CN101108228A - Pharmaceutical composition and method of preparing the same - Google Patents

Pharmaceutical composition and method of preparing the same Download PDF

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CN101108228A
CN101108228A CNA2006100993626A CN200610099362A CN101108228A CN 101108228 A CN101108228 A CN 101108228A CN A2006100993626 A CNA2006100993626 A CN A2006100993626A CN 200610099362 A CN200610099362 A CN 200610099362A CN 101108228 A CN101108228 A CN 101108228A
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weight portion
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ethanol
pharmaceutical composition
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CN100553660C (en
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王秉岐
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Guilong Pharmaceutical Anhui Co Ltd
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XIAMEN GUILONG INVESTMENT MANAGEMENT CO Ltd
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Abstract

The invention discloses a remedy compound to treat acute and chronic bronchitis, bronchial asthma, emphysema merger and cor pulmonale and the preparation process thereof. The compound is mainly composed of cassia twig, baked licorice, os draconis, oyster, radix paeoniaalba, pinellia tuberifera, pericarpium trichosanthis, and fried bitter almond. The process comprises the following steps: percolate the cassia twig and collect the percolated liquid; decoct the left cassia twig and other materials by adding water, then mix and filter the decoction and concentrate the filter liquor into paste; crush the cassia twig and part of radix paenoiaalba into fine powder and sieve and mix uniformly; decoct the left radix paenoiaabla and other materials by adding water, mix and filter the decoction, then decompress and concentrate the filter liquor to add conventional accessories. The medicine can be made into any acceptable clinical formulations according to the conventional way. The invention also provides the quality control method of the remedy compound and the usage in preparation for the acute and chronic bronchitis, bronchial asthma, emphysema merger and cor pulmonale drugs.

Description

A kind of pharmaceutical composition and preparation method thereof
Technical field
The present invention relates to a kind of pharmaceutical composition and preparation method thereof and method of quality control, particularly a kind of pharmaceutical composition for the treatment of acute/chronic bronchitis, bronchial asthma and merging emphysema thereof, pulmonary heart disease and preparation method thereof and method of quality control.
Background technology
Cough, expectorant, to breathe heavily be the modal clinical manifestation of respiratory system disease.Pathogenesis is mainly exterior deficiency, invades lung, spleen, renal function imbalance in the exopathogen.Lung controlling breathing, kidney governing inspiration is come in and gone out with department's gas.The lung being damaged by lasted cough, impairment of dispersing and descending function of the lung, pneumonopathy and spleen, dysfunction of the spleen in transportation is given birth in expectorant is turbid, on then do in lung, phlegm stagnancy is given birth to heat, obstruction of lung-QI intercepts air flue and breathing heavily is short; Instability of kidney QI is taken the photograph and is received not normally, and gas is not returned unit, and superinverse is breathed heavily in lung.The principle of traditional Chinese medical science utilization determination of treatment based on pathogenesis obtained through differentiation of symptoms and signs, treatment is from integral body.And western medical treatment mainly relies on antibiotic therapy, takes for a long time, is easy to generate drug resistance, state of an illness long-term control poor effect.
Summary of the invention
The object of the invention is to provide a kind of pharmaceutical composition, and another purpose of the present invention is to provide this preparation of drug combination method, method of quality control and uses thereof.
The present invention seeks to be achieved through the following technical solutions:
The crude drug of pharmaceutical composition of the present invention consists of:
Ramulus Cinnamomi 5-20 weight portion Radix Glycyrrhizae 3-9 weight portion Os Draconis 10-30 weight portion
Concha Ostreae 10-30 weight portion Radix Paeoniae Alba 5-20 weight portion Rhizoma Pinelliae Preparatum 6-15 weight portion
Pericarpium Trichosanthis 5-20 weight portion Semen Armeniacae Amarum 6-15 weight portion Rhizoma Coptidis 0.5-5 weight portion.
The preferred weight proportioning is:
Ramulus Cinnamomi 10 weight portion Radix Glycyrrhizae Preparatas 6 weight portion Os Draconis 20 weight portions
The Concha Ostreae 20 weight portion Radix Paeoniae Albas 10 weight portion Rhizoma Pinelliae Preparatum 9 weight portions
Pericarpium Trichosanthis 10 weight portion Semen Armeniacae Amarum (parched) 9 weight portion Rhizoma Coptidis 2 weight portions;
Ramulus Cinnamomi 6 weight portion Radix Glycyrrhizae Preparatas 8 weight portion Os Draconis 12 weight portions
The Concha Ostreae 28 weight portion Radix Paeoniae Albas 8 weight portion Rhizoma Pinelliae Preparatum 14 weight portions
Pericarpium Trichosanthis 7 weight portion Semen Armeniacae Amarum (parched) 14 weight portion Rhizoma Coptidis, 1 weight portions or
Ramulus Cinnamomi 18 weight portion Radix Glycyrrhizae Preparatas 4 weight portion Os Draconis 28 weight portions
The Concha Ostreae 12 weight portion Radix Paeoniae Albas 15 weight portion Rhizoma Pinelliae Preparatum 7 weight portions
Pericarpium Trichosanthis 19 weight portion Semen Armeniacae Amarum (parched) 7 weight portion Rhizoma Coptidis 4 weight portions.
The invention described above pharmaceutical composition also can add Rhizoma Zingiberis Recens, the Fructus Jujubae two flavor crude drug of following weight portion and form:
Rhizoma Zingiberis Recens 5-15 weight portion Fructus Jujubae 5-15 weight portion.
The preferred weight proportioning is: Rhizoma Zingiberis Recens 10 weight portions, Fructus Jujubae 10 weight portions; Rhizoma Zingiberis Recens 14 weight portions, Fructus Jujubae 8 weight portions or Rhizoma Zingiberis Recens 6 weight portions, Fructus Jujubae 14 weight portions.
Pharmaceutical composition crude drug of the present invention adds conventional adjuvant, according to common process, makes clinical acceptable any dosage form, as: capsule, pill, tablet, granule, soft extract with bee honey agent, oral liquid or injection.
The concrete preparation technology of pharmaceutical composition soft extract with bee honey preparation of the present invention is as follows:
The above-mentioned raw materials medicine, Ramulus Cinnamomi is that solvent carries out percolation according to percolation with 90% ethanol, collects percolate; Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug are decocted with water 2-4 time, and each 0.5-2 hour, collecting decoction filtered the clear paste that it is 1.25-1.33 that filtrate is concentrated into 80 ℃ of relative densities; Get sucrose 350-400 weight portion, add Mel 35-40 weight portion, after adding water boil and dissolving, boil and transform 2-4 hour; Add 320-380 weight portion liquid glucose, mixing; Add above-mentioned clear paste again, stir evenly, boil, 100 ℃ of relative densities are 1.33～1.39 thick paste; Constantly stir and make cooling, when waiting to be chilled to 45-55 ℃, add Ramulus Cinnamomi percolate and 0.5-1 ‰ essence, receive cream, promptly.
