CN101129473B - Radix fici simplicissimatis extractive and method of producing the same and use thereof - Google Patents
Radix fici simplicissimatis extractive and method of producing the same and use thereof Download PDFInfo
- Publication number
- CN101129473B CN101129473B CN2007100298167A CN200710029816A CN101129473B CN 101129473 B CN101129473 B CN 101129473B CN 2007100298167 A CN2007100298167 A CN 2007100298167A CN 200710029816 A CN200710029816 A CN 200710029816A CN 101129473 B CN101129473 B CN 101129473B
- Authority
- CN
- China
- Prior art keywords
- fici simplicissimae
- radix fici
- extract
- simplicissimae extract
- ethanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses an extract of five-finger wild peach and the preparing method. The extract of five-finger wild peach contains coumarins and chromocor, wherein the mass percent content of coumarins is 15%-40%, the mass percent content of chromocor is 20%-55%. The invention also discloses the application of the five-finger wild peach in the medicine of treating the urgent and chronic bronchitis, asthma, pneumonectasis, chronic obstructive pulmonary disease, immune disease, viral hepatitis, chronic hepatitis B. The medicine composition with five-finger wild peach extract as the active component can be made into tablet, capsule, granule, ball, oral liquid, mist or the like. The preparing method of the invention is simple and low cost, which can produce continuously. The invention gets celery element by separating and purifying from five-finger wild peach firstly and gets the efficient section extract of chromocor and coumarins from five-finger wild peach.
Description
Technical field
The present invention relates to a kind of natural plants effective part extract, particularly a kind of Radix Fici Simplicissimae extract and its production and use.
Background technology
Herba Fici Simplicissimae is a Guangdong genuine traditional Chinese medicine material, Herba Fici Simplicissimae another name the five fingers milk, Herba Ipomoeae Cairicae, southern stilbene, and be described as " panacis quinquefolii radix ", refering in particular to formal name used at school is the dry root of moraceae plants ficus simplicissima Ficux hirta vahl..Use among the people has history of more than one thousand years to Herba Fici Simplicissimae in Guangdong, among the peoplely is used for the health care, and invigorating the spleen to clear away damp pathogen, relieving cough and resolving phlegm, tendon activating and callateral obstruction expelling effect are arranged.The use of Herba Fici Simplicissimae is with a long history, safe without toxic side effect, but the medical value of Herba Fici Simplicissimae can not get deep research always.Herba Fici Simplicissimae mainly concentrates on the treatment chronic lung disease at medication experience among the people and clinically, as chronic bronchitis, emphysema, pulmonary tuberculosis and treatment chronic hepatitis.But among the people and clinically, Herba Fici Simplicissimae mainly uses with the Chinese medicine compound form, and single medicinal material Herba Fici Simplicissimae application experience is few, is difficult to determine its medical value and meaning.Ceng Xiaochun is in Chinese Chinese medicine information magazine the 2nd phase of February in 2002, delivers the research article and shows that Herba Fici Simplicissimae has antitussive, eliminates the phlegm, antiasthmatic effect.Chinese patent application 200510002111.7 discloses the adjuvant therapy medicaments purposes of Herba Fici Simplicissimae at preparation chemical hepatic injury.But further investigate for the effective ingredient of Herba Fici Simplicissimae up to now always.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, primary and foremost purpose of the present invention is to provide a kind of Radix Fici Simplicissimae extract.
Another object of the present invention is to provide the preparation method of above-mentioned Radix Fici Simplicissimae extract.
A further object of the present invention is to provide the application of above-mentioned Radix Fici Simplicissimae extract.
Purpose of the present invention is achieved through the following technical solutions: a kind of Radix Fici Simplicissimae extract is prepared from as follows:
(1) Herba Fici Simplicissimae extracted 1～3 hour with the ethanol of 50～100% (V/V) or methanol heating extraction 1～3 time at every turn, filtered merge extractive liquid;
Perhaps, with 50～100% (V/V) ethanol or methanol dipping 12～24 hours, 3～10ml/kgmin speed percolation, collect the percolate of 8～16 times of weight 50～100% (V/V) ethanol or methanol.
(2) extracting solution that step (1) is obtained or percolate through concentrated eliminate ethanol or methanol after, after adding the water of 2～6 times of volumes, fully extract, collect the organic solvent dissolution part and eliminate solvent through concentrating with petroleum ether or ethyl acetate, drying promptly obtains Radix Fici Simplicissimae extract.
Perhaps, after extracting solution that step (1) is obtained or percolate concentrate and eliminate ethanol or methanol, adding 5～10% (V/V) dissolve with ethanol disperses the back to go up macroporous resin adsorption, first water wash with 2～4 times of column volume amounts, discard water wash liquid, 40～70% (V/V) ethanol elution of 2～6 times of column volume amounts of reuse is collected eluent and is eliminated solvent through concentrating, drying promptly gets Radix Fici Simplicissimae extract.
[chemical composition analysis of Radix Fici Simplicissimae extract]
Radix Fici Simplicissimae extract contains coumarin and flavone component, wherein accounts for 15～40% (mass percents) with coumarin component content in the ultraviolet spectrophotometer mensuration Radix Fici Simplicissimae extract, and flavone component content accounts for 20～55% (mass percents).Wherein, the coumarin composition is psoralen, bergapton class, and flavone component is the apigenin class.
