dissolve with methanol, admix in about 90g silica gel evaporate to dryness methanol, adorn in the silicagel column of about 900g silica gel in packing into, use chloroform, the methanol gradient elution is collected the stream part that contains irigenine, reclaims solvent, gained solid reuse ethyl acetate, acetone recrystallization, get the about 1g of irigenine, detect [Malin, Song Wanzhi through HPLC, Wu Feng, the rp-hplc of Rhizoma Belamcandae effective ingredient, Acta Pharmaceutica Sinica, 1996,31 (12): 945-949], content 93%, as follows through the physics and chemistry determination data, with pertinent literature [JP63030417; Phytochem, 1983,22 (9): 2061] the contrast basically identical, identify that it is an irigenine.
The physical and chemical determination data of irigenine:
Fusing point: 179-181 ℃ EI-MS, m/z360 (M
+) UV
Max MeOHNm:269,337 IR (KBr, cm
-1): 3439,1661,1624,1580,1512
1H-NMR (DMSO-d
6, 400MHz): 12.88 (1H, s), 8.25 (1H, s), 6.67 (1H, d, J=1.89), 6.70 (1H, d, J=1.89), 6.47 (1H, s), 3.80 (3H, s), 3.79 (3H, s), 3.74 (3H, s)
13C-NMR (DMSO-d
6, 100MHz): 180.0,157.2,154.1,152.9,152.5,152.3,150.0,136.8,131.6,125.6,121.7,110.3,105.2,104.9,93.8,59.5,59.5,55.8
Preparation example 9. preparation general flavone from blackberry lily glycoside injection liquids (50mg/ props up)
Take by weighing 50g general flavone from blackberry lily glycosides, add 1600ml water for injection, stirring makes it to dissolve fully, regulate pH value, in go into 0.3% (w/v) pin charcoal, 60 ℃ of stirrings 30 minutes, filter, filtrate is added water for injection to 2000ml, with 0.45 μ m membrane filtration, fill, every 2ml, in 100 ℃ of flowing steam sterilizations 30 minutes, make 1000 altogether, every contains general flavone from blackberry lily glycosides 50mg.
Preparation example 10. preparation general flavone from blackberry lily aglycon injection (5mg/ props up)
Take by weighing 5g general flavone from blackberry lily aglycon, add 800ml propylene glycol and 800ml water for injection, stirring makes it to dissolve fully, regulate pH value, in go into 0.3% (w/v) pin charcoal, 60 ℃ of stirrings 30 minutes, filter, filtrate is added water for injection to 2000ml, with 0.45 μ m membrane filtration, fill, every 2ml, in 100 ℃ of flowing steam sterilizations 30 minutes, make 1000 altogether, every contains general flavone from blackberry lily aglycon 5mg.
Preparation example 11. preparation general flavone from blackberry lily injection (20mg/ props up)
Take by weighing the 20g general flavone from blackberry lily, add 800ml propylene glycol and 800ml water for injection, stirring makes it to dissolve fully, regulate pH value, in go into 0.3% (w/v) pin charcoal, 60 ℃ of stirrings 30 minutes, filter, filtrate is added water for injection to 2000ml, with 0.45 μ m membrane filtration, fill, every 2ml, in 100 ℃ of flowing steam sterilizations 30 minutes, make 1000 altogether, every contains general flavone from blackberry lily 20mg.
Preparation example 12. preparation iridin injection (5mg/ props up)
Take by weighing 5g iridin 16g sodium chloride for injection and hydroxypropyl, add 1600ml water for injection, stirring makes it to dissolve fully, regulate pH value, add 0.3% (w/v) pin charcoal, 60 ℃ were stirred 30 minutes, filter, filtrate is added water for injection to 2000ml, with 0.45 μ m membrane filtration, fill, every 2ml, in 100 ℃ of flowing steam sterilizations 30 minutes, make 1000 altogether, every contains iridin 5mg.
Preparation example 13. preparation irigenine injection (1mg/ props up)
Take by weighing 1g irigenine 16g sodium chloride for injection and hydroxypropyl, add 1600ml water for injection, stirring makes it to dissolve fully, regulate pH value, add 0.3% (w/v) pin charcoal, 60 ℃ were stirred 30 minutes, filter, filtrate is added water for injection to 2000ml, with 0.45 μ m membrane filtration, fill, every 2ml, in 100 ℃ of flowing steam sterilizations 30 minutes, make 1000 altogether, every contains irigenine 1mg.
Preparation example 14. preparation general flavone from blackberry lily glycosides sheets (50mg/ sheet)
Take by weighing 50g general flavone from blackberry lily glycosides, 140g starch, 50g pregelatinized Starch and 10g carboxymethyl starch sodium, fully mix homogeneously is crossed 80 mesh sieves, adds 95% ethanol and makes soft material in right amount, 12 orders are granulated, 60 ℃ of dryings 3 hours, 12 mesh sieve granulate add the magnesium stearate of granule gross weight 0.3%, the heavily about 250mg of tab, tabletting makes 1000 altogether, and every contains general flavone from blackberry lily glycosides 50mg.
Preparation example 15. preparation general flavone from blackberry lily aglycon soft capsules (50mg/ grain)
Take by weighing the 20g hydrogenated palm oil, join in the medicinal Oleum Glycines of 120g, the heating mixing makes soft capsule matrix, and 50g general flavone from blackberry lily aglycon is joined in the substrate, stirs, and colloid mill grinds, and makes soft capsule content.Press gelatin: glycerol: water (1: 0.3: 1) glue, adopt the encapsulating machine pelleting, make 1000 soft capsules, every contains general flavone from blackberry lily aglycon 50mg.
Preparation example 16. preparation general flavone from blackberry lily buccal tablets (500mg/ bag)
Take by weighing the 50g general flavone from blackberry lily, 24.5g dextrin, 25g starch, 0.5g protein sugar, cross behind 120 mesh sieves and fully mix, use the 80-90% alcohol granulation, 40 ℃ of dryings down, dried granule is with 12 eye mesh screen granulate, tabletting makes 100 altogether, and general flavone from blackberry lily content is the 500mg/ sheet.
Preparation example 17. preparation iridin sheets (50mg/ sheet)
Take by weighing the 50g iridin, 140g starch, 50g pregelatinized Starch and 10g carboxymethyl starch sodium, fully mix homogeneously is crossed 80 mesh sieves, adds 95% ethanol and makes soft material in right amount, 12 orders are granulated, 60 ℃ of dryings 3 hours, 12 mesh sieve granulate add the magnesium stearate of granule gross weight 0.3%, the heavily about 250mg of tab, tabletting makes 1000 altogether, and every contains iridin 50mg.
Preparation example 18. preparation iridin capsules (200mg/ grain)
Take by weighing the 20g iridin, use 95% alcohol granulation, cross 12 mesh sieves, be filled in No. 1 capsule, make 100 altogether, every contains iridin 200mg.
Preparation example 19. preparation iridin buccal tablets (500mg/ sheet)
Take by weighing the 50g iridin, 24.5g dextrin, 25g starch, 0.5g protein sugar, cross behind 120 mesh sieves and fully mix, use the 80-90% alcohol granulation, 40 ℃ of dryings down, dried granule is with 12 eye mesh screen granulate, tabletting makes 100 altogether, and iridin content is the 500mg/ sheet.