The preferred for preparation technology of pharmaceutical composition soft extract with bee honey preparation of the present invention is as follows:
The above-mentioned raw materials medicine, Ramulus Cinnamomi is that solvent carries out percolation according to percolation with 90% ethanol, collects percolate; Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug are decocted with water three times, and 2 hours for the first time, 1 hour for the second time, 0.5 hour for the third time, collecting decoction filtered the clear paste that it is 1.28-1.3 that filtrate is concentrated into 80 ℃ of relative densities; Get sucrose 380 weight portions, add Mel 38 weight portions, after adding water boil and dissolving, boil and transform 3 hours; Add 350 weight portion liquid glucoses, mixing; Add above-mentioned clear paste again, stir evenly, boil, get 100 ℃ of thick pastes that relative density is 1.34-1.38; Constantly stir and make cooling, when waiting to be chilled to 50 ℃, add Ramulus Cinnamomi percolate and 0.75 ‰ essence, receive cream, promptly.
The concrete preparation technology of medicament composition granule agent of the present invention is as follows:
The above-mentioned raw materials medicine, Ramulus Cinnamomi is that solvent carries out percolation according to percolation with 90% ethanol, collects percolate; With the Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug, decoct with water 2-4 time, each 0.5-2 hour, collecting decoction, filter, relative density was the clear paste of 1.20-1.38 when filtrate was concentrated into 60 ℃, added the Ramulus Cinnamomi percolate, mixing adds conventional adjuvant, makes granule.
The preferred for preparation technology of medicament composition granule agent of the present invention is as follows:
The above-mentioned raw materials medicine, Ramulus Cinnamomi is that solvent carries out percolation according to percolation with 90% ethanol, collects percolate; With the Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug, decoct with water three times, 2 hours for the first time, 1 hour for the second time, 0.5 hour for the third time, collecting decoction filters, and relative density was the clear paste of 1.25-1.33 when filtrate was concentrated into 60 ℃, add the Ramulus Cinnamomi percolate, mixing adds conventional adjuvant, makes granule.
The concrete preparation technology of medicament composition capsule agent of the present invention is as follows:
The above-mentioned raw materials medicine, the Radix Paeoniae Alba of getting Ramulus Cinnamomi and half weight portion is ground into fine powder, sieves mixing; The remaining Radix Paeoniae Alba and all the other crude drug decoct with water 2-4 time, and each 0.5-2 hour, collecting decoction filtered, and it is 1.25-1.30 that filtrate decompression is concentrated into 60 ℃ of relative densities, add above-mentioned fine powder, mixing, cold drying is ground into fine powder, sieve, mixing incapsulates, promptly.
The preferred for preparation technology of medicament composition capsule agent of the present invention is as follows:
The above-mentioned raw materials medicine, the Radix Paeoniae Alba of getting Ramulus Cinnamomi and half weight portion is ground into fine powder, sieves mixing; The remaining Radix Paeoniae Alba and all the other crude drug decoct with water three times, and 2 hours for the first time, 1 hour for the second time, for the third time half an hour, collecting decoction filters, it is 1.26-1.29 that filtrate decompression is concentrated into 60 ℃ of relative densities, adds above-mentioned fine powder, mixing, cold drying, be ground into fine powder, sieve, mixing, incapsulate, promptly.
The method of quality control of pharmaceutical composition soft extract with bee honey preparation of the present invention comprises following discriminating and/or assay:
Discriminating comprises one or more in the following method:
A, get pharmaceutical composition soft extract with bee honey preparation of the present invention 30 grams, add the 30ml water dissolution, add the 25-35ml ether gently jolting extract, place layering, divide and get ether solution, put in 40 ℃ of water-baths and fling to ether, residue adds the 2ml dissolve with ethanol, as need testing solution; Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the solution that every 1ml contains 10 μ l, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with 60-90 ℃ of petroleum ether-ethyl acetate ratio be 15-20: 1-5 as developing solvent, launch, take out, dry, spray is with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
B, get pharmaceutical composition soft extract with bee honey preparation of the present invention 30 grams, add ethanol 60ml, room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill 10 minutes, divides and gets ethanol liquid; Get 20ml ethanol liquid, water-bath is steamed to thick, cooling, and residue adds 2ml ethanol, stirs dipping 10 minutes, leaves standstill, and gets supernatant as need testing solution; Other gets berberine hydrochloride and palmatine hydrochloride reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg respectively, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, putting respectively on same silica gel g thin-layer plate, is 5-9 with n-butyl alcohol-glacial acetic acid-water ratio: 1: 1-3 launches as developing solvent, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the fluorescence speckle of same color;
C, get pharmaceutical composition soft extract with bee honey preparation of the present invention 30 grams, add ethanol 60ml, room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill 10 minutes, divides and gets ethanol liquid; Get 30ml ethanol liquid, water-bath is steamed to 2ml, adds water 20ml, extract three times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, the water 15ml saturated with n-butyl alcohol washs once, discard water liquid, n-butyl alcohol liquid adds active carbon 0.3-0.8 gram, stirs evenly, filter, filtrate water bath method, residue add ethanol 1ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 6 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid ratio is 38-42: 4-6: 8-12: 0.1-0.3 is as developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
Assay in the method for quality control is as follows:
The test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica, acetonitrile-0.1% phosphoric acid solution ratio be 25-35: 65-75 as mobile phase, the detection wavelength is 285nm, number of theoretical plate should be not less than 2000 by the calculating of cinnamic acid peak; The preparation of reference substance solution, precision takes by weighing through the cinnamic acid reference substance 10mg of phosphorus pentoxide drying under reduced pressure to constant weight, put in the brown measuring bottle of 100ml, add 50% dissolve with methanol and be diluted to scale, shake up, precision is measured 0.7ml, put in the 10ml measuring bottle, add 50% methanol to scale, shake up, promptly get reference substance solution; Drug regimen soft extract with bee honey preparation 10 grams of the present invention are got in the preparation of need testing solution, and accurate the title decides, and adds water 20ml, stirs, and makes dissolving fully, and add chloroform and extract three times, each 20ml, placement is 30 minutes after the jolting, divides and gets chloroform solution; Combined chloroform liquid adds the 20g anhydrous sodium sulfate, jolting 10 minutes, filter, with 20-30ml chloroform washing container and filtering residue, washing liquid is incorporated in the filtrate, evaporate to dryness, filtering residue add 50% dissolve with methanol, move in the 50ml measuring bottle, add 50% methanol to scale, shake up, filter, get subsequent filtrate, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Algoscopy, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; The every 1g of pharmaceutical composition soft extract with bee honey preparation of the present invention contains Ramulus Cinnamomi with cinnamic acid C 9H 8O 2Meter must not be less than 0.020mg.