Radix Fici Simplicissimae extract passes through silicagel column, the thin layer preparative hplc, with petroleum ether: the ethyl acetate gradient elution, use petroleum ether: the ethyl acetate crystallization, obtain psoralen, bergapton, apigenin respectively, it is as follows that process is chemical, the wave spectrum mode is measured these three chemical compound general formulas:
The preparation method of described Radix Fici Simplicissimae extract comprises the steps:
(1) Herba Fici Simplicissimae extracted 1～3 hour with 50～100% (V/V) ethanol or methanol heating extraction 1～3 time at every turn, filtered merge extractive liquid;
Perhaps, with 50～100% (V/V) ethanol or methanol dipping 12～24 hours, 3～10ml/kgmin speed percolation, collect the percolate of 8～16 times of weight 50～100% (V/V) ethanol or methanol;
(2) extracting solution that step (1) is obtained or percolate through concentrated eliminate ethanol or methanol after, behind the water with 2～6 times of volumes, fully extract, collect the organic solvent dissolution part and eliminate solvent through concentrating with petroleum ether or ethyl acetate, drying promptly obtains Radix Fici Simplicissimae extract;
Perhaps, after extracting solution that step (1) is obtained or percolate concentrate and eliminate ethanol or methanol, disperse the back to go up macroporous resin adsorption with 5～10% (V/V) dissolve with ethanol, first water wash with 2～4 times of column volume amounts, discard water wash liquid, 40～70% (V/V) ethanol elution of 2～6 times of column volume amounts of reuse is collected eluent and is eliminated solvent through concentrating, drying promptly gets Radix Fici Simplicissimae extract.
In order to realize the present invention better, in the step (1) preferred especially Herba Fici Simplicissimae with 50～100% (V/V) ethanol of 4～10 times of weight or methanol in 50～85 ℃ of heating extraction 1～3 time.
In the step (1), especially preferably use 50～100% (V/V) ethanol of 3～6 times of weight or methanol to flood 12～24 hours.
In the step (2), after especially preferably extracting solution that step (1) is obtained or percolate concentrate and eliminate ethanol or methanol, go up macroporous resin adsorption with 5～10% (V/V) dissolve with ethanol dispersion back of 2～6 times of volumes.
The pharmaceutical composition of above-mentioned Radix Fici Simplicissimae extract is as active component with Radix Fici Simplicissimae extract; Described pharmaceutical composition can be made into tablet, capsule, granule, drop pill, oral liquid or spray.
Radix Fici Simplicissimae extract of the present invention has cough-relieving, reduces phlegm, antiasthmatic effect, can use in medicines such as preparation acute/chronic bronchitis, asthma, emphysema or chronic obstructive pulmonary disease.
Radix Fici Simplicissimae extract of the present invention has the effect of the immunity of organisms of adjusting, can use in medicines such as hypoimmunity disease such as preparation tumor or acquired immune deficiency syndrome (AIDS).
Radix Fici Simplicissimae extract of the present invention has the hepatitis B virus DNA of inhibition and duplicates effect, can use in medicines such as preparation viral hepatitis or chronic hepatitis B.
The present invention compared with prior art has following advantage and beneficial effect:
Preparation method of the present invention is simple, production cost is low, can be continuously produced.The present invention first from Herba Fici Simplicissimae separation and purification obtain apigenin, show and contain apigenin flavonoid composition in the five fingers peach, and obtain the extract of flavone, coumarin effective site in Herba Fici Simplicissimae simultaneously, Radix Fici Simplicissimae extract of the present invention can be used for medicines such as preparation treatment chronic lung disease, chronic hepatitis, immunocompromised disease.Radix Fici Simplicissimae extract of the present invention can be marked, originally rule together in the treatment chronic lung disease, has tangible anti-pulmonary bronchial chronic inflammation, tangible cough-relieving arranged, eliminate the phlegm, antiasthmatic effect, and has tangible human body immunity improving power, improve respiratory tract defence capability, improve the resistivity of pulmonary's respiratory tract to destructive stimuluses such as various antibacterials, viruses, prevent the outbreak repeatedly of chronic lung disease, Radix Fici Simplicissimae extract has remarkable advantages at treatment chronic lung disease and present other medicines.Radix Fici Simplicissimae extract of the present invention has tangible anti-hepatitis B virus effect; and the immunological liver infringement that protection virus causes; make Radix Fici Simplicissimae extract realize direct antiviral simultaneously during chronic hepatitis B and through two kinds of approach of immunologic mechanism antiviral in treatment; improve its hepatitis B virus surface antigen negative conversion rate, compare with present treatment chronic hepatitis B medicine and have clear superiority.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment, but embodiments of the present invention are not limited thereto.
Embodiment 1: the preparation of Radix Fici Simplicissimae extract
Get Herba Fici Simplicissimae decoction pieces 10kg, use 80 ℃ of heating and refluxing extraction of 60kg 75% (V/V) ethanol 2 times, each 2 hours, filter, after merging filtrate (being extracting solution) concentrating under reduced pressure reclaimed and eliminates ethanol, concentrated solution fully extracted with ethyl acetate after adding the water of 3 times of volumes, collect the acetic acid ethyl acetate extract part, concentrating under reduced pressure reclaims ethyl acetate, eliminates solvent, must extract extractum, to extract the extractum vacuum drying, promptly obtain Radix Fici Simplicissimae extract 96g.
Embodiment 2: the preparation of Radix Fici Simplicissimae extract
Get Herba Fici Simplicissimae 10kg, use 50 ℃ of heating and refluxing extraction of 40kg 75% (V/V) methanol 3 times, extracted 1 hour at every turn, filter, merging filtrate (being extracting solution) concentrating under reduced pressure gets concentrated solution after reclaiming methanol.After adding 5% (V/V) dissolve with ethanol dispersion of 4 times of volumes, last 20 liters of AB-8 macroporous resin adsorption, remove impurity with the drip washing of 40L water elution, the ethanol drip washing of reuse 40L 70% (V/V), collect the eluent concentrating under reduced pressure and reclaim ethanol, get the Herba Fici Simplicissimae post and separate extractum, the extractum vacuum drying is promptly got Radix Fici Simplicissimae extract 85g.
Embodiment 3: the preparation of Radix Fici Simplicissimae extract
Get Herba Fici Simplicissimae 10kg, use 40kg 70% (V/V) alcohol dipping 24 hours, 3ml/kgmin speed percolation is collected the alcoholic acid percolate of 100kg 70% (V/V); Percolate after concentrating under reduced pressure eliminates ethanol, add the water of 2 times of volumes after, fully extract with petroleum ether, collect the organic solvent dissolution part and eliminate solvent through concentrating under reduced pressure, vacuum drying promptly obtains Radix Fici Simplicissimae extract 91g.