Preparation example 20. preparation iridin granules (1000mg/ bag)
Take by weighing the 50g iridin, the 50g dextrin, the 150g cane sugar powder fully mixes behind 120 mesh sieves excessively, makes suitable soft material with distilled water, granulate with 18 eye mesh screens, dry under 40 ℃, dried granule is packed as the 5g/ bag with 12 eye mesh screen granulate, make 50 bags altogether, iridin content is the 1000mg/ bag.
Preparation example 21. preparation irigenine soft capsules (50mg/ grain)
Take by weighing the 20g hydrogenated palm oil, join in the medicinal Oleum Glycines of 120g, the heating mixing makes soft capsule matrix, and the 50g irigenine is joined in the substrate, stirs, and colloid mill grinds, and makes soft capsule content.Press gelatin: glycerol: water (1: 0.3: 1) glue, adopt the encapsulating machine pelleting, make 1000 soft capsules, every contains irigenine 50mg.
Preparation example 22. preparation irigenine sheets (200mg/ sheet)
Take by weighing the 20g irigenine, 18g starch, 10g pregelatinized Starch and 2g carboxymethyl starch sodium, fully mix homogeneously is crossed 80 mesh sieves, adds 95% ethanol and makes soft material in right amount, 12 orders are granulated, 60 ℃ of dryings 3 hours, 12 mesh sieve granulate add the magnesium stearate of granule gross weight 0.3%, the heavily about 500mg of tab, tabletting makes 100 altogether, and every contains irigenine 200mg.
Preparation example 23. preparation irigenine buccal tablets (500mg/ bag)
Take by weighing the 50g irigenine, 24.5g dextrin, 25g starch, 0.5g protein sugar, cross behind 120 mesh sieves and fully mix, use the 80-90% alcohol granulation, 40 ℃ of dryings down, dried granule is with 12 eye mesh screen granulate, tabletting makes 100 altogether, and irigenine content is the 500mg/ sheet.
Preparation example 24. preparation irigenine granules (1000mg/ bag)
Take by weighing the 50g irigenine, the 50g dextrin, the 150g cane sugar powder fully mixes behind 120 mesh sieves excessively, makes suitable soft material with distilled water, granulate with 18 eye mesh screens, dry under 40 ℃, dried granule is packed as the 5g/ bag with 12 eye mesh screen granulate, make 50 bags altogether, irigenine content is the 1000mg/ bag.
Test example 1. oral iridins, irigenine Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raise therapeutical effect
Male mice in kunming is selected in this experiment for use, adopts acetic acid to cause the acute inflammation model that mouse peritoneal hair cell vascular permeability raises, and the anti-inflammatory activity of iridin, irigenine is studied.
80 of Kunming mouses, be divided into 8 groups at random, be respectively model group, positive drug control group (hydrocortisone 25mg/kg), iridin height (60mg/kg), in (20mg/kg), low (6mg/kg) dosage group, irigenine height (45mg/kg), in 10 every group of (15mg/kg), low (4.5mg/kg) dosage groups.Iridin, irigenine are made into respective concentration, gastric infusion with 0.5% sodium carboxymethyl cellulose suspendible.Hydrocortisone is made into respective concentration with the injection normal saline, and the tail intravenously administrable once before the modeling.Give relative medicine by body weight every day, administration volume 0.2ml/10g body weight.Successive administration 3 days, after the last administration 1 hour, press document [Zhu Shemin, etc.The main pharmacodynamics research of Shuanghuangli dripping pill.Contemporary Chinese is used pharmaceutical journal.2001,18:120] method, every mouse tail vein injection 0.5% azovan blue 0.1ml/10g body weight, and lumbar injection 0.6% acetic acid normal saline solution 0.2ml/ immediately, take off cervical vertebra behind the 20min and put to death, open the abdominal cavity, with 6ml normal saline washing abdominal cavity, collect cleaning mixture and centrifugal, get supernatant and absorb in the photometry of 590nm place.The results are shown in Table 1.Utilize student t test organize between relatively.The result shows, 6～60mg/kg iridin and 4.5～45mg/kg irigenine gastric infusion, and all Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raises and has certain inhibitory action, and certain dose-effect relationship is arranged.60mg/kg iridin or 45mg/kg irigenine effect are suitable.
The influence that table 1. iridin, irigenine Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raise (x ± s, n=10)
| Group | Dosage (mg/kg) | OD 590 |
| Model hydrocortisone iridin (height) iridin (in) iridin (low) irigenine (height) irigenine (in) irigenine (low) | —— 25 60 20 6 45 15 4.5 | 0.831±0.112 0.490±0.081 ** 0.408±0.106 ** 0.527±0.129 ** 0.626±0.204 * 0.404±0.128 ** 0.503±0.089 ** 0.623±0.228 * |
Compare with model group:
*, P＜0.05;
*, P＜0.01.
Test example 2. oral general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raise therapeutical effect
By the method for test example 1, the anti-inflammatory activity of Rhizoma Belamcandae total flavonoid glycoside, general flavone from blackberry lily aglycon, general flavone from blackberry lily is studied.The result shows (table 2), 12～120mg/kg general flavone from blackberry lily glycosides, 9～90mg/kg general flavone from blackberry lily aglycon and 10～100mg/kg general flavone from blackberry lily gastric infusion, all Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raises and has certain inhibitory action, and certain dose-effect relationship is arranged.
The influence that the oral general flavone from blackberry lily glycosides of table 2., general flavone from blackberry lily aglycon, general flavone from blackberry lily Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raise (x ± s, n=10)
| Group | Dosage (mg/kg) | OD 590 |
| Model hydrocortisone general flavone from blackberry lily glycosides (height) general flavone from blackberry lily glycosides (in) general flavone from blackberry lily glycosides (low) general flavone from blackberry lily aglycon (height) general flavone from blackberry lily aglycon (in) general flavone from blackberry lily aglycon (low) general flavone from blackberry lily (height) general flavone from blackberry lily (in) general flavone from blackberry lily (low) | —— 25 120 40 12 90 30 9 100 30 10 | 0.901±0.113 0.495±0.095 ** 0.429±0.023 ** 0.532±0.137 ** 0.601±0.089 * 0.444±0.101 ** 0.509±0.145 ** 0.679±0.093 * 0.435±0.113 ** 0.528±0.111 ** 0.646±0.135 * |
Compare with model group:
*, P＜0.05;
*, P＜0.01.
The therapeutical effect that test example 3. injection iridins, irigenine Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raise
Male mice in kunming is selected in this experiment for use, adopts acetic acid to cause the acute inflammation model that mouse peritoneal hair cell vascular permeability raises, and the anti-inflammatory activity of iridin, irigenine is studied.