The method of quality control of pharmaceutical composition soft extract with bee honey preparation of the present invention is preferably as follows to be differentiated and/or assay:
Discriminating comprises one or more in the following method:
A, get pharmaceutical composition soft extract with bee honey preparation of the present invention 30 grams, add the 30ml water dissolution, add the 30ml ether gently jolting extract, place layering, divide and get ether solution, put in 40 ℃ of water-baths and fling to ether, residue adds the 2ml dissolve with ethanol, as need testing solution; Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the solution that every 1ml contains 10 μ l, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with 60-90 ℃ of petroleum ether-ethyl acetate ratio be 17: 3 as developing solvent, launch, take out, dry, spray is with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
B, get pharmaceutical composition soft extract with bee honey preparation of the present invention 30 grams, add ethanol 60ml, room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill 10 minutes, divides and gets ethanol liquid; Get 20ml ethanol liquid, water-bath is steamed to thick, cooling, and residue adds 2ml ethanol, stirs dipping 10 minutes, leaves standstill, and gets supernatant as need testing solution; Other gets berberine hydrochloride and palmatine hydrochloride reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg respectively, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol-glacial acetic acid-water ratio be 7: 1: 2 as developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the fluorescence speckle of same color;
C, get pharmaceutical composition soft extract with bee honey preparation of the present invention 30 grams, add ethanol 60ml, room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill 10 minutes, divides and gets ethanol liquid; Get 30ml ethanol liquid, water-bath is steamed to 2ml, adds water 20ml, extract three times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, the water 15ml saturated with n-butyl alcohol washs once, discard water liquid, n-butyl alcohol liquid adds active carbon 0.5 gram, stirs evenly, filter, filtrate water bath method, residue add ethanol 1ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 6 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid ratio is 40: 5: 10: 0.2 as developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
Assay in the method for quality control is as follows:
The test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica, acetonitrile-0.1% phosphoric acid solution ratio be 30: 70 as mobile phase, the detection wavelength is 285nm, number of theoretical plate should be not less than 2000 by the calculating of cinnamic acid peak; The preparation of reference substance solution, precision takes by weighing through the cinnamic acid reference substance 10mg of phosphorus pentoxide drying under reduced pressure to constant weight, put in the brown measuring bottle of 100ml, add 50% dissolve with methanol and be diluted to scale, shake up, precision is measured 0.7ml, put in the 10ml measuring bottle, add 50% methanol to scale, shake up, promptly get reference substance solution; Pharmaceutical composition soft extract with bee honey preparation 10 grams of the present invention are got in the preparation of need testing solution, and accurate the title decides, and adds water 20ml, stirs, and makes dissolving fully, and add chloroform and extract three times, each 20ml, placement is 30 minutes after the jolting, divides and gets chloroform solution; Combined chloroform liquid adds the 20g anhydrous sodium sulfate, jolting 10 minutes, filter, with 25ml chloroform washing container and filtering residue, washing liquid is incorporated in the filtrate, evaporate to dryness, filtering residue add 50% dissolve with methanol, move in the 50ml measuring bottle, add 50% methanol to scale, shake up, filter, get subsequent filtrate, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Algoscopy, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; The every 1g of pharmaceutical composition soft extract with bee honey preparation of the present invention contains Ramulus Cinnamomi with cinnamic acid C 9H 8O 2Meter must not be less than 0.020mg.
The method of quality control of drug combination preparation of the present invention shows that according to experimental result linear relationship is good between cinnamic acid peak area and the cinnamic acid amount; Chromatographic condition precision is good; This drug combination preparation stability, repeatability are good, response rate height.
Drug combination preparation of the present invention can relieving cough and resolving phlegm, lowering the adverse-rising QI to subdue asthma.Be used for disease and acute and chronic bronchitis such as cough that wind and cold or accumulation of phlegm-damp in the lung cause, asthma, accumulation and obstruction of sputum.The energy expelling pathognic wind from muscles that exterior symptoms gets is with the pathogen of loosing, and internal evidence gets it, the energy tonify deficiency therapeutic method to keep the adverse QI flowing downwards, spleen invigorating in the accent and regulating YIN and YANG, the dissipating fluid-retention softening the hard mass with control cough with asthma this, wash away that expectorant is turbid to accumulate strongly fragrant pathogenic heat with wind and cold, sharp lung the chest stuffiness relieving, and control cough with asthma expectorant heat at last mark, so for treatment is coughed, the good medicine of the turbid heap soil or fertilizer over and around the roots lung of the expectorant of panting.Clinical experiment shows: drug combination preparation total effective rate of the present invention is 92.70%, showing the control rate is 59.68%, good effect to cough, the expectoration of wind-cold type, phlegm-damp type, asthenic cold type, panting has better curative effect, the treatment acute/chronic bronchitis, is coughed, expectorant, is breathed heavily and truly have curative effect; Can obviously improve patient's ventilatory function, when acute bronchitis, chronic bronchitis or its concurrent infection, have infection, reduce peripheral white blood cells, pulmonary ventilation function improving effect.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
The experiment of experimental example 1 assay
Linear relationship is investigated: experimental result shows: between 0.025 μ g～0.1 μ g, linear relationship is good between peak area and the cinnamic acid amount in reference substance solution for cinnamic acid, and correlation coefficient r is 0.9992.
The breakdown of emulsion test method of chloroform solution: experimental result shows: add the 20g anhydrous sodium sulfate, get final product rapid breakdown of emulsion, water layer is absorbed by anhydrous sodium sulfate, chloroform layer is golden yellow to be separated, and through overtesting, do not have obvious influence to measurement result the standing time that adds behind the anhydrous sodium sulfate, carry cinnamic acid secretly in order to prevent anhydrous sodium sulfate, in the test the fine ground back of anhydrous sodium sulfate is added, simultaneously continuous jolting 10 minutes filters the back with chloroform washing container and sodium sulfate.
Negative interference test in the content assaying method: get negative sample solution 10 μ l, inject chromatograph of liquid, with the contrast of cinnamic acid reference substance solution, the result shows that negative solution is noiseless to cinnamic acid mensuration.
The precision test: prepare need testing solution as stated above, draw need testing solution, continuous sample introduction 5 times, each 10 μ l measure cinnamic acid peak area integrated value, and RSD (%) is 1.18, and the result shows that determined chromatographic condition precision is good.
Stability test: draw above-mentioned need testing solution 10 μ l respectively, in 3,6,9,12 hours sample introductions, measure its peak area integrated value, RSD (%) is 0.898, and the result shows that need testing solution peak area value in 12 hours is basicly stable.
Repeatability test: get 6 parts of pharmaceutical composition soft extract with bee honey of the present invention agent, every part is 10g, the accurate title, decide, be prepared into need testing solution by above-mentioned test sample preparation method, measure according to above-mentioned chromatographic condition, cinnamic acid content in the calculation sample, RSD (%) is 1.67, the result shows: this method repeatability is better.Recovery test: average recovery rate is 97.8%, and RSD is 1.57%, and method is feasible.
Sample determination and result: according to above-mentioned content assaying method, get test agent in 10 batches of different lot numbers respectively, be prepared into need testing solution as stated above, draw 10 μ l respectively, inject chromatograph of liquid, measure the content of cinnamic acid, the results are shown in Table 1.
Ten batches of pilot scale sample sizes of table 1 measurement result table
Lot number Content (mg/g) Average content (mg/g)
020105 020108 020109 020114 020115 020119 020121 020125 020128 020201 0.0332 0.0347 0.0347 0.0346 0.0309 0.0319 0.0324 0.0320 0.0344 0.0326 0.0325 0.0338 0.0339 0.0346 0.0307 0.0320 0.0342 0.0319 0.0345 0.0331 0.0328 0.0342 0.0343 0.0346 0.0308 0.0320 0.0333 0.0320 0.0344 0.0328
The average content of the cinnamic acid of test agent is between 0.0308～0.0344mg/g in above-mentioned 10 batches, average content is 0.0331mg/g, consider the problems such as loss in the big production, calculate according to 60% of average content, pharmaceutical composition soft extract with bee honey of the present invention agent contains Ramulus Cinnamomi must not be less than 0.020mg by the every gram content of cinnamic acid.