Embodiment 4: the preparation of Radix Fici Simplicissimae extract
Get Herba Fici Simplicissimae 10kg, use 30kg 100% (V/V) alcohol dipping 20 hours, 10ml/kgmin speed percolation is collected the alcoholic acid percolate of 80kg 100% (V/V); After the percolate concentrating under reduced pressure eliminates ethanol, after adding 10% (V/V) dissolve with ethanol dispersion of 2 times of volumes, last 20 liters of DA-201 macroporous resin adsorption, remove impurity with the drip washing of 80L water elution successively, the ethanol drip washing of reuse 120L 40% (V/V), collect the eluent concentrating under reduced pressure and reclaim ethanol, get the Herba Fici Simplicissimae post and separate extractum, the extractum vacuum drying is promptly got Radix Fici Simplicissimae extract 88g.
Embodiment 5: the preparation of Radix Fici Simplicissimae extract
Get Herba Fici Simplicissimae decoction pieces 10kg, use 85 ℃ of heating and refluxing extraction of 100kg 50% (V/V) ethanol 1 time, each 3 hours, filter, merging filtrate (being extracting solution) concentrating under reduced pressure reclaims and eliminates ethanol, and concentrated solution fully extracts with petroleum ether after adding the water of 6 times of volumes, collect petroleum ether extraction liquid part, concentrating under reduced pressure reclaims petroleum ether, eliminates solvent, must extract extractum, to extract the extractum vacuum drying, promptly obtain Radix Fici Simplicissimae extract 97g.
Embodiment 6: the preparation of Radix Fici Simplicissimae extract
Get Herba Fici Simplicissimae 10kg, flooded 12 hours, 8ml/kgmin speed percolation, the percolate of collection 160kg 50% methanol with 60kg 50% methanol; The percolate concentrating under reduced pressure eliminates methanol, after adding the 8% dissolve with ethanol dispersion of 4 times of volumes, last 20 liters of DA-201 macroporous resin adsorption, remove impurity with the drip washing of 60L water elution successively, the ethanol drip washing of reuse 100L 50% (V/V), collect the eluent concentrating under reduced pressure and reclaim ethanol, get the Herba Fici Simplicissimae post and separate extractum, the extractum vacuum drying is promptly got Radix Fici Simplicissimae extract 84g.
Embodiment 7: the mensuration of coumarin, flavone in the Radix Fici Simplicissimae extract
1. coumarin assay
Instrument: uv-spectrophotometric instrument: Perk Elmer Lambda 35 (Germany).
The preparation of reference substance solution: precision takes by weighing reference substance psoralen 4.9mg in the 50ml volumetric flask, add dissolve with ethanol and be diluted to scale, precision takes by weighing this solution 4ml in the 10ml volumetric flask, adds dissolve with ethanol and is diluted to scale, gets the 0.0392mg/ml reference substance solution.
The preparation of need testing solution: precision takes by weighing 1. Radix Fici Simplicissimae extract (embodiment 1 makes) 18.6mg respectively, 2. Radix Fici Simplicissimae extract (embodiment 2 makes) 18.4mg, 3. Radix Fici Simplicissimae extract (embodiment 3 makes) 18.5mg, 4. Radix Fici Simplicissimae extract (embodiment 4 makes) 18.4mg puts in the volumetric flask of 100ml, adds dissolve with ethanol and be diluted to scale to get need testing solution.Precision is measured four each 1ml of need testing solution in the 5ml volumetric flask respectively, adds the concentration that ethanol dilution to scale gets four need testing solutions and is respectively 0.0372mg/ml, 0.0368mg/ml, 0.0370mg/ml, 0.0368mg/ml.
Measure the selection of wavelength: scan 1. need testing solution of psoralen reference substance and sample respectively at 190～550nm, both all have an absworption peak at 286nm place, and peak shape changes gently, are convenient to quantitative assay, therefore, with 286nm as the mensuration wavelength.
The formulation of standard curve: accurate draw the psoralen reference substance solution each 0.2,0.4,0.6,0.8,1.0,1.2ml, be settled in the 5ml volumetric flask with ethanol respectively.With ethanol is blank, measures in the 286nm place.With concentration (C) is abscissa, and absorbance (A) is the vertical coordinate mapping, gets regression equation: A=0.0672C-0.0241 (r
2=0.9995, n=6).The result shows that psoralen reference substance solution concentration is in 1.57～9.41 μ g/ml scopes, and the linear relationship of absorbance and concentration is good.
The result is as shown in table 1 for the coumarin assay.
1. table 1 measure, 2., 3., the 4. content results of total coumarins in the sample
2. flavones content is measured
Instrument: uv-spectrophotometric instrument: Perk Elmer Lambda 35 (Germany).
The preparation of reference substance solution: precision takes by weighing reference substance apigenin 4.7mg in the 50ml volumetric flask, add dissolve with ethanol and be diluted to scale, precision takes by weighing this solution 4ml in the 10ml volumetric flask, adds dissolve with ethanol and is diluted to scale, gets the 0.0376mg/ml reference substance solution.
The preparation of need testing solution: precision takes by weighing 1. Radix Fici Simplicissimae extract (embodiment 1 makes) 18.6mg respectively, 2. Radix Fici Simplicissimae extract (embodiment 2 makes) 18.4mg, 3. Radix Fici Simplicissimae extract (embodiment 3 makes) 18.5mg, 4. Radix Fici Simplicissimae extract (embodiment 4 makes) 18.4mg puts in the volumetric flask of 100ml, adds dissolve with ethanol and be diluted to scale to get need testing solution.Precision is measured four each 1ml in the 5ml volumetric flask respectively, adds the concentration that ethanol dilution to scale gets four test samples and is respectively 0.0372mg/ml, 0.0368mg/ml, 0.0370mg/ml, 0.0368mg/ml.