Kunming mouse, the random packet of dosage shown in the according to the form below, 10 every group.Iridin, irigenine are made into respective concentration solution with the injection normal saline, and give relative medicine by the body weight tail vein injection every day, administration volume 0.2ml/10g body weight.Successive administration 3 days, after the last administration 1 hour, press document [Zhu Shemin, etc.The main pharmacodynamics research of Shuanghuangli dripping pill.Contemporary Chinese is used pharmaceutical journal.2001,18:120] method, every mouse tail vein injection 0.5% azovan blue 0.1ml/10g body weight, and lumbar injection 0.6% acetic acid normal saline solution 0.2ml/ immediately, take off cervical vertebra behind the 20min and put to death, open the abdominal cavity, with 6ml normal saline washing abdominal cavity, collect cleaning mixture and centrifugal, get supernatant and absorb in the photometry of 590nm place.The results are shown in Table 1.Utilize student t test organize between relatively.The result shows, 2.5～25mg/kg iridin and 2～20mg/kg irigenine intravenous administration, and all Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raises and has certain inhibitory action, and certain dose-effect relationship is arranged.25mg/kg iridin or 20mg/kg irigenine effect are suitable.
The influence that table 3. intravenous injection iridin, irigenine Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raise (x ± s, n=10)
| Group | Dosage (mg/kg) | OD 590 |
| Model hydrocortisone iridin (height) iridin (in) iridin (low) irigenine (height) irigenine (in) irigenine (low) | —— 25 25 10 2.5 20 8 2 | 0.977±0.408 0.468±0.188 ** 0.478±0.140 ** 0.527±0.099 ** 0.626±0.204 * 0.501±0.106 ** 0.543±0.106 ** 0.641±0.111 * |
Compare with model group:
*, P＜0.05;
*, P＜0.01.
The therapeutical effect that the wild general flavone from blackberry lily glycosides of test example 4. injections, general flavone from blackberry lily aglycon, general flavone from blackberry lily Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raise
By the method for test example 3, the anti-inflammatory activity of Rhizoma Belamcandae total flavonoid glycoside, general flavone from blackberry lily aglycon, general flavone from blackberry lily is studied.The result shows (table 4), 8～80mg/kg general flavone from blackberry lily glycosides, 4～40mg/kg general flavone from blackberry lily aglycon and 6～60mg/kg general flavone from blackberry lily drug administration by injection, all Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raises and has certain inhibitory action, and certain dose-effect relationship is arranged.
The influence that table 4. injection general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily Dichlorodiphenyl Acetate induced mice abdominal cavity capillary permeability raise (x ± s, n=10)
| Group | Dosage (mg/kg) | OD 590 |
| Model hydrocortisone general flavone from blackberry lily glycosides (height) general flavone from blackberry lily glycosides (in) general flavone from blackberry lily glycosides (low) general flavone from blackberry lily aglycon (height) general flavone from blackberry lily aglycon (in) general flavone from blackberry lily aglycon (low) general flavone from blackberry lily (height) general flavone from blackberry lily (in) general flavone from blackberry lily (low) | —— 25 80 27 8 40 13 4 60 20 6 | 0.894±0.078 0.508±0.110 ** 0.439±0.101 ** 0.511±0.089 ** 0.599±0.145 * 0.401±0.136 ** 0.517±0.108 ** 0.529±0.088 * 0.453±0.100 ** 0.542±0.094 ** 0.645±0.112 * |
Compare with model group:
*, P＜0.05;
*, P＜0.01.
The therapeutical effect of rat paw edema due to test example 5. oral iridins, the irigenine on Carrageenan
Male Wistar rat is selected in this experiment for use, adopt rat paw edema due to the carrageenin the subacute inflammation model, to studying with the anti-inflammatory activity of iridin, irigenine.
90 of Wistar rats, body weight 130～150g, be divided into 9 groups at random by body weight, be respectively model group, positive drug control group (hydrocortisone 15mg/kg), iridin height (30mg/kg), in (10mg/kg), low (3mg/kg) dosage group and irigenine height (22.5mg/kg), in (7.5mg/kg), low (2.2mg/kg) dosage group.Every group 10.Iridin, irigenine are made into respective concentration with 0.5% sodium carboxymethyl cellulose suspendible.Irritate stomach by body weight and give relative medicine, administration volume 0.4ml/100g body weight every day.Successive administration 3 days, press document [Xu Shuyun, etc.Analgesic, anti-inflammatory drug laboratory method.Pharmacological experimental methodology.2002,911] method carrageenin modeling.Measure right back sufficient sole of the foot position Zhou Jing with the moccasin chi before the medication of every rat last, after each group gives relative medicine then, only give rat right hind leg foot plantar subcutaneous injection 1% carrageenin suspension 0.1ml/ immediately, in injection back 3h, measure right back sufficient sole of the foot position Zhou Jing at same position with method, so that scorching metapedes sole of the foot Zhou Jing deducts to cause and scorching front foot sole of the foot week directly makes the swelling degree, calculates the difference of respectively organizing between swelling degree and comparable group.
The influence of rat paw edema due to the oral iridin of table 5., the irigenine on Carrageenan (x ± s, n=10)
| Dosage (mg/kg) | Swelling degree (mm) | |
| Model hydrocortisone iridin (height) iridin (in) iridin (low) irigenine (height) irigenine (in) irigenine (low) | —— 15 30 10 3 22.5 7.5 2.25 | 11.2±1.88 7.0±1.11 ** 6.7±0.91 ** 7.5±0.94 ** 9.0±1.15 * 7.0±0.95 ** 8.0±1.11 ** 9.1±1.34 * |
Compare with model group:
*, P＜0.05;
*, P＜0.01.
The therapeutical effect of rat paw edema due to test example 6. oral general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, the general flavone from blackberry lily on Carrageenan
By the method for test example 5, the anti-inflammatory activity of Rhizoma Belamcandae total flavonoid glycoside, general flavone from blackberry lily aglycon, general flavone from blackberry lily is studied.The result shows (table 6), 12～120mg/kg general flavone from blackberry lily glycosides, 9～90mg/kg general flavone from blackberry lily aglycon and 10～100mg/kg general flavone from blackberry lily gastric infusion, all rat paw edema has certain inhibitory action due to the on Carrageenan, and certain dose-effect relationship is arranged.
The influence of rat paw edema due to the oral general flavone from blackberry lily glycosides of table 6., general flavone from blackberry lily aglycon, the general flavone from blackberry lily on Carrageenan (x ± s, n=10)
| Dosage (mg/kg) | Swelling degree (mm) | |
| Model hydrocortisone general flavone from blackberry lily glycosides (height) general flavone from blackberry lily glycosides (in) general flavone from blackberry lily glycosides (low) general flavone from blackberry lily aglycon (height) general flavone from blackberry lily aglycon (in) general flavone from blackberry lily aglycon (low) general flavone from blackberry lily (height) general flavone from blackberry lily (in) general flavone from blackberry lily (low) | —— 15 120 40 12 90 30 9 100 30 10 | 12.3±1.44 6.9±1.03 ** 7.0±0.82 ** 8.1±1.03 ** 9.4±0.09 * 6.2±1.14 ** 7.6±1.07 ** 8.7±1.12 * 6.5±0.89 ** 7.8±1.11 ** 9.2±0.93 * |
Compare with model group:
*, P＜0.05;
*, P＜0.01.
The therapeutical effect of rat paw edema due to test example 7. injection iridins, the irigenine on Carrageenan
Male Wistar rat is selected in this experiment for use, adopt rat paw edema due to the carrageenin the subacute inflammation model, the anti-inflammatory activity of iridin, irigenine is studied.