The clinical experiment of experimental example 2 treatment bronchitis, bronchial asthma and merging emphysema thereof, pulmonary heart disease
1. treatment 425 routine patients are observed in this clinical experiment altogether, are outpatient service and inpatient, are divided into observation group at random, two groups of matched groups.Observation group: 315 examples, male's 168 examples, women's 147 examples; Minimum 7 years old of age, maximum 82 years old, 48 ± 16 years old mean age; The course of disease is the shortest to be 2 days, and the longest is 40 years, 64 examples below 3 months, 90 examples below 10 years, 10-19 72 examples, 69 examples more than 20 years, state of an illness the lighter's 38 examples, moderate person's 91 examples, severe person's 186 examples; Matched group: 110 examples, male's 57 examples, women's 53 examples; Minimum 5 years old of age, maximum 85 years old, 44 ± 16 years old mean age; The course of disease is the shortest to be 1 day, and the longest is 50 years, 37 examples below 3 months, 41 examples below 10 years, 10-19 16 examples, 16 examples more than 20 years, state of an illness the lighter's 15 examples, moderate person's 38 examples, severe person's 57 examples.Learning processing aspect sex, age, the state of an illness by statistics, difference that there are no significant (P＞0.05) for two groups.
2. case is selected: all genus wind-cold types, phlegm-damp type, asthenic cold type person all can be used as the object of observation.Observation group: belong to wind-cold type 103 examples, phlegm-damp type 181 examples, asthenic cold type 31 examples belong to acute bronchitis person's 64 examples, chronic simple type bronchitis 78 examples, chronic asthmatic bronchitis 173 examples; Matched group: belong to wind-cold type 41 examples, phlegm-damp type 55 examples, asthenic cold type 14 examples belong to acute bronchitis person's 41 examples, chronic simple type bronchitis 26 examples, chronic asthmatic bronchitis 43 examples.
3. observational technique: observation group's drug combination preparation of the present invention, matched group FUFANG CHUANBEIJING capsule, two kinds of medicines are each 4, and 3 times on the one, oral, the 7-14 days course of treatment.Observation item: main observed content is bronchitic three primary symptoms: cough, expectoration, pant main physical signs: do moist rale, wheezing sound.And give paired observation in conjunction with pulmonary function, hemogram and Chest X-rays etc.
4. observed result and analysis:
(1) total effects: observation group's total effective rate is 92.7%, and the matched group total effective rate is 50%, two group and compares X 2=99.1954.P＜0.001; It is 59.68% that observation group shows the control rate, and the apparent control rate of matched group is 19.09%, two group and compares X 2=53.7483, P＜0.001; Two groups of total effective rates and apparent control rate all have significant differences, illustrate that observation group's curative effect is apparently higher than matched group.The results are shown in Table 2.
Table 2 liang group total effects relatively
Group The example number Face control Produce effects Take a turn for the better Invalid Effectively Show control
Example ％ Example ％ Example ％ Example ％ Example ％ Example ％
Observation group's matched group 315 110 59 10 18.73 9.09 129 11 40.95 10 104 34 33.02 30.91 23 55 7.3 50 29.2 55 92.7 50 188 21 59.68 19.09
Two groups of total effective rates are compared: X 2=99.1954, P＜0.001; Two groups show the control rate and compare: X 2=53.7483, P＜0.001.
The effective percentage of two groups of curative effects and apparent control rate all have the difference of highly significant.
(2) individual event curative effect: cough: observation group's effective percentage is 92.7%, and the matched group effective percentage is 49.09%, two group and compares X 2=102.449, P＜0.001; It is 65.08% that observation group shows the control rate, and the apparent control rate of matched group is 22.73%, two group and compares X 2=58.895, P＜0.001; Expectoration: observation group's effective percentage is 91.96%, and the matched group effective percentage is 44.76%, two group and compares X 2=109.4953, P＜0.001; It is 60.45% that observation group shows the control rate, and the apparent control rate of matched group is 19.05%, two group and compares X 2=53.8233, P＜0.001; Pant: observation group's effective percentage is 91.38%, and the matched group effective percentage is 43.55%, two group and compares X 2=62.6307, P＜0.001; It is 61.49% that observation group shows the control rate, and the apparent control rate of matched group is 17.74%, two group and compares X 2=35.0019, P＜0.001; Rale: observation group's effective percentage is 92.35%, and the matched group effective percentage is 54.39%, two group and compares X 2=45.1009, P＜0.001; It is 63.93% that observation group shows the control rate, and the apparent control rate of matched group is 24.56%, two group and compares X 2=27.1792, P＜0.001.The results are shown in Table 3.
Table 3 liang group individual event curative effect relatively
Project Group The example number Face control Produce effects Take a turn for the better Invalid Effectively Show control
Example ％ Example ％ Example ％ Example ％ Example ％ X 2 P Example ％ X 2 P
Cough Observation group 315 91 28.89 114 39.19 87 27.62 23 7.3 292 92.7 102.449 ＜0.001 205 65.08 58.895 ＜0.001
Matched group 110 12 10.91 13 11.82 29 26.36 56 50.91 54 49.09 25 22.73
Expectoration Observation group 311 61 19.61 127 40.84 98 31.51 25 8.04 286 91.96 109.495 ＜0.001 188 60.45 53.8233 ＜0.001
Matched group 105 8 7.62 12 11.43 27 25.71 58 55.24 47 44.76 20 19.05
Pant Observation group 174 47 27.01 60 34.48 52 29.89 15 8.62 159 91.38 62.6307 ＜0.001 107 64.19 35.0019 ＜0.001
Matched group 62 5 8.06 6 9.68 16 25.81 35 56.45 27 43.55 11 17.74
Rale Observation group 183 59 32.24 58 31.69 52 28.42 14 7.65 169 92.35 45.1009 ＜0.001 117 63.93 27.1792 ＜0.001
Matched group 57 7 12.28 7 12.28 17 29.82 26 45.61 31 54.39 14 24.56
Two groups of coughs, expectorations, pant, each individual event curative effect of rale compares, the P value of effective percentage and apparent control rate all＜0.001 has significant difference.
Illustrate observation group to cough, expectoration, pant and each individual event curative effect such as rale all obviously is better than matched group.
(3) doctor trained in Western medicine typing and therapeutic effect relationship: compare between two groups: the simple type and the type effective percentage of panting are respectively 94.87%, 90.75% in the observation group, and simple type is respectively 61.54%, 41.86% with the type effective percentage of panting in the matched group.Compare simple type X for two groups 2=18.599, P＜0.001, the type of panting X 2=53.531, P＜0.001; Simple type and the apparent control rate of the type of panting are respectively 55.13%, 60.69% in the observation group, and simple type is respectively 30.77%, 13.95% with the apparent control rate of the type of panting in the matched group; Compare simple type X for two groups 2=4.63, P＜0.02, the type of panting X 2=30.119, P＜0.001.The results are shown in Table 4.