Measure the selection of wavelength: accurate respectively absorption apigenin reference substance solution reaches 1. need testing solution, put respectively in the 5mL measuring bottle, add the 5%NaOH alcoholic solution of 1mL, add ethanol, shake up to scale, in 50 ℃ of heating in water bath 2h, be placed to room temperature, make blank with corresponding reagent, with reference to ultraviolet one visible spectrophotometry, in 190～600nm wave-length coverage, carry out spectral scan, investigate maximum absorption wavelength.The result shows that reference substance solution and need testing solution all have absorption maximum at the 250nm place, so determine that 250nm is for measuring wavelength.
The formulation of standard curve: accurate draw the apigenin reference substance solution each 0.8,1.0,1.2,1.4,1.6,1.8ml, develop the color by the NaOH coloration method.With ethanol is blank, measures in the 250nm place.With concentration (C) is abscissa, and absorbance (A) is the vertical coordinate mapping, gets regression equation: A=0.066C-0.2786 (r
2=0.9993, n=6).The result shows that apigenin reference substance solution concentration is in 6.02～13.54 μ g/ml scopes, and the linear relationship of absorbance and concentration is good.
The flavones content measurement result is as shown in table 2.
1. table 2 measure, 2., 3., 4. content of total flavone result in the sample
Embodiment 8: the Radix Fici Simplicissimae extract cough-relieving, reduce phlegm, Study on Antiasthmatic
Medicine: 1. Radix Fici Simplicissimae extract (embodiment 1 makes), 2. Radix Fici Simplicissimae extract (embodiment 2 makes), 3. Radix Fici Simplicissimae extract (embodiment 3 makes), 4. Radix Fici Simplicissimae extract (embodiment 4 makes).
Animal: SPF level NIH mice, 18～22g, male and female half and half; The albefaction Cavia porcellus, 200g～220g, male and female half and half.
Instrument: YLS-8A is multi-functional to be lured to cough to draw and breathes heavily instrument, 752N type ultraviolet-uisible spectrophotometer, SIGMA3K30 high-speed refrigerated centrifuge, Sartorius BS224S ten thousand/electronic balance.
1, mice ammonia is caused the influence of coughing:
Get the NIH mice, male and female half and half are divided into 7 groups at random, are respectively blank group, codeine phosphate matched group, oleum viticis negundo dripping pills matched group, Radix Fici Simplicissimae extract 1., 2., 3., 4. four groups, every group of 5.20 crude drugs/kg dosed administration.Each administration group is gastric infusion according to dosage, and blank group gives the equal-volume normal saline, every day 1 time, 3d continuously.Behind the last administration 1h, with mice by only put into YLS-8A multi-functional lure to cough to draw breathe heavily instrument, by instrument spraying ammonia 15s, cough latent period of record mice and the cough number of times in the 2min calculate cough number of times suppression ratio.
Table 3 Radix Fici Simplicissimae extract causes the influence of coughing to mice ammonia
Annotate: 1. codeine, Oleum Viticis Negundo dosage unit are mg/kg; 2. compare with the blank group,
*P＜0.05,
*P＜0.01.
Experimental result is as shown in table 3, and Radix Fici Simplicissimae extract has tangible antitussive effect, and the Radix Fici Simplicissimae extract antitussive effect approaches the codeine antitussive effect, and obviously is better than the antitussive effect of Oleum Viticis Negundo.
2, to the influence of the phenol red excretion of mice trachea:
Get the NIH mice, male and female half and half are divided into 7 groups at random, are respectively blank group, ammonia chloride matched group, oleum viticis negundo dripping pills matched group, Radix Fici Simplicissimae extract 1., 2., 3., 4. four groups, every group of 5.20 crude drugs/kg dosed administration.Each administration group is gastric infusion according to dosage, and matched group gives the equal-volume normal saline, every day 1 time, 3d continuously.Behind the last administration 1h, each Mus is 0.01mL/g according to dosage
-1The phenol red solution of body weight lumbar injection 5%, injection back 0.5h puts to death the dislocation of mice cervical vertebra, faces upward the position and is fixed on the operation plate and cuts off throat skin, separate trachea, peel off the trachea surrounding tissue, cut the trachea of thyroid cartilage lower edge, with 5% sodium bicarbonate solution 0.5mL flushing trachea to the trachea crotch, continuous 3 times, eluate merges, and places on the ultraviolet-uisible spectrophotometer and to measure A in 546nm wavelength place, and calculate phenol red concentration in the irrigation of trachea liquid according to the standard curve of formulating before the experiment.
Experimental result is as shown in table 4, and Radix Fici Simplicissimae extract has tangible phlegm-dispelling functions, and the Radix Fici Simplicissimae extract phlegm-dispelling functions obviously is better than Oleum Viticis Negundo, near the ammonia chloride phlegm-dispelling functions.
3, histamine's spraying is caused the influence of Cavia porcellus asthma:
Get Cavia porcellus, male and female half and half are divided into 7 groups at random, are respectively blank group, aminophylline matched group, oleum viticis negundo dripping pills matched group, Radix Fici Simplicissimae extract 1., 2., 3., 4. four groups, every group of 5.20 crude drugs/kg dosed administration.Each administration group is gastric infusion according to dosage, and matched group gives the equal-volume normal saline, every day 1 time, 3d continuously.Behind the last administration 1h, with Cavia porcellus by only put into YLS-8A multi-functional lure to cough to draw breathe heavily instrument, by instrument spraying 1mg/mL histamine phosphate 1min, observation and record Cavia porcellus begin to the time (promptly draw and breathe heavily incubation period) that tic is fallen takes place from accepting spraying, draw to breathe heavily and surpass 5min person incubation period in 5min, to breathe heavily latent time poor to draw before and after the administration, calculates to draw and breathe heavily latent time.