80 of Wistar rats, body weight 130～150g, be divided into 8 groups at random by body weight, be respectively model group, positive drug control group (hydrocortisone 15mg/kg), iridin height (12.5mg/kg), in (3.6mg/kg), low (1.2mg/kg) dosage group and irigenine height (10mg/kg), in (3mg/kg), low (1mg/kg) dosage group.Every group 10.Iridin, irigenine are made into respective concentration with 0.5% sodium carboxymethyl cellulose suspendible.Give relative medicine by body weight tail vein every day, administration volume 0.4ml/100g body weight.Successive administration 3 days, press document [Xu Shuyun, etc.Analgesic, anti-inflammatory drug laboratory method.Pharmacological experimental methodology.2002,911] method carrageenin modeling.Measure right back sufficient sole of the foot position Zhou Jing with the moccasin chi before the medication of every rat last, after each group gives relative medicine then, irritate stomach feedwater 25ml/kg, only give rat right hind leg foot plantar subcutaneous injection 1% carrageenin suspension 0.1ml/ immediately, in injection back 1,2,3,4,6h, measure right back sufficient sole of the foot position Zhou Jing at same position with method,, calculate the difference between each time point swelling degree and comparable group sufficient sole of the foot week directly to make the swelling degree.
The influence of rat paw edema due to table 7. injection iridin, the irigenine on Carrageenan (x ± s, n=10)
| Group | Dosage (mg/kg) | Swelling degree (mm) |
| Model hydrocortisone iridin (height) iridin (in) iridin (low) irigenine (height) irigenine (in) irigenine (low) | —— 100 12.5 3.6 1.2 10 3 1 | 11.2±1.92 6.9±1.17 ** 6.6±0.80 ** 8.1±0.85 ** 8.7±1.02 * 6.6±0.80 ** 8.1±1.04 ** 8.7±1.34 * |
Compare with model group:
*, P＜0.05;
*, P＜0.01.
The therapeutical effect of rat paw edema due to test example 8. injection general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, the general flavone from blackberry lily on Carrageenan
By the method for test example 7, the anti-inflammatory activity of Rhizoma Belamcandae total flavonoid glycoside, general flavone from blackberry lily aglycon, general flavone from blackberry lily is studied.The result shows (table 8), 8～80mg/kg general flavone from blackberry lily glycosides, 4～40mg/kg general flavone from blackberry lily aglycon and 6～60mg/kg general flavone from blackberry lily drug administration by injection, all rat paw edema has certain inhibitory action due to the on Carrageenan, and certain dose-effect relationship is arranged.
The influence of rat paw edema due to table 8. injection general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, the general flavone from blackberry lily on Carrageenan (x ± s, n=10)
| Dosage (mg/kg) | Swelling degree (mm) | |
| Model hydrocortisone general flavone from blackberry lily glycosides (height) general flavone from blackberry lily glycosides (in) general flavone from blackberry lily glycosides (low) general flavone from blackberry lily aglycon (height) general flavone from blackberry lily aglycon (in) general flavone from blackberry lily aglycon (low) general flavone from blackberry lily (height) general flavone from blackberry lily (in) general flavone from blackberry lily (low) | —— 15 80 27 8 40 13 4 60 20 6 | 12.5±1.08 6.5±1.18 ** 7.1±0.78 ** 8.3±1.22 ** 9.0±1.01 * 6.1±0.99 ** 6.9±1.38 ** 8.4±0.98 * 6.9±1.15 ** 7.6±1.26 ** 8.8±1.26 * |
Compare with model group:
*, P＜0.05;
*, P＜0.01.
Test example 9. oral iridins, irigenine cause the protective effect of dead mouse to the lumbar injection staphylococcus aureus
Male mice in kunming is by the body weight random packet, and 11 every group, the filling stomach gives iridin, irigenine, and dosage is as shown in table 5.Be administered once every day, successive administration 7d, and the last time behind the administration 30min, the THIOGLYCOLLIC ACID salt culture fluid of lumbar injection staphylococcus aureus (37 ℃ ± 1 ℃, 24h, bacterial population about 10
8/ ml), 0.5ml/ only observes at once, and observes 7d continuously, record dead mouse situation every day, and survival mice Bliss ' s method calculates median effective dose (ED50).The results are shown in Table 9.The result shows that the dead mouse that iridin, irigenine all cause the lumbar injection staphylococcus aureus has the certain protection effect, and ED50 is respectively 53.6mg/kg and 40.8mg/kg.Both ED50 difference does not have significance meaning (P＞0.05).
The oral iridin of table 9., irigenine to the lumbar injection staphylococcus aureus cause dead mouse influence (x ± s, n=10)
| Group | Dosage (mg/kg) | The survival number | Survival rate | ED 50(mg/kg) |
| Model | —— | 0 | 0 | |
| Iridin | 100 60 36 22 13 | 10 6 2 1 0 | 90.91 54.55 18.18 9.09 0 | 53.6±9.4 |
| Irigenine | 60 36 22 13 | 9 4 1 0 | 81.82 36.36 9.09 0 | 40.8±6.2 |
Test example 10. oral general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily cause the protective effect of dead mouse to the lumbar injection staphylococcus aureus
By the method for test example 9, the anti-inflammatory activity of Rhizoma Belamcandae total flavonoid glycoside, general flavone from blackberry lily aglycon, general flavone from blackberry lily is studied.The result shows (table 10), and the dead mouse that general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily all cause the lumbar injection staphylococcus aureus has the certain protection effect, and ED50 is respectively 50.52mg/kg, 32.10mg/kg and 43.10mg/kg.
The oral general flavone from blackberry lily glycosides of table 10., general flavone from blackberry lily aglycon, general flavone from blackberry lily to the lumbar injection staphylococcus aureus cause dead mouse influence (x ± s, n=10)
| Group | Dosage (mg/kg) | The survival number | Survival rate | ED 50(mg/kg) |
| Model | —— | 0 | 0 | |
| The general flavone from blackberry lily glycosides | 200 100 50 25 12.5 6.25 | 11 9 6 2 1 0 | 91.67 75.00 50.00 13.67 8.33 0 | 50.52±8.7 |
| The general flavone from blackberry lily aglycon | 150 75 37.5 18.75 9.38 4.69 | 12 10 7 2 1 0 | 100.00 83.33 58.33 13.67 8.33 0 | 32.10±9.1 |
| Rhizoma Belamcandae extract | 180 90 45 22.5 11.25 5.63 | 10 10 6 3 1 0 | 83.33 83.33 50.00 25.00 8.33 0 | 43.10±6.5 |
Test example 11. injection iridins, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily cause the protective effect of dead mouse to the lumbar injection staphylococcus aureus
By the method for test example 9,10, injection iridin, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily are caused that to the lumbar injection staphylococcus aureus protective effect of dead mouse studies.The result shows; the dead mouse that iridin, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily all cause the lumbar injection staphylococcus aureus has the certain protection effect, and ED50 is respectively 32.15mg/kg, 22.03mg/kg, 33.09mg/kg, 20.35mg/kg, 28.97mg/kg.
Test example 12. iridins, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, the test of general flavone from blackberry lily in-vitro antibacterial
Staphylococcus aureus, beta hemolytic streptococcus, Diplococcus pneumoniae, stream bar bacillus, Type B streptococcus, escherichia coli, bacillus pyocyaneus provide by the Beijing Biological Product Inst., Ministry of Public Health.