Table 4 doctor trained in Western medicine typing and therapeutic effect relationship
Project Group The example number Face control Produce effects Take a turn for the better Invalid Effectively Show control
Example ％ Example ％ Example ％ Example ％ Example ％ X 2 P Example ％ X 2 P
Simple type Observation group 78 14 17.95 29 37.18 31 39.74 4 5.13 74 94.87 18.599 ＜0.001 43 55.13 4.63 ＜0.001
Matched group 26 5 19.23 3 11.54 8 30.77 10 38.46 16 61.54 8 30.77
The type of panting Observation group 173 36 20.81 69 39.88 52 30.06 16 9.25 157 90.75 53.531 ＜0.001 105 60.69 30.119 ＜0.001
Matched group 43 1 2.33 5 11.63 12 27.91 25 58.14 18 41.86 6 13.95
The simple type of observation group's doctor trained in Western medicine typing is described and pants the type curative effect all apparently higher than matched group.
(4) observation group's Chinese and western medicine typing and therapeutic effect relationship: the curative effect of the simple type and the type of panting compares no significant difference in the observation group, and effective percentage is compared X 2=1.194, P＞0.2; Show the control rate and compare X 2=0.6882, P＞0.4.
Illustrate that drug combination preparation of the present invention all has better curative effect to the simple type of chronic bronchitis and the type of panting.
(5) Chinese medical discrimination and therapeutic effect relationship: compare between two groups: wind and cold, phlegm-damp, asthenic cold type effective percentage are respectively 89.32%, 94.48%, 96.77% in the observation group, matched group wind and cold, phlegm-damp, asthenic cold type effective percentage are respectively 51.22%, 58.18%, 14.29%, compare wind-cold type X for two groups 2=25.2007, P＜0.001; Phlegm-damp type X 2=46.1952, P＜0.001; Asthenic cold type X 2=31.9445, P＜0.001; Observation group's wind and cold, phlegm-damp, asthenic cold type show the control rate and are respectively 61.17%, 58.56%, 64.52%, and matched group wind and cold, phlegm-damp, the apparent control rate of asthenic cold type are respectively 17.07%, 25.45%, 0, two group and compare wind-cold type X 2=22.8229, P＜0.001; Phlegm-damp type X 2=18.5015, P＜0.001; Asthenic cold type X 2=16.2581, P＜0.001; Illustrate that the various curative effect of observation group's Chinese medical discrimination is apparently higher than matched group.Observation group's Chinese medical discrimination and therapeutic effect relationship: curative effect no significant difference between observation group's three types.Effective percentage is compared X 2=3.4326, P＞0.1; Show the control rate and compare X 2=0.4773, P＞0.7.The results are shown in Table 5.
Table 5 Chinese medical discrimination and therapeutic effect relationship
Project Group The example number Face control Produce effects Take a turn for the better Invalid Effectively Show control
Example ％ Example ％ Example ％ Example ％ Example ％ X 2 P Example ％ X 2 P
Wind and cold Observation group is right 103 19 18.45 44 42.72 29 28.16 11 10.68 92 89.32 25.2007 ＜0.001 63 61.17 22.8229 ＜0.001
According to group 41 4 9.76 3 7.31 14 34.15 20 48.78 21 51.22 7 17.07
Phlegm-damp Observation group is right 181 33 18.23 73 40.33 65 35.91 10 5.52 171 94.48 46.1952 ＜0.001 106 58.56 18.5015 ＜0.001
According to group 55 6 10.91 8 14.55 18 32.73 23 41.82 32 58.18 14 25.45
Deficiency and coldness Observation group is right 31 8 25.81 12 38.71 10 32.26 1 3.23 30 96.77 31.9445 ＜0.001 20 64.52 16.2581 ＜0.001
According to group 14 0 0 0 0 2 14.29 0 85.71 2 14.29 0 0
Two groups of severity extents are light, in, heavy between effective percentage and apparent control rate there are no significant the difference (X of observation group 2=1.4943, P＞0.3 and X 2=4.5535, P＞0.1; Matched group X 2=1.1439, P＞0.5 and X 2=2.8715, P＞0.37.Compare effective percentage highly significant P＜0.01 for two groups.
Illustrate that drug combination preparation of the present invention all has better curative effect to treatment wind and cold, phlegm-damp, deficiency and coldness, cough.
(6) relation of the state of an illness and curative effect: observation group's state of an illness is than the lighter's 38 examples, and effective percentage 94.74% shows control rate 44.74%; Moderate person's 91 examples, effective percentage 94.51% shows control rate 64.84%; Severe person's 186 examples, effective percentage 90.86% shows control rate 60.22%; Matched group the lighter 15 examples, effective percentage 60% shows control rate 6.67%; Moderate person's 38 examples, effective percentage 52.63% shows control rate 15.79%; Severe person's 57 examples, effective percentage 45.61% shows control rate 24.57%; The state of an illness of matched group is light, in, heavy between effective percentage compare with apparent control rate and all do not have significant difference (X 2=1.1439, P＞0.5 and X 2=2.8715, P＞0.3); The state of an illness of observation group is light, in, heavy between effective percentage compare with apparent control rate and all do not have significant difference (X 2=1.4943, P＞0.3 and X 2=4.5535, P＞0.1); Observation group compares with matched group, and slight effective percentage and apparent control rate have the difference X of highly significant 2=10.1258, P＜0.01 and X 2=6.9499, p＜0.01; The effective percentage of moderate and apparent control rate have the difference X of highly significant 2=32.825, P＜0.001 and X 2=25.7943, P＜0.001, the effective percentage of severe and apparent control rate have the difference X of highly significant 2=56.3485, P＜0.001 and X 2=22.2150, P＜0.001.
The patient that severe extent is different is described, the curative effect of observation group all obviously is better than matched group.
5. lab test results:
(1) changes before and after the treatment of blood leucocyte counting: complete data person 163 examples before and after observation group's treatment, treatment proleukocyte weighted mean value is 12147.546 ± 3325.652, treatment back numeration of leukocyte meansigma methods is 9602.208 ± 2820.188, the average leukopenia 2445.337 ± 3307.469 in treatment back, change before and after the treatment relatively, t=9.4392, P＜0.001.
Complete data person 51 examples before and after the treatment of control group, treatment proleukocyte weighted mean value is 11933.333 ± 4973.677, be 9347.058 ± 2534.155 after the treatment, the average drop-out value of treatment back leukocyte is 2586.274 ± 4519.248, change before and after the treatment relatively, t=4.0819, P＜0.001.The results are shown in Table 6.
Change before and after the treatment of table 6 blood leucocyte counting
Group The example number Mm before the treatment 3X ±SD Treatment back mm 3X ±SD Change X ± SD before and after treating Change relatively before and after treating Change two groups before and after treating relatively
t p t p
Observation group 163 12147±3325 9602±2820 2445±3307 9.4392 ＜0.001 0.2420 0.8
Matched group 51 11933±4973 9347±2534 2586±4519 4.0819 ＜0.001 V＝212
Two groups of treatment front and back numeration of leukocyte all have the difference of highly significant, P＜0.001.Change before and after the treatment between two groups and compare there was no significant difference, P＞0.8.
Analysis-by-synthesis can find out that numeration of leukocyte changes before and after observation group's treatment highly significant difference, and highly significant difference is also arranged before and after the treatment of control group; Changing before and after the treatment between two groups does not relatively have significant difference, illustrates that two groups is similar in curative effect aspect the reduction leukocyte.