Table 4 Radix Fici Simplicissimae extract is with the influence of the phenol red excretion of mice trachea
Annotate: 1. ammonia chloride, Oleum Viticis Negundo dosage unit are mg/kg; 2. compare with the blank group,
*P＜0.05,
*P＜0.01.
Table 5 Herba Fici Simplicissimae is to the influence of histamine's spraying Cavia porcellus asthma
Annotate: 1. aminophylline, Oleum Viticis Negundo dosage unit are mg/kg.
Experimental result is as shown in table 5, and Radix Fici Simplicissimae extract has tangible antiasthmatic effect, and the Radix Fici Simplicissimae extract antiasthmatic effect approaches the aminophylline effect, and obviously is better than the antiasthmatic effect of Oleum Viticis Negundo
Embodiment 9: the research of Radix Fici Simplicissimae extract treatment chronic bronchitis
Medicine: 1. Radix Fici Simplicissimae extract (embodiment 1 makes), 2. Radix Fici Simplicissimae extract (embodiment 2 makes), 3. Radix Fici Simplicissimae extract (embodiment 3 makes), 4. Radix Fici Simplicissimae extract (embodiment 4 makes).
Reagent: endotoxin.
Instrument: ten thousand/electronic scale, automatic clinical chemistry analyzer, Olympus microscope etc.
Animal: SPF level Wistar rat.
Get male SPF level Wistar rat, body weight 180～220g, be divided at random blank group, COPD model group (model group), oleum viticis negundo dripping pills positive drug group, Radix Fici Simplicissimae extract 1., 2., 3., 4. four groups of every group of 5.20 crude drugs/kg dosed administrations, 10 every group.Except that the blank group, all the other are respectively organized rat and injected 2g/2L endotoxin LPS (Sigma company) 200uL in the trachea in the 1st, 14 days, and (except the 14d) inserted rat in the lucite storehouse in the 2nd～28 day, injected big Qianmen cigarette with filter tip smog, about 5% (v/v) of concentration, 0.5h/d.In the time of modeling, each administration group is gastric infusion according to dosage, and blank group and model group give the equal-volume distilled water, every day 1 time, 28d continuously.
Diameter in the picked at random HE stained is measured in bronchus morphology, and (100～200um) more regular bronchia cross sections, every animal selects 3, adopts multifunctional colour image analysis system (CMIAS).The tube chamber measurement module is measured following index: lumen diameter, tube chamber external diameter.
Table 6 Radix Fici Simplicissimae extract influences rat chronic bronchitis bronchial wall thickness
Annotate: 1. the Oleum Viticis Negundo dosage unit is mg/kg; 2. compare with model group,
*P＜0.05,
*P＜0.01.
Experimental result is as shown in table 6, and Radix Fici Simplicissimae extract can obviously alleviate bronchioles inflammation that sootiness+LPS causes rat chronic bronchitis model and thicken narrowly, and effect obviously is better than the Oleum Viticis Negundo matched group.Show that the five fingers hair has the effect of obvious treatment bronchial chronic inflammation.
Embodiment 10: Radix Fici Simplicissimae extract is to hepatitis B virus surface antigen and the antigenic inhibitory action of e
Medicine: 1. Radix Fici Simplicissimae extract (embodiment 1 makes), 2. Radix Fici Simplicissimae extract (embodiment 2 makes), 3. Radix Fici Simplicissimae extract (embodiment 3 makes), 4. Radix Fici Simplicissimae extract (embodiment 4 makes); Culture fluid is made into 5mg/ml, 1000 rev/mins centrifugal 5 minutes, the aseptic filtration of 0.2um filter membrane.
Experiment cell: 2.2.15 cell strain.
2.2.15 cell strain is to change clone's HBV-DNA and anti-6418 plasmids over to human hepatoma cell strain HepG2 simultaneously and set up with the cotransfection method, can secrete HbsAg, HBcAg and complete Dane granule steadily in the long term, be external anti-HBV drug screening at present and estimate cell model preferably.2.2.15 cell DMEM culture fluid, culture fluid adds 10% hyclone, the 100U/ml penicillin, and the 100U/ml streptomycin, 80ug/ml G418,0.03% glutaminase is transferred pH to 6.8 with 0.238%Hepes.With 0.06% trypsin the 2.2.15 cell is dispersed into the individual cells suspension, by 3 * 10
4Cell/0.1ml/ hole branch is planted in 96 orifice plates, use the pastille culture fluid behind the 2d instead, each concentration adds four holes, according to the preliminary experiment result, 3 groups of Radix Fici Simplicissimae extract are diluted to 8 concentration 10mg/ml, 5mg/ml, 2.50mg/ml, 1.25g/ml, 0.625mg/ml, 0.312mg/ml, 0.156mg/ml, 0.078mg/ml respectively with cell maintenance medium, and establish blank group and cell matched group.Behind cytosis 11d, suct clear liquid and measure HBsAg and HBeAg with the ELISA method, remaining cell is measured drug cell toxicity with mtt assay.Mtt assay is measured the half toxic concentration of medicine cell growth, adds 400ug/ml MTT 0.1ml/ hole, 37 ℃ of 5%CO to cell
2Hatch 4h, visible yellow black first is collected together granule, discards MTT liquid, adds 100%DMSO 0.1ml/ hole, treat that first is collected together granule and dissolved (about 10min) fully after, with microplate reader 570nm wavelength mensuration OD value, blank is established four holes, adds 100%DMSO 0.1ml/ hole.Be calculated as follows half toxic concentration (TC
50).