Iridin, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily are mixed with 100,50,25,12.5,6.25,3.12 and the pastille culture fluid of 1.6mg/L with meat extract soup respectively, totally 7 drug level, every pipe total amount 1ml, flowing steam sterilization.Streptococcic test is added 1% glucose in the sterilization medicinal liquid, blank is not for containing the culture medium of medicine.Add 10 respectively
-3Test organisms liquid (8 hours cultures) 0.1ml cultivates observed result after 18 hours for 37 ℃.Judge minimal inhibitory concentration (MIC).The result shows (table 11) iridin, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily, and equal growth has the obvious suppression effect to various bacteria, and minimum inhibitory concentration is between 1.6～25mg/L.
Table 11. iridin, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, the external bacteriostasis of general flavone from blackberry lily
| Medicine | MIC(mg/L) | ||||||
| Staphylococcus aureus | Beta hemolytic streptococcus | Diplococcus pneumoniae | Hemophilus influenza | The Type B streptococcus | Escherichia coli | Bacillus pyocyaneus | |
| Iridin irigenine general flavone from blackberry lily glycosides general flavone from blackberry lily aglycon general flavone from blackberry lily | 3.12 1.6 3.12 1.6 3.12 | 6.25 3.12 12.5 3.12 6.25 | 12.5 12.5 12.5 12.5 12.5 | 12.5 12.5 25 12.5 12.5 | 25 25 25 25 25 | 12.5 12.5 25 12.5 25 | 6.25 6.25 6.25 6.25 6.25 |
Test example 13. iridins, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, the effect of general flavone from blackberry lily extracorporeal antivirus effect
Influenza virus (A3), Parainfluenza type 1 virus (HVJ), respiratory syncytial virus (RSV), adenovirus 3,7 type (AdV
3,7), Coxsackie virus B 4 types (CoxB4), echovirus type (ECHO
11), herpes simplex virus I, II type (HSV I, II).All available from Inst. of Viruses, China Preventive Medicine Science Academy.
Human hepatoma cell strain HepG-2 is available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
Get 24 well culture plates that grow up to cell monolayer, outwell culture fluid, inoculate 100 TCID
50The different virus liquid 50 μ l of (making the half cell culture tube viral dilution degree logarithm of pathological changes occur) put 37 ℃ of 5% CO in cell hole
2Adsorb 1h in the incubator, outwell viral liquid, after keeping liquid and wash cell face 3 times with the Eagl ' s that does not contain calf serum, add 50～3.12mg/L, continue to cultivate by the pastille culture medium of 0.5 times of doubling dilution, each concentration is established three parallel holes.Establish virus, medicinal liquid contrast and normal cell matched group simultaneously relatively.Put 37 ℃ of 5%CO
2Cultivated in the incubator four days, every day under inverted microscope microscopy once, observation of cell pathological changes, continuous three days.The judgement of cytopathy degree: "-": the cell growth is normal, and no pathological changes occurs; " 1 ": cytopathy account for whole cell monolayer＜25%; " 2 ": cytopathy accounts for 25%～50% of whole cell monolayer; " 3 ": cytopathy accounts for 50%～75% of whole cell monolayer; " 4 ": cytopathy accounts for 75%～100% of whole cell monolayer.
Judge according to above cytopathy Pyatyi standard, utilize Reed Mucnch method to calculate 50% valid density (EC
50).The results are shown in Table 12.
The result shows that iridin, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily have protective effect to the cell injury that multiple virus causes, and its 50% valid density is between 4.3～35.2mg/L.And under this concentration, the medicine pair cell does not produce obviously damage substantially.
The extracorporeal antivirus effect effect of table 12. iridin, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily
| Virus | EC 50(mg/L) | ||||
| Iridin | Irigenine | The general flavone from blackberry lily glycosides | The general flavone from blackberry lily aglycon | General flavone from blackberry lily | |
| A3 HVJ RSV AdV 3 AdV 7 CoxB4 ECHO 11 HSV-I HSV-II | 5.8 9.6 7.1 12.5 22.4 26.9 29.7 30.8 35.2 | 4.3 7.4 6.6 10.3 20.8 24.2 21.2 34.6 32.1 | 6.3 9.8 7.0 11.3 23.6 26.5 29.3 31.3 33.9 | 4.1 7.2 5.9 9.2 15.6 23.8 22.0 29.8 30.6 | 5.3 8.2 7.1 11.3 20.6 25.9 25.1 30.0 32.3 |
Test example 14. oral iridins, irigenine are to the therapeutical effect of mice influenzal pneumonia
Kunming mouse is irritated iridin, irigenine that stomach gives various dose by the body weight random packet, and viral infection matched group and intact animal's matched group are all to the volumetrical distilled water of identical medicinal liquid.Except that the normal control group, mice is slightly anaesthetized with ether, with 15 LD
50Influenza virus drop nose infects, every 0.05ml.Begin administration or water the previous day from infecting, every day 1 time, 6d infects and fixes after the back took by weighing the mice body weight on the 6th day continuously, and blood-letting, dissection are won full lung and weighed, and calculate the lung exponential quantity one by one, and obtain lung index suppression ratio.Heavy (the g)/body weight (g) * 100 of lung index=lung; The lung exponential quantity is big, and expression pneumonopathy range degree is serious.The results are shown in Table 8.Utilize student t test organize between relatively.
The result shows, infects back mouse lung exponential quantity and obviously increases, and the pneumonia that iridin and aglycon cause the influenza virus infecting mouse has the obvious suppression effect, and the lung exponential quantity obviously reduces.Show that oral wild flag tail glycosides, irigenine become pneumonopathy due to the influenza virus infecting mouse therapeutical effect is arranged.
Table 13. iridin, irigenine to the influence of influenza virus infecting mouse pneumonia (lung index) (x ± s, n=10)
| Group | Dosage | The lung index |
| Normal model iridin (height) iridin (in) iridin (low) irigenine (height) irigenine (in) irigenine (low) | —— —— 60 20 6 45 15 4.5 | 0.91±0.05 1.78±0.23 ## 1.08±0.14 ** 1.35±0.16 ** 1.57±0.15 * 1.09±0.20 ** 1.36±0.16 ** 1.53±0.17 * |
Compare with normal group:
##, P＜0.01.Compare with model group:
*, P＜0.05;
*, P＜0.01.
Test example 15. oral general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily are to the therapeutical effect of mice influenzal pneumonia
By the method for test example 13, the pneumonia therapeutical effect of Rhizoma Belamcandae total flavonoid glycoside, general flavone from blackberry lily aglycon, general flavone from blackberry lily is studied.The result shows (table 14), the pneumonia that general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily cause the influenza virus infecting mouse has the obvious suppression effect, the lung exponential quantity obviously reduces, and shows that oral general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily become pneumonopathy due to the influenza virus infecting mouse therapeutical effect is arranged.