(2) change relatively before and after the pulmonary function treatment, the results are shown in Table 7.
Change relatively before and after the table 7 liang group pulmonary function treatment
Project Group The example number Mm before the treatment 3X±SD Treatment back mm 3X±SD Change X ± SD before and after treating Change relatively before and after treating Change two groups before and after treating relatively
t p t p
FVC Observation group 31 2.399±0.942 2.757±0.918 0.36±0.59 3.39 ＜0.02 1.53 ＞0.05
Matched group 13 2.313±0.831 2.456±0.958 0.14±0.24 2.12 ＞0.05
PEER Observation group 31 2.386±1.41 2.82±0.33 0.433±0.95 2.54 ＜0.02 1.19 ＞0.05
Matched group 13 2.45±2.03 2.51±1.88 0.663±0.95 0.24 ＞0.05
All there were significant differences for FVC and PEER after observation group was treated, P＜0.02.Treat the back variation between two groups and compare no significant difference, P＞0.05.
More than shown in, observation group's treatment back pulmonary ventilation function has remarkable change, more preceding average all has obviously and increases after FVC and the PEER treatment, increment is respectively 15% and 18%; Matched group ventilatory function treatment back does not have obviously improvement.
(3) fluoroscopy of chest: the Chest X-rays complete data person of observation group 219 examples, normal person's 58 examples before the treatment, unusual person's 161 examples wherein belong to chronic bronchitis changer 89 examples, chronic bronchitis concurrent infection person 24 examples, chronic bronchitis merges emphysema person's 45 examples, and chronic bronchitis merges emphysema, pulmonary heart disease person's 3 examples.Treatment back 93 examples transfer to normally, and unusual person's 126 examples wherein belong to chronic bronchitis changer 78 examples, merge emphysema 45 examples, and chronic bronchitis merges emphysema, pulmonary heart disease person's 3 examples.Treat preceding 24 routine concurrent infection persons, the inflammation shade all disappears.The treatment back is described along with the state of an illness alleviates, the performance of part patient X line also takes a turn for the better to some extent.
Following embodiment all can realize the described effect of above-mentioned experimental example.
The specific embodiment
Embodiment 1: the preparation of tablet
Ramulus Cinnamomi 10kg Radix Glycyrrhizae Preparata 6kg Os Draconis 20kg Concha Ostreae 20kg Radix Paeoniae Alba 10kg
Rhizoma Pinelliae Preparatum 9kg Pericarpium Trichosanthis 10kg Semen Armeniacae Amarum (parched) 9kg Rhizoma Coptidis 2kg.
Get the above-mentioned raw materials medicine, add conventional adjuvant,, make tablet according to common process.
Embodiment 2: the preparation of pill
Ramulus Cinnamomi 6kg Radix Glycyrrhizae Preparata 8kg Os Draconis 12kg Concha Ostreae 28kg Radix Paeoniae Alba 8kg
Rhizoma Pinelliae Preparatum 14kg Pericarpium Trichosanthis 7kg Semen Armeniacae Amarum (parched) 14kg Rhizoma Coptidis 1kg.
Get the above-mentioned raw materials medicine, add conventional adjuvant,, make pill according to common process.
Embodiment 3: the preparation of oral liquid
Ramulus Cinnamomi 6kg Radix Glycyrrhizae Preparata 8kg Os Draconis 12kg Concha Ostreae 28kg Radix Paeoniae Alba 8kg
Rhizoma Pinelliae Preparatum 14kg Pericarpium Trichosanthis 7kg Semen Armeniacae Amarum (parched) 14kg Rhizoma Coptidis 1kg Rhizoma Zingiberis Recens 14kg
Fructus Jujubae 8kg.
Get the above-mentioned raw materials medicine, add conventional adjuvant,, make oral liquid according to common process.
Embodiment 4: the preparation of injection
Ramulus Cinnamomi 18kg Radix Glycyrrhizae Preparata 4kg Os Draconis 28kg Concha Ostreae 12kg Radix Paeoniae Alba 15kg
Rhizoma Pinelliae Preparatum 7kg Pericarpium Trichosanthis 19kg Semen Armeniacae Amarum (parched) 7kg Rhizoma Coptidis 4kg.
Get the above-mentioned raw materials medicine, add conventional adjuvant,, make injection according to common process.
Embodiment 5: the preparation of capsule
Ramulus Cinnamomi 10kg Radix Glycyrrhizae Preparata 6kg Os Draconis 20kg Concha Ostreae 20kg Radix Paeoniae Alba 10kg
Rhizoma Pinelliae Preparatum 9kg Pericarpium Trichosanthis 10kg Semen Armeniacae Amarum (parched) 9kg Rhizoma Coptidis 2kg.
The above-mentioned raw materials medicine, the Ramulus Cinnamomi and the 5kg Radix Paeoniae Alba are ground into fine powder, sieve mixing; The remaining Radix Paeoniae Alba and all the other crude drug decoct with water 2 times, and 1 hour for the first time, 0.5 hour for the second time, collecting decoction filters the clear paste that it is 1.28-1.30 that filtrate decompression is concentrated into 60 ℃ of relative densities, add the Ramulus Cinnamomi fine powder, mixing, cold drying is ground into fine powder, sieve, mixing incapsulates, promptly.
Embodiment 6: the preparation of capsule
Ramulus Cinnamomi 6kg Radix Glycyrrhizae Preparata 8kg Os Draconis 12kg Concha Ostreae 28kg Radix Paeoniae Alba 8kg
Rhizoma Pinelliae Preparatum 14kg Pericarpium Trichosanthis 7kg Semen Armeniacae Amarum (parched) 14kg Rhizoma Coptidis 1kg.
The above-mentioned raw materials medicine, the Ramulus Cinnamomi and the 4kg Radix Paeoniae Alba are ground into fine powder, sieve mixing; The remaining Radix Paeoniae Alba and all the other crude drug decoct with water three times, and 2 hours for the first time, 1 hour for the second time, for the third time half an hour, collecting decoction filters, it is 1.26-1.29 that filtrate decompression is concentrated into 60 ℃ of relative densities, adds above-mentioned fine powder, mixing, cold drying, be ground into fine powder, sieve, mixing, incapsulate, promptly.
Embodiment 7: the preparation of capsule
Ramulus Cinnamomi 6kg Radix Glycyrrhizae Preparata 8kg Os Draconis 12kg Concha Ostreae 28kg Radix Paeoniae Alba 8kg
Rhizoma Pinelliae Preparatum 14kg Pericarpium Trichosanthis 7kg Semen Armeniacae Amarum (parched) 14kg Rhizoma Coptidis 1kg Rhizoma Zingiberis Recens 14kg
Fructus Jujubae 8kg.
Get Ramulus Cinnamomi and the 4kg Radix Paeoniae Alba is ground into fine powder, sieve mixing; The remaining Radix Paeoniae Alba and all the other crude drug decoct with water 4 times, and 2 hours for the first time, 1 hour for the second time, 1 hour for the third time, the 4th 0.5 hour, collecting decoction, filter, the clear paste that it is 1.25-1.27 that filtrate decompression is concentrated into 60 ℃ of relative densities adds above-mentioned fine powder, mixing, cold drying is ground into fine powder, sieve, mixing incapsulates, promptly.