A=log＞50% drug level; B=log＜50% drug level; C=A-B
The detection of HBsAg, HBeAg is adopted ELISA to measure box and is detected.Measure every hole OD value with microplate reader 450/630nm dual wavelength, and calculate the medium effective concentration (IC of medicine
50)
A=log＞50% drug level; B=log＜50% drug level; C=A-B;
Therapeutic index (TI) TI=TC
50/ IC
50
Select HBsAg, HBeAg Preliminary screening index as effect of drugs, measure the cytotoxicity concentration of medicine by mtt assay, and the corresponding therapeutic index that calculates estimates the clinical drug application prospect, wherein TI＞2 are effective low toxicity, 1＜TI＜2 are that poor efficiency is poisonous, and TI＜1 is a toxic action.Result of study shows that it is less influenced by the survival of reagent thing pair cell, and therapeutic index all belongs to effective low toxicity greater than 2, and Radix Fici Simplicissimae extract is outstanding inhibitory action to the secretion of HBsAg and HBeAg.
Table 7 Herba Fici Simplicissimae extracts inhibition effect and the cytotoxicity thereof to HBsAg and HBeAg
Experimental result is as shown in table 7, and Radix Fici Simplicissimae extract has obvious external anti-HBsAg and HBeAg effect.
Embodiment 11: Radix Fici Simplicissimae extract is to the protective effect research of immunological liver infringement
Medicine: 1. Radix Fici Simplicissimae extract (embodiment 1 makes), 2. Radix Fici Simplicissimae extract (embodiment 2 makes), 3. Radix Fici Simplicissimae extract (embodiment 3 makes), 4. Radix Fici Simplicissimae extract (embodiment 4 makes).
Animal: SPF level NIH mice, 18～22g, male and female half and half.
Experiment mice is divided into 7 groups at random, model group, positive drug matched group, Radix Fici Simplicissimae extract 1., 2., 3., 4. four groups, every group of 5.20 crude drugs/kg dosed administration, (BCG, bacteria containing amount is about 5 * 10 to every each injection of BCG vaccine of tail vein
6/ only) and 0.2ml, blank group injection equal-volume physiologic dose brine 0.2ml, the medication group is administered once every day, infects behind the BCG 12 days, and behind the last administration 2h, the ivLPS10ug/ Mus is surveyed the serum transaminase level behind the 16h.
Table 8 Radix Fici Simplicissimae extract is to the protective effect of BCG+LPS inducing mouse immunologic liver injury
Annotate: 1. the bifendate dosage unit is mg/kg; 2. compare with the blank group,
*P＜0.05,
*P＜0.01.
Experimental result is as shown in table 8; obviously raise with BCG+LPS induction of immunity liver damage model mouse Serum ALT; and Radix Fici Simplicissimae extract can significantly reduce Serum ALT levels, and near blank group, illustrates that Radix Fici Simplicissimae extract has obvious protective effect to the mouse immune liver damage.
Embodiment 12: Radix Fici Simplicissimae extract causes the low effect of immune function of mice to cyclophosphamide
Experiment medicine: 1. Radix Fici Simplicissimae extract (embodiment 1 makes), 2. Radix Fici Simplicissimae extract (embodiment 2 makes), 3. Radix Fici Simplicissimae extract (embodiment 3 makes), 4. Radix Fici Simplicissimae extract (embodiment 4 makes).
Laboratory animal: female Sexual health Balb/c mice, body weight 18～22g.
Get 72 of female healthy mices, be divided into 7 groups at random, normal saline blank group, Radix Fici Simplicissimae extract 1., 2., 3., 4. four groups, every group of 5.20 crude drugs/kg dosed administration, model group, 12 every group.Except that the normal control group, all the other respectively organize the respectively every 3d of mice intraperitoneal injection of cyclophosphamide 30mg/kg, 60mg/kg, 120mg/kg respectively, totally 3 times during the experiment beginning.Begin gastric infusion by each dosage group simultaneously, normal control group and cyclophosphamide model group are irritated stomach every day and are given normal saline with volume.2 weeks of administration, behind last administration 30min, mice is put to death, dissect, get spleen, thymus is accurately weighed.Result organ index (mg/10g)=thymus or spleen weight (mg)/mice body weight * 10g.
Table 9 Radix Fici Simplicissimae extract is to normal mouse immune organ, spleen index, the influence of thymus index
Annotate: contrast with the blank group
*P＜0.01.
Experimental result is as shown in table 9, cause that with cyclophosphamide mouse immune hangs down drag, mouse spleen index and thymus index obviously reduce, to cause mouse immune low and Radix Fici Simplicissimae extract can significantly resist cyclophosphamide, and, illustrate that Radix Fici Simplicissimae extract is to the effect of being significantly improved of mouse immune power near blank group.
Embodiment 13: Radix Fici Simplicissimae extract is to the influence of macrophage phagocytosis of mice
Experiment medicine: 1. Radix Fici Simplicissimae extract (embodiment 1 makes), 2. Radix Fici Simplicissimae extract (embodiment 2 makes), 3. Radix Fici Simplicissimae extract (embodiment 3 makes), 4. Radix Fici Simplicissimae extract (embodiment 4 makes).
Laboratory animal: female Sexual health Balb/c mice, body weight 18～22g.
Get 50 female Sexual health Balb/c mices, be divided into 6 groups at random, normal saline blank group, Radix Fici Simplicissimae extract 1., 2., 3., 4. four groups, every group of 5.20 crude drugs/kg dosed administration, HUANGQI KELI matched group, 10 every group.Organize medicine to mouse stomach to each respectively, give 7d continuously.Took off neck on the 8th day and put to death mice, cut off abdominal cavity skin rapidly, aseptic injection Hank ' s solution 3ml gently rubs abdominal part in the abdominal cavity, extracts peritoneal fluid, and the centrifugal 10min of 1000r/min gets supernatant.Be settled to 5ml with the PH7.4 phosphate buffer, add 0.5% chicken red blood cell 0.4ml, in 37 ℃, 5%CO
2Foster case is hatched 30min.Get 1～2 centrifugal push jack, with Rui Shi liquid dyeing 1 minute, add the equivalent distilled water again, mix gently, after 5 minutes, use distilled water flushing, wait to do, oily mirror is observed microscopy down, calculates and engulfs percent=(engulfing the macrophage number of macrophage number/counting of CRBC) * 100% and phagocytic index=(the macrophage number of CRBC number/counting of being engulfed).