Table 14. general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily to the influence of influenza virus infecting mouse pneumonia (lung index) (x ± s, n=10)
| Group | Dosage | The lung index |
| Normal model general flavone from blackberry lily glycosides (height) general flavone from blackberry lily glycosides (in) general flavone from blackberry lily glycosides (low) general flavone from blackberry lily aglycon (height) general flavone from blackberry lily aglycon (in) general flavone from blackberry lily aglycon (low) general flavone from blackberry lily (height) general flavone from blackberry lily (in) general flavone from blackberry lily (low) | —— —— 120 40 12 90 30 9 100 30 10 | 0.88±0.04 1.82±0.22 ## 1.09±0.14 ** 1.25±0.21 ** 1.40±0.03 ** 0.98±0.23 ** 1.19±0.15 ** 1.46±0.08 ** 1.18±0.15 ** 1.38±0.25 ** 1.60±0.11 * |
Compare with normal group:
##, P＜0.01.Compare with model group:
*, P＜0.05;
*, P＜0.01.
Test example 16. injection iridins, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily are to the therapeutical effect of little influenzal pneumonia
With reference to test example 13,14 methods, use the injection system administration, the pneumonia therapeutical effect of injection wild flag tail glycosides, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily is studied.。
The result shows (table 15), and injection wild flag tail glycosides, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily become pneumonopathy due to the influenza virus infecting mouse and have therapeutical effect equally.
Table 15. injection iridin, irigenine, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily to the influence of influenza virus infecting mouse pneumonia (lung index) (x ± s, n=10)
| Group | Dosage | The lung index |
| The normal model iridin, (height) iridin, (in) iridin, (low) irigenine, (height) irigenine, (in) irigenine, (low) general flavone from blackberry lily glycosides, (height) general flavone from blackberry lily glycosides, (in) the general flavone from blackberry lily glycosides, (low) general flavone from blackberry lily aglycon, (height) general flavone from blackberry lily aglycon, (in) the general flavone from blackberry lily aglycon, (low) general flavone from blackberry lily, (height) general flavone from blackberry lily, (in) general flavone from blackberry lily, (low) | —— —— 25 10 2.5 20 8 2 80 27 8 40 13 4 60 20 6 | 0.93±1.01 1.90±0.56 ## 1.10±0.29 ** 1.29±0.61 ** 1.57±0.45 * 1.06±0.38 ** 1.25±0.87 ** 1.50±1.07 * 1.19±1.30 ** 1.27±0.54 ** 1.51±1.11 ** 1.03±0.64 ** 1.30±0.62 ** 1.42±0.98 ** 1.15±1.04 ** 1.41±0.22 ** 1.64±0.31 * |
Compare with normal group:
##, P＜0.01.Compare with model group:
*, P＜0.05;
*, P＜0.01.
Test example 17. oral iridins, wild flag aglycon, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily are to the influence of airway of mice phenol red Excretion
Adopt the mice phenol red to drain method, utilize phenol red mouse peritoneal injection rear section, measure the excretion of airway of mice phenol red, to judge influence to airway of mice secretion liquid measure from the excretory characteristics of air flue.
90 of Kunming mouses, be divided into 9 groups at random: the blank group, positive drug control group (JIZHI TANGJIANG 0.15ml/10g), iridin height (40mg/kg), in (15mg/kg), low (4mg/kg) dosage group and wild flag aglycon height (30mg/kg), in (10mg/kg), low (3mg/kg) dosage group and ammonium chloride group (1000mg/kg).The blank group is irritated stomach and is given 0.5% sodium carboxymethyl cellulose liquid, and iridin, wild flag aglycon are made into respective concentration, gastric infusion with 0.5% sodium carboxymethyl cellulose suspendible.JIZHI TANGJIANG directly gives pharmaceutical liquid, and ammonium chloride is made into corresponding concentration with 0.5% sodium carboxymethyl cellulose.Give relative medicine by body weight every day, administration volume 0.2ml/10g body weight.All the other respectively organize equal gastric infusion 2 days except that the ammonium chloride group, and the 3rd day together with the administration of ammonium chloride group after 1 hour, press document [Xie Qiangmin, etc.P-Cymene phlegm-dispelling functions and the side's of analysing research.Contemporary Chinese is used pharmacy.2002,03:192] method, mouse peritoneal is injected 2.5% phenol red normal saline solution 0.2ml/10g mice, mice is put to death in dislocation after 30 minutes, separates trachea, cuts off along the little edge of thyroid cartilage again and cuts off to proximal part prolongation 0.5cm, put into the 1ml normal saline solution, vibrated 10 minutes, and added 1mol/L sodium hydroxide 0.1ml, measure content with BIO-RAD Model550 at 570nm behind the mixing.Make standard curve with phenol red, calculate phenol red content, compare the phenol red amount of each administration medicine group and NS group with the T check.
The result shows, oral iridin, wild flag aglycon, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily all can make airway of mice phenol red excretion increase, and have stronger phlegm-dispelling functions, and have certain dose-effect relationship.
The oral iridin of table 16., wild flag aglycon to the influence of airway of mice phenol red Excretion (x ± s, n=10)
| Group | Dosage (mg/kg) | Trachea phenol red excretion amount (μ g/ml) |
| Anxious syrup group ammonium chloride group wild flag glycosides (height) the wild flag glycosides of blank control group (in) wild flag glycosides (low) Tectorigenin (height) Tectorigenin (in) Tectorigenin (low) general flavone from blackberry lily glycosides (height) general flavone from blackberry lily glycosides (in) (height) general flavone from blackberry lily glycosides unit of general flavone from blackberry lily glycosides (low) general flavone from blackberry lily glycosides unit (in) general flavone from blackberry lily glycosides unit (low) general flavone from blackberry lily (height) general flavone from blackberry lily (in) general flavone from blackberry lily (low) | —— 15ml/kg 1000 40 15 4 30 10 3 120 40 12 90 30 9 100 30 10 | 1.60±0.022 2.46±0.012 * 2.87±0.041 ** 3.16±0.015 ** 2.96±0.022 * 2.17±0.021 * 3.28±0.018 ** 3.01±0.037 * 2.24±0.019 * 3.01±0.032 ** 2.87±0.013 * 2.19±0.028 * 3.35±0.024 ** 3.00±0.014 ** 2.22±0.017 * 3.14±0.020 ** 2.90±0.033 * 2.24±0.015 * |
*P＜0.05,
*Compare with the blank group P＜0.01.
Test example 18. injection iridins, wild flag aglycon, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily are to the influence of airway of mice phenol red Excretion
Adopt the mice phenol red to drain method, utilize phenol red mouse peritoneal injection rear section, measure the excretion of airway of mice phenol red, to judge influence to airway of mice secretion liquid measure from the excretory characteristics of air flue.