Embodiment 8: the preparation of granule
Ramulus Cinnamomi 18kg Radix Glycyrrhizae Preparata 4kg Os Draconis 28kg Concha Ostreae 12kg Radix Paeoniae Alba 15kg
Rhizoma Pinelliae Preparatum 7kg Pericarpium Trichosanthis 19kg Semen Armeniacae Amarum (parched) 7kg Rhizoma Coptidis 4kg Rhizoma Zingiberis Recens 6kg
Fructus Jujubae 14kg.
The above-mentioned raw materials medicine, Ramulus Cinnamomi is that solvent carries out percolation according to the percolation under the fluid extract item with 90% ethanol, collects percolate; With the Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug, decoct with water 2 times, each 1.5 hours, collecting decoction filtered, and relative density was 1.37 clear paste when filtrate was concentrated into 60 ℃, added the Ramulus Cinnamomi percolate, and mixing adds conventional adjuvant, makes granule.
Embodiment 9: the preparation of granule
Ramulus Cinnamomi 6kg Radix Glycyrrhizae Preparata 8kg Os Draconis 12kg Concha Ostreae 28kg Radix Paeoniae Alba 8kg
Rhizoma Pinelliae Preparatum 14kg Pericarpium Trichosanthis 7kg Semen Armeniacae Amarum (parched) 14kg Rhizoma Coptidis 1kg Rhizoma Zingiberis Recens 14kg
Fructus Jujubae 8kg.
The above-mentioned raw materials medicine, Ramulus Cinnamomi is that solvent carries out percolation according to the percolation under the pharmacopeia fluid extract item with 90% ethanol, collects percolate; With the Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug, decoct with water three times, 2 hours for the first time, 1 hour for the second time, 0.5 hour for the third time, collecting decoction filters, and relative density was the clear paste of 1.25-1.33 when filtrate was concentrated into 60 ℃, add the Ramulus Cinnamomi percolate, mixing adds conventional adjuvant, makes granule.
Embodiment 10: the preparation of soft extract with bee honey
Ramulus Cinnamomi 10kg Radix Glycyrrhizae Preparata 6kg Os Draconis 20kg Concha Ostreae 20kg Radix Paeoniae Alba 10kg
Rhizoma Pinelliae Preparatum 9kg Pericarpium Trichosanthis 10kg Semen Armeniacae Amarum (parched) 9kg Rhizoma Coptidis 2kg Rhizoma Zingiberis Recens 10kg
Fructus Jujubae 10kg.
The above-mentioned raw materials medicine, Ramulus Cinnamomi is that solvent carries out percolation according to the percolation under the pharmacopeia fluid extract item with 90% ethanol, collects percolate; Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug are decocted with water 2 times, and 2 hours for the first time, 1 hour for the second time, collecting decoction filtered, and it is 1.28 clear paste that filtrate is concentrated into 80 ℃ of relative densities; Get sucrose 355kg, add Mel 38kg, after adding water boil and dissolving, boil and transform 3 hours; Add the 330kg liquid glucose, mixing; Add above-mentioned clear paste again, stir evenly, boil, 100 ℃ of relative densities are 1.35 thick paste; Constantly stir and make cooling, when waiting to be chilled to 50 ℃, add Ramulus Cinnamomi percolate and 0.6 ‰ essence, receive cream, promptly.
Embodiment 11: the preparation of soft extract with bee honey
Ramulus Cinnamomi 18kg Radix Glycyrrhizae Preparata 4kg Os Draconis 28kg Concha Ostreae 12kg Radix Paeoniae Alba 15kg
Rhizoma Pinelliae Preparatum 7kg Pericarpium Trichosanthis 19kg Semen Armeniacae Amarum (parched) 7kg Rhizoma Coptidis 4kg Rhizoma Zingiberis Recens 6kg
Fructus Jujubae 14kg.
The above-mentioned raw materials medicine, Ramulus Cinnamomi is that solvent carries out percolation according to the percolation under the fluid extract item with 90% ethanol, collects percolate; Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug are decocted with water 4 times, and 2 hours for the first time, 1 hour for the second time, 0.5 hour for the third time, the 4th time 0.5 hour, collecting decoction filtered, and it is 1.30 clear paste that filtrate is concentrated into 80 ℃ of relative densities; Get sucrose 398kg, add Mel 36kg, after adding water boil and dissolving, boil and transform 3 hours; Add the 370kg liquid glucose, mixing; Add above-mentioned clear paste again, stir evenly, boil, 100 ℃ of relative densities are 1.35 thick paste; Constantly stir and make cooling, when waiting to be chilled to 50 ℃, add Ramulus Cinnamomi percolate and an amount of 0.9 ‰ essence, receive cream, promptly.
Embodiment 12: the preparation of soft extract with bee honey
Ramulus Cinnamomi 6kg Radix Glycyrrhizae Preparata 8kg Os Draconis 12kg Concha Ostreae 28kg Radix Paeoniae Alba 8kg
Rhizoma Pinelliae Preparatum 14kg Pericarpium Trichosanthis 7kg Semen Armeniacae Amarum (parched) 14kg Rhizoma Coptidis 1kg.
The above-mentioned raw materials medicine, Ramulus Cinnamomi is that solvent carries out percolation according to the percolation under the fluid extract item with 90% ethanol, collects percolate; Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug are decocted with water three times, and 2 hours for the first time, 1 hour for the second time, 0.5 hour for the third time, collecting decoction filtered, and it is 1.28～1.3 clear paste that filtrate is concentrated into 80 ℃ of relative densities; Get sucrose 380kg, add Mel 38kg, after adding water boil and dissolving, boil and transform 3 hours; Add the 350kg liquid glucose, mixing; Add above-mentioned clear paste again, stir evenly, boil, get 100 ℃ of thick pastes that relative density is 1.35-1.36; Constantly stir and make cooling, when waiting to be chilled to 50 ℃, add Ramulus Cinnamomi percolate and 0.75 ‰ essence, receive cream, promptly.