Table 10 Radix Fici Simplicissimae extract is to the influence of macrophage phagocytosis of mice
Annotate: contrast with the blank group
*P＜0.05,
*P＜0.01
Experimental result is as shown in table 10, and Radix Fici Simplicissimae extract can obviously improve the mouse macrophage phagocytic activity, and effect obviously is better than Radix Astragali matched group.
Embodiment 14: the preparation of Radix Fici Simplicissimae extract drop pill
The weight proportion of Herba Fici Simplicissimae drop pill each component is:
Radix Fici Simplicissimae extract 4.35g
Polyethylene Glycol (4000) 26.10g
Polyethylene Glycol (6000) 6.53g
The method for preparing the Herba Fici Simplicissimae drop pill is as follows:
Polyethylene Glycol (4000) 26.10g, Polyethylene Glycol (6000) 6.53g are placed in the water-bath and heat, make fusion; Add the 4.35g Radix Fici Simplicissimae extract, stir, continue to stir 98 ℃ of heat preservation for standby use; With the preheating of drop pill machine, fluid storage compartment constant temperature is 98 ± 2 ℃, and the cooling soybean oil is chilled to 10～12 ℃ in advance, regulates drip nozzle and the distance of cooling off liquid level, pours medicinal liquid into fluid storage compartment, starts valve, and medicinal liquid is dropwise splashed in the coolant, drips speed and is about 30 droplets/minute; Open and collect a mouthful valve, collect drop pill, gauze filtering coolant, and absorb surperficial remaining oil stain, and spread out, dry, promptly get the Radix Fici Simplicissimae extract drop pill of molding.
Embodiment 15: the capsular preparation of Radix Fici Simplicissimae extract
The weight proportion of Herba Fici Simplicissimae capsule each component is:
Radix Fici Simplicissimae extract 5g
Starch 100g
Lactose 20g
Hyprolose 20g
Polyoxyethylene sorbitan monoleate 16g
Pulvis Talci 2.5g
To cross 60 mesh sieves by Radix Fici Simplicissimae extract, starch, lactose and the hyprolose of said ratio and be mixed, and add the polyoxyethylene sorbitan monoleate of 16g, the system soft material is crossed 20 mesh sieves and is granulated.20 mesh sieve granulate are crossed in 40～50 ℃ of baking oven forced air dryings, dried granule, add the Pulvis Talci of 2.5g, mix homogeneously.Press No. 1 capsule of recipe quantity fill, promptly get the Radix Fici Simplicissimae extract capsule.
Embodiment 16: the preparation of Radix Fici Simplicissimae extract sheet
The weight proportion of Herba Fici Simplicissimae sheet each component is:
Radix Fici Simplicissimae extract 5g
Starch 100g
Microcrystalline Cellulose 20g
Carboxymethyl cellulose sodium 20g
Polyoxyethylene sorbitan monoleate 16g
Pulvis Talci 2.5g
To cross 60 mesh sieves by Radix Fici Simplicissimae extract, starch and microcrystalline Cellulose, the Carboxymethyl cellulose sodium of said ratio and be mixed, and add the polyoxyethylene sorbitan monoleate of 16g, the system soft material is crossed 20 mesh sieves and is granulated.40～50 ℃ of baking oven forced air dryings.Dried granule is crossed 20 mesh sieve granulate, adds the Pulvis Talci of 2.5g, mix homogeneously, and tabletting promptly gets the Radix Fici Simplicissimae extract sheet.
Embodiment 17: the particulate preparation of Radix Fici Simplicissimae extract
The weight proportion of Herba Fici Simplicissimae granule each component is:
Radix Fici Simplicissimae extract 5g
Methylcellulose 15g
Icing Sugar 240g
Radix Fici Simplicissimae extract, methylcellulose and Icing Sugar by the said ratio mix homogeneously, are made soft material with 70% ethanol, granulate, fling to ethanol, make granule, promptly get the Radix Fici Simplicissimae extract granule.
Embodiment 18: Herba Fici Simplicissimae extracts the preparation of oral liquid
Radix Fici Simplicissimae extract 5g
Icing Sugar 100g
Tween 80 10ml
Sterilized water 1000ml
To be dissolved in the 1000ml sterilized water by the Radix Fici Simplicissimae extract and the Icing Sugar of said ratio, add the 10ml tween 80, stir evenly dissolving, filter, be sub-packed in the 10ml brown bottle, put in the sterilization cabinet and sterilize, promptly get the Radix Fici Simplicissimae extract oral liquid.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
- 4. the preparation method of Radix Fici Simplicissimae extract according to claim 2 is characterized in that: 50～100% ethanol or methanol with 3～6 times of weight in the described step (1) flooded 12～24 hours.
- 5. the preparation method of Radix Fici Simplicissimae extract according to claim 2, it is characterized in that: after extracting solution that in the described step (2) step (1) is obtained or percolate concentrate and eliminate ethanol or methanol, go up macroporous resin adsorption with 5～10% dissolve with ethanols dispersion back of 2～6 times of volumes.
- 6. the preparation method of a kind of Radix Fici Simplicissimae extract according to claim 2, it is characterized in that: described Radix Fici Simplicissimae extract contains coumarin and flavone component, described coumarin composition quality degree accounts for 15～40%, and the flavone component mass percentage content accounts for 20～55%.
- 7. the pharmaceutical composition of the described Radix Fici Simplicissimae extract of claim 1, it is characterized in that: described pharmaceutical composition is as active component with Radix Fici Simplicissimae extract; Described pharmaceutical composition is made tablet, capsule, granule, drop pill, oral liquid or spray.
- 8. the application of the described Radix Fici Simplicissimae extract of claim 1 in preparation treatment acute/chronic bronchitis, asthma, emphysema or chronic obstructive pulmonary disease thing.