90 of Kunming mouses, be divided into 9 groups at random: the blank group, positive drug control group (JIZHI TANGJIANG 0.15ml/10g), iridin height (25mg/kg), in (10mg/kg), low (2.5mg/kg) dosage group and wild flag aglycon height (20mg/kg), in (8mg/kg), low (2mg/kg) dosage group and ammonium chloride group (1000mg/kg).Blank group tail vein injection gives normal saline, iridin, wild flag aglycon are made into respective concentration solution with the injection normal saline, give relative medicine by the body weight tail vein injection every day, JIZHI TANGJIANG is directly irritated stomach and is given pharmaceutical liquid, ammonium chloride is made into corresponding concentration with deionized water, administration volume 0.2ml/10g body weight.All the other respectively organize equal administration 2 days except that the ammonium chloride group, and the 3rd day together with the administration of ammonium chloride group after 1 hour, press document [Xie Qiangmin, etc.P-Cymene phlegm-dispelling functions and the side's of analysing research.Contemporary Chinese is used pharmacy.2002,03:192] method, mouse peritoneal is injected 2.5% phenol red normal saline solution 0.2ml/10g mice, mice is put to death in dislocation after 30 minutes, separates trachea, cuts off along the little edge of thyroid cartilage again and cuts off to proximal part prolongation 0.5cm, put into the 1ml normal saline solution, vibrated 10 minutes, and added 1mol/L sodium hydroxide 0.1ml, measure content with BIO-RAD Model 550 at 570nm behind the mixing.With the phenol red standard curve of doing, calculate phenol red content, compare the phenol red amount of each administration medicine group and NS group with the T check.
The result shows, injection iridin, wild flag aglycon, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily all can make airway of mice phenol red excretion increase, and have stronger phlegm-dispelling functions, and have certain dose-effect relationship.
Table 17. injection iridin, wild flag aglycon to the influence of airway of mice phenol red Excretion (x ± s, n=10)
| Group | Dosage (mg/kg) | Trachea phenol red excretion amount (μ g/ml) |
| Anxious syrup group ammonium chloride group wild flag glycosides (height) the wild flag glycosides of blank control group (in) wild flag glycosides (low) Tectorigenin (height) Tectorigenin (in) Tectorigenin (low) general flavone from blackberry lily glycosides (height) general flavone from blackberry lily glycosides (in) (height) general flavone from blackberry lily glycosides unit of general flavone from blackberry lily glycosides (low) general flavone from blackberry lily glycosides unit (in) general flavone from blackberry lily glycosides unit (low) general flavone from blackberry lily (height) general flavone from blackberry lily (in) general flavone from blackberry lily (low) | —— 15ml/kg 1000 25 10 2.5 20 8 2 80 27 8 40 13 4 60 20 6 | 1.72±0.012 2.52±0.019 * 2.93±0.021 ** 3.09±0.035 ** 2.98±0.028 * 2.20±0.027 * 3.17±0.028 ** 3.05±0.017 * 2.44±0.016 * 3.05±0.018 ** 2.96±0.030 * 2.24±0.027 * 3.29±0.013 ** 2.91±0.025 ** 2.34±0.019 * 3.10±0.021 ** 2.97±0.026 * 2.21±0.021 * |
*P＜0.05,
*Compare with the blank group P＜0.01.
Test example 19. oral iridins, wild flag aglycon, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily cause the influence of coughing mice to strong aqua ammonia
Ammonia pungent aerosols such as (25%-28%) sucks in the respiratory tract, stimulates the sensor under the airway epithelial, can cause cough.The variation of mouse cough number of times in cough latent period and the 2min is observed strong aqua ammonia is caused the influence of coughing mice before and after the administration of this measuring mice.
80 of Kunming mouses, be divided into 8 groups at random: the blank group, positive drug control group (codeine phosphate 5mg/kg), iridin height (40mg/kg), in (15mg/kg), low (4mg/kg) dosage group and wild flag aglycon height (30mg/kg), in (10mg/kg), low (3mg/kg) dosage group.The blank group is irritated stomach and is given 0.5% sodium carboxymethyl cellulose liquid, and iridin, wild flag aglycon and codeine phosphate are made into respective concentration, gastric infusion with 0.5% sodium carboxymethyl cellulose suspendible.Give relative medicine by body weight every day, administration volume 0.2ml/10g body weight.Each organizes continuous gastric infusion 2 days, respectively organizes administration after 60 minutes on the 3rd day, by [chatting uncle's cloud etc.Pharmacological experimental methodology.The People's Health Publisher.2001:1363] method, mice is put into 500ml glass bell jar (each 1), connect the PARIMASTER ultrasound atomizer, constant voltage sprays into ammonia (25%-28%) in the glass bell jar uniformly, spraying 5S observes and writes down cough latent period (s) (beginning to the required time of cough occurring from spraying ammonia) and the interior cough of the 2min number of times of mice then.Respectively be subjected to the difference of reagent group and blank group with the T check.
The result shows, oral iridin, wild flag aglycon, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily all can prolong to cause and cough incubation period, reduces cough number of times in the 2min (comparing P＜0.05 with the NS group); 40mg/kg iridin and 30mg/kg wild flag aglycon obviously prolong to cause coughs incubation period, reduce cough number of times in the 2min (with the NS group relatively, P＜0.01), have stronger antitussive effect.
The oral iridin of table 18., wild flag aglycon to strong aqua ammonia cause the influence of coughing mice (x ± s, n=10)
| Group | Dosage (mg/kg) | Cause and cough incubation period (s) | Cause and cough number of times | ||
| Before the administration | After the administration | Before the administration | After the administration | ||
| Blank group codeine phosphate group iridin, (height) iridin, (in) iridin, (low) Tectorigenin, (height) Tectorigenin, (in) Tectorigenin, (low) general flavone from blackberry lily glycosides, (height) general flavone from blackberry lily glycosides, (in) the general flavone from blackberry lily glycosides, (low) general flavone from blackberry lily aglycon, (height) general flavone from blackberry lily aglycon, (in) the general flavone from blackberry lily aglycon, (low) general flavone from blackberry lily, (height) general flavone from blackberry lily, (in) general flavone from blackberry lily, (low) | —— 5 40 20 10 30 15 7.5 120 40 12 90 30 9 100 30 10 | 24.5±2.4 24.0±1.7 23.5±2.0 24.8±3.4 24.6±1.8 23.9±2.1 24.0±2.2 23.7±1.7 24.3±1.5 24.3±2.5 24.1±1.6 23.3±2.2 24.2±1.9 24.2±1.8 23.8±2.1 24.1±2.2 24.0±1.6 | 25.1±2.8 32.4±2.3 ** 38.2±3.0 ** 35.7±1.8 * 28.6±2.7 * 40.5±3.8 ** 36.8±2.7 * 29.2±1.5 * 35.1±3.2 ** 32.3±2.2 * 28.1±2.5 * 40.5±3.0 ** 35.3±2.1 * 28.0±1.8 * 38.9±2.6 ** 34.3±1.7 * 28.9±2.1 * | 21.7±3.1 21.0±3.6 21.9±2.1 22.5±3.8 20.4±1.7 21.1±2.9 20.3±3.0 21.1±2.4 22.3±2.0 21.6±3.1 21.1±1.9 22.6±2.5 20.3±3.3 20.0±2.2 22.1±3.0 22.0±2.8 21.2±1.4 | 20.3±2.4 13.1±1.9 ** 10.2±1.4 * 12.8±2.5 * 18.9±3.0 * 11.7±2.8 ** 11.3±3.4 * 17.9±2.7 * 11.5±1.5 * 13.2±2.0 * 18.0±2.3 * 10.7±2.1 ** 11.4±2.3 * 16.4±2.8 * 10.5±1.9 * 12.4±2.8 * 19.7±2.8 * |
*P＜0.05,
*Compare with the blank group P＜0.01.