- 9. the application of the described Radix Fici Simplicissimae extract of claim 1 in preparation treatment hypoimmunity disease medicament.
- 10. the application of the described Radix Fici Simplicissimae extract of claim 1 in preparation treatment viral hepatitis or chronic hepatitis B medicine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100298167A CN101129473B (en) | 2007-08-21 | 2007-08-21 | Radix fici simplicissimatis extractive and method of producing the same and use thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100298167A CN101129473B (en) | 2007-08-21 | 2007-08-21 | Radix fici simplicissimatis extractive and method of producing the same and use thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101129473A CN101129473A (en) | 2008-02-27 |
| CN101129473B true CN101129473B (en) | 2010-07-14 |
Family
ID=39126983
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007100298167A Expired - Fee Related CN101129473B (en) | 2007-08-21 | 2007-08-21 | Radix fici simplicissimatis extractive and method of producing the same and use thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101129473B (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101911984A (en) * | 2010-08-27 | 2010-12-15 | 王勇 | Health-care plant oil and preparation method thereof |
| CN103356746A (en) * | 2012-03-30 | 2013-10-23 | 陈继慈 | Chinese herbal medicine composition for chronic bronchitis and quality control method thereof |
| CN103191105B (en) * | 2013-03-18 | 2015-08-19 | 中山大学 | One class furocoumarin compound is preparing the application in anti-hepatitis B virus (HBV) medicine |
| CN103784685B (en) * | 2014-03-05 | 2016-02-03 | 江苏农牧科技职业学院 | Chinese medicine composition for the treatment of livestock and poultry virus sexually transmitted disease and its preparation method and application |
| CN104585244B (en) * | 2014-10-08 | 2017-08-29 | 江西农业大学 | A kind of preparation method of radix fici simplicissimatis extractive and its radix fici simplicissimatis extractive of preparation and purposes |
| CN104940625A (en) * | 2015-06-10 | 2015-09-30 | 刘冰 | Traditional Chinese medicine composition for treating chronic obstructive lung disease |
| CN107703242A (en) * | 2017-09-26 | 2018-02-16 | 暨南大学 | A kind of detection method of content of psoralen in radix fid simplids simae and apiolin |
| CN108283672A (en) * | 2018-01-18 | 2018-07-17 | 深圳中科锐智糖尿病研究所 | A kind of drug for treating hepatitis B |
| CN111671749A (en) * | 2020-06-12 | 2020-09-18 | 重庆医科大学 | Application of dicoumarol in preparation of HBx protein stability inhibitor |
| CN115873672B (en) * | 2022-07-29 | 2024-07-30 | 江南大学 | Bacterial biomembrane scavenger and preparation method thereof |
| CN116171857B (en) * | 2023-02-27 | 2023-12-05 | 广西壮族自治区农业科学院 | Method for efficiently rooting of Ficus simplicissima lour outside bottle |
-
2007
- 2007-08-21 CN CN2007100298167A patent/CN101129473B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101129473A (en) | 2008-02-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101129473B (en) | Radix fici simplicissimatis extractive and method of producing the same and use thereof | |
| CN102114044B (en) | Artificially processed bear bile powder and preparation method thereof | |
| CN100574768C (en) | A kind of anticancer pharmaceutical composition and its production and use | |
| CN101869595A (en) | Preparation method and quality detection method of liquorice and gall oral liquid | |
| CN103784427B (en) | Containing the pharmaceutical composition of eudesmane type sesquiterpene and the application in pharmacy thereof | |
| CN103356728B (en) | Pharmaceutical composition, preparation method thereof, preparations thereof and application thereof | |
| CN100493522C (en) | Medicinal composition of oxymatrine and polysaccharide | |
| CN102198192B (en) | Traditional Chinese medicine composition for treating HINI and application thereof | |
| CN1923241B (en) | Medicine composition containing epimedium extract, uncaria extract, and gastrodine, and its preparation and use | |
| CN101011543B (en) | Antineoplastic medicine composition | |
| CN113559207A (en) | Traditional Chinese medicine composition for clearing lung, eliminating phlegm, relieving cough and asthma and application thereof | |
| CN113616764B (en) | Antiviral traditional Chinese medicine composition and application thereof | |
| CN100482266C (en) | Medical composite prepared by sarcandra and oldenlandia | |
| CN103655544A (en) | Application of jaceosidin in preparation of drugs used for preventing or treating chronic liver injury and hepatic fibrosis | |
| CN102133336B (en) | Traditional Chinese medicine composite, and preparation method and application thereof | |
| CN102362993B (en) | Chinese medicinal preparation with effects of protecting intestines and removing toxic materials, and preparation method thereof | |
| CN102697800B (en) | Herba stellariae mediae polysaccharide composition and the application in preparation antiviral drugs thereof | |
| CN105572262A (en) | Method for detecting traditional Chinese medicine composition heat clearing and dredging granules | |
| CN102349956B (en) | Compound extract for moisturizeing pathogenic dryness and relieving itching and preparation thereof | |
| CN101371861A (en) | High-efficient antiviral medicament composition in chickweed as well as preparation method and use thereof | |
| CN101485753B (en) | Chinese medicine for treating hepatitis B and preparation method thereof | |
| CN101502536B (en) | Cedar total flavone and preparation method and medical application thereof | |
| CN105017376B (en) | A kind of Herba Sarcopyramis nepalensis steroidal saponin and application thereof | |
| CN104069149A (en) | Method for processing traditional Chinese medicine decoction piece by using bear gall as matrix | |
| CN106822229A (en) | A kind of application of subprostrate sophora polysaccharide active component |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Maoming Liqi Pharmaceutical Co.,Ltd. Assignor: Heyuan Jinyuan Green Life Co.,Ltd. Contract record no.: 2011440000905 Denomination of invention: Radix fici simplicissimatis extractive and method of producing the same and use thereof Granted publication date: 20100714 License type: Exclusive License Open date: 20080227 Record date: 20110809 |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100714 Termination date: 20210821 |