Test example 20. injection iridins, wild flag aglycon, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily cause the influence of coughing mice to strong aqua ammonia
Ammonia pungent aerosols such as (25%-28%) sucks in the respiratory tract, stimulates the sensor under the airway epithelial, can cause cough.The variation of mouse cough number of times in cough latent period and the 2min is observed strong aqua ammonia is caused the influence of coughing mice before and after the administration of this measuring mice.
80 of Kunming mouses, be divided into 8 groups at random: the blank group, positive drug control group (codeine phosphate 5mg/kg), iridin height (25mg/kg), in (10mg/kg), low (2.5mg/kg) dosage group and wild flag aglycon height (20mg/kg), in (8mg/kg), low (2mg/kg) dosage group.。Blank group tail vein injection gives normal saline, iridin, wild flag aglycon are made into respective concentration solution with the injection normal saline, give relative medicine by the body weight tail vein injection every day, and codeine phosphate is made into respective concentration with deionized water, gastric infusion.Administration volume 0.2ml/10g body weight.Each organizes continuous gastric infusion 2 days, respectively organizes administration after 60 minutes on the 3rd day, by [chatting uncle's cloud etc.Pharmacological experimental methodology.The People's Health Publisher.2001:1363] method, mice is put into 500ml glass bell jar (each 1), connect the PARIMASTER ultrasound atomizer, constant voltage sprays into ammonia (25%-28%) in the glass bell jar uniformly, spraying 5S observes and writes down cough latent period (s) (beginning to the required time of cough occurring from spraying ammonia) and the interior cough of the 2min number of times of mice then.Respectively be subjected to the difference of reagent group and blank group with the T check.
The result shows that injection iridin, wild flag aglycon, general flavone from blackberry lily glycosides, general flavone from blackberry lily aglycon, general flavone from blackberry lily all can prolong to cause and cough incubation period, reduces cough number of times in the 2min (organizing relatively P＜0.05 with NS); 25mg/kg iridin and 20mg/kg wild flag aglycon obviously prolong to cause coughs incubation period, reduce cough number of times in the 2min (with the NS group relatively, P＜0.01), have stronger antitussive effect.
Table 19. injection iridin, wild flag aglycon to strong aqua ammonia cause the influence of coughing mice (x ± s, n=10)
| Group | Dosage (mg/kg) | Cause and cough incubation period (s) | Cause and cough number of times | ||
| Before the administration | After the administration | Before the administration | After the administration | ||
| Blank group codeine phosphate group iridin, (height) iridin, (in) iridin, (low) Tectorigenin, (height) Tectorigenin, (in) Tectorigenin, (low) general flavone from blackberry lily glycosides, (height) general flavone from blackberry lily glycosides, (in) the general flavone from blackberry lily glycosides, (low) general flavone from blackberry lily aglycon, (height) general flavone from blackberry lily aglycon, (in) the general flavone from blackberry lily aglycon, (low) general flavone from blackberry lily, (height) general flavone from blackberry lily, (in) general flavone from blackberry lily, (low) | —— 5 25 10 2.5 20 8 2 80 27 8 40 13 4 60 20 6 | 24.5±2.1 24.7±1.7 23.2±2.2 24.1±1.4 24.9±2.8 23.3±2.7 24.8±1.2 23.1±1.9 23.8±2.2 24.7±2.0 23.6±2.1 25.0±1.5 23.8±2.7 23.1±2.5 24.5±2.1 23.0±1.2 23.2±2.0 | 24.1±1.1 33.4±1.3 ** 38.7±2.2 ** 36.8±2.8 * 27.9±1.7 * 39.5±1.7 ** 35.8±2.5 * 28.4±1.7 * 37.8±2.3 ** 36.9±2.0 * 27.4±1.5 * 39.4±1.2 ** 34.1±0.9 ** 28.6±1.9 * 37.8±2.1 * 35.7±1.3 * 24.1±1.5 | 21.9±1.1 22.7±2.6 22.6±2.8 21.4±2.7 20.9±2.1 21.1±1.6 21.8±2.1 22.0±1.9 22.1±1.3 22.5±2.2 20.8±3.0 22.1±2.5 21.4±1.8 20.3±1.8 21.5±2.2 23.1±1.4 20.9±1.5 | 20.3±2.4 12.8±2.9 ** 11.7±2.8 * 12.0±1.6 * 17.9±2.9 * 10.9±1.7 ** 12.3±2.7 * 18.4±2.6 * 12.3±1.2 * 13.6±2.8 * 18.1±1.9 * 11.0±1.8 ** 12.5±2.7 * 16.9±2.5 * 10.3±1.4 * 11.5±2.6 * 20.3±1.9 * |
*P＜0.05,
*Compare with the blank group P＜0.01.
Claims (10)
1. a general flavone from blackberry lily (forming) extract by flavonoid glycoside and aglycon, in iridin, 100%＞Rhizoma Belamcandae isoflavone weight 〉=50%, the ratio between iridin and the irigenine is 1: (0.1-1).
2. extract according to claim 1 in iridin, is preferably 100%＞Rhizoma Belamcandae isoflavone weight 〉=80%.
3. general flavone from blackberry lily glucoside extract, in iridin, 100%＞Rhizoma Belamcandae isoflavone weight 〉=50%, 100%＞iridin weight 〉=10%.
4. extract according to claim 3 in iridin, is preferably weight 〉=25% of 100%＞Rhizoma Belamcandae isoflavone weight 〉=80%, 100%＞iridin.
5. general flavone from blackberry lily aglycon extract, in irigenine, the weight of 100%＞Rhizoma Belamcandae isoflavone weight 〉=50%, 100%＞irigenine is 〉=10%.
6. extract according to claim 5 in irigenine, is preferably 100%＞Rhizoma Belamcandae isoflavone weight 〉=80%, 100%＞irigenine weight 〉=25%.
7. the arbitrary described extract of claim 1-6, irigenine or the iridin application in the medicine of preparation treatment or prevention respiratory system disease.
8. application according to claim 7, the arbitrary described extract of claim 1-6, irigenine or iridin are in preparation treatment or prevent application in the medicine of acute and chronic pharyngolaryngitis, tonsillitis, pneumonia.
9. be the pharmaceutical composition of active component with the arbitrary described extract of claim 1-6, irigenine or iridin, the content range of its active component is 1-1000mg.
10. pharmaceutical composition according to claim 9, the content range of its active component is preferably 5-500mg.
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| CN101912156B (en) * | 2010-08-13 | 2013-01-30 | 川渝中烟工业有限责任公司 | Blackberry lily essential oil extraction method and application of blackberry lily essential oil in cigarette |
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| CN102603834B (en) * | 2012-01-17 | 2014-03-12 | 武汉回盛生物科技有限公司 | Method for extracting and separating tectoridin from iris tectorum |
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| TWI669122B (en) * | 2018-06-20 | 2019-08-21 | 大葉大學 | Use of tectoridin and extract containing thereof for preparation of medication for treatment of lung inflammation |
| CN110846354A (en) * | 2019-11-29 | 2020-02-28 | 邯郸学院 | Preparation method of blackberry lily isoflavone aglycone |
| CN110846354B (en) * | 2019-11-29 | 2021-05-04 | 邯郸学院 | Preparation method of blackberry lily isoflavone aglycone |
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