Embodiment 13: the method for quality control of honey refining agent
Discrimination method: A, the content soft extract with bee honey preparation of getting among the embodiment 12 30 restrain, and add the 30ml water dissolution, add the jolting extraction gently of 30ml ether, place layering, divide and get ether solution, put in 40 ℃ of water-baths and fling to ether, and residue adds the 2ml dissolve with ethanol, as need testing solution; Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the solution that every 1ml contains 10 μ l, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with 60～90 ℃ of petroleum ether-ethyl acetate ratio be 17: 3 as developing solvent, launch, take out, dry, spray is with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
B, the content soft extract with bee honey preparation of getting among the embodiment 12 30 restrain, and add ethanol 60ml, and room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill 10 minutes, divides and gets ethanol liquid; Get 20ml ethanol liquid, water-bath is steamed to thick, cooling, and residue adds 2ml ethanol, stirs dipping 10 minutes, leaves standstill, and gets supernatant as need testing solution; Other gets berberine hydrochloride and palmatine hydrochloride reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg respectively, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol-glacial acetic acid-water ratio be 7: 1: 2 as developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the fluorescence speckle of same color;
C, the content soft extract with bee honey preparation of getting among the embodiment 12 30 restrain, and add ethanol 60ml, and room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill about 10 minutes, divides and gets ethanol liquid; Get 30ml ethanol liquid, water-bath is steamed to about 2ml, adds water 20ml, extract three times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, the water 15ml saturated with n-butyl alcohol washs once, discard water liquid, n-butyl alcohol liquid adds active carbon 0.5 gram, stirs evenly, filter, filtrate water bath method, residue add ethanol 1ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 6 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid ratio is 40: 5: 10: 0.2 as developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
Assay in the method for quality control is as follows:
The test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica, acetonitrile-0.1% phosphoric acid solution ratio be 30: 70 as mobile phase, the detection wavelength is 285nm, number of theoretical plate should be not less than 2000 by the calculating of cinnamic acid peak; The preparation of reference substance solution, precision takes by weighing through the cinnamic acid reference substance 10mg of phosphorus pentoxide drying under reduced pressure to constant weight, put in the brown measuring bottle of 100ml, add 50% dissolve with methanol and be diluted to scale, shake up, precision is measured 0.7ml, put in the 10ml measuring bottle, add 50% methanol to scale, shake up, promptly get reference substance solution; Content soft extract with bee honey preparation 10 grams among the embodiment 12 are got in the preparation of need testing solution, and accurate the title decides, and adds water 20ml, stirs, and makes dissolving fully, and add chloroform and extract three times, each 20ml, placement is 30 minutes after the jolting, divides and gets chloroform solution; Combined chloroform liquid adds the 20g anhydrous sodium sulfate, jolting 10 minutes, filter, with 25ml chloroform washing container and filtering residue, washing liquid is incorporated in the filtrate, evaporate to dryness, filtering residue add 50% dissolve with methanol, move in the 50ml measuring bottle, add 50% methanol to scale, shake up, filter, get subsequent filtrate, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Algoscopy, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; The every 1g of soft extract with bee honey preparation contains Ramulus Cinnamomi with cinnamic acid C 9H 8O 2Meter must not be less than 0.020mg.
Embodiment 14: the method for quality control of honey refining agent
Discrimination method: A, the content soft extract with bee honey preparation of getting among the embodiment 11 30 restrain, and add the 30ml water dissolution, add the jolting extraction gently of 26ml ether, place layering, divide and get ether solution, put in 40 ℃ of water-baths and fling to ether, and residue adds the 2ml dissolve with ethanol, as need testing solution; Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the solution that every 1ml contains 10 μ l, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with 60～90 ℃ of petroleum ether-ethyl acetate ratio be 16: 4 as developing solvent, launch, take out, dry, spray is with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
B, the content soft extract with bee honey preparation of getting among the embodiment 11 30 restrain, and add ethanol 60ml, and room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill about 10 minutes, divides and gets ethanol liquid; Get 20ml ethanol liquid, water-bath is steamed to thick, cooling, and residue adds 2ml ethanol, stirs dipping 10 minutes, leaves standstill, and gets supernatant as need testing solution; Other gets berberine hydrochloride and palmatine hydrochloride reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg respectively, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol-glacial acetic acid-water ratio be 6: 1: 2 as developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the fluorescence speckle of same color;
C, the content soft extract with bee honey preparation of getting among the embodiment 11 30 restrain, and add ethanol 60ml, and room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill about 10 minutes, divides and gets ethanol liquid; Get 30ml ethanol liquid, water-bath is steamed to about 2ml, adds water 20ml, extract three times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, the water 15ml saturated with n-butyl alcohol washs once, discard water liquid, n-butyl alcohol liquid adds active carbon 0.4 gram, stirs evenly, filter, filtrate water bath method, residue add ethanol 1ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 6 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid ratio is 39: 5: 9: 0.25 as developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color.
Embodiment 15: the method for quality control of honey refining agent
A, the content soft extract with bee honey preparation of getting among the embodiment 10 30 restrain, and add the 30ml water dissolution, add the jolting extraction gently of 34ml ether, place layering, divide and get ether solution, put in 40 ℃ of water-baths and fling to ether, and residue adds the 2ml dissolve with ethanol, as need testing solution; Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the solution that every 1ml contains 10 μ l, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with 60～90 ℃ of petroleum ether-ethyl acetate ratio be 19: 2 as developing solvent, launch, take out, dry, spray is with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
B, the content soft extract with bee honey preparation of getting among the embodiment 10 30 restrain, and add ethanol 60ml, and room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill about 10 minutes, divides and gets ethanol liquid; Get 20ml ethanol liquid, water-bath is steamed to thick, cooling, and residue adds 2ml ethanol, stirs dipping 10 minutes, leaves standstill, and gets supernatant as need testing solution; Other gets berberine hydrochloride and palmatine hydrochloride reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg respectively, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol-glacial acetic acid-water ratio be 8: 1: 2 as developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the fluorescence speckle of same color.
Embodiment 16: the method for quality control of honey refining agent
A, the content soft extract with bee honey preparation of getting among the embodiment 10 30 restrain, and add ethanol 60ml, and room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill about 10 minutes, divides and gets ethanol liquid; Get 20ml ethanol liquid, water-bath is steamed to thick, cooling, and residue adds 2ml ethanol, stirs dipping 10 minutes, leaves standstill, and gets supernatant as need testing solution; Other gets berberine hydrochloride and palmatine hydrochloride reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg respectively, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol-glacial acetic acid-water ratio be 7: 1: 1 as developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the fluorescence speckle of same color;
B, the content soft extract with bee honey preparation of getting among the embodiment 10 30 restrain, and add ethanol 60ml, and room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill about 10 minutes, divides and gets ethanol liquid; Get 30ml ethanol liquid, water-bath is steamed to about 2ml, adds water 20ml, extract three times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, the water 15ml saturated with n-butyl alcohol washs once, discard water liquid, n-butyl alcohol liquid adds active carbon 0.7 gram, stirs evenly, filter, filtrate water bath method, residue add ethanol 1ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 6 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid ratio is 41: 5: 11: 0.15 as developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color.
Embodiment 17: the method for quality control of honey refining agent
Assay in the method for quality control is as follows:
The test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica, acetonitrile-0.1% phosphoric acid solution ratio be 21: 74 as mobile phase, the detection wavelength is 285nm, number of theoretical plate should be not less than 2000 by the calculating of cinnamic acid peak; The preparation of reference substance solution, precision takes by weighing through the cinnamic acid reference substance 10mg of phosphorus pentoxide drying under reduced pressure to constant weight, put in the brown measuring bottle of 100ml, add 50% dissolve with methanol and be diluted to scale, shake up, precision is measured 0.7ml, put in the 10ml measuring bottle, add 50% methanol to scale, shake up, promptly get reference substance solution; Content soft extract with bee honey agent 10 grams among the embodiment 13 are got in the preparation of need testing solution, and accurate the title decides, and adds water 20ml, stirs, and makes dissolving fully, and add chloroform and extract three times, each 20ml, placement is 30 minutes after the jolting, divides and gets chloroform solution; Combined chloroform liquid adds the 20g anhydrous sodium sulfate, jolting 10 minutes, filter, with 21ml chloroform washing container and filtering residue, washing liquid is incorporated in the filtrate, evaporate to dryness, filtering residue add 50% dissolve with methanol, move in the 50ml measuring bottle, add 50% methanol to scale, shake up, filter, get subsequent filtrate, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Algoscopy, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; The every 1g of soft extract with bee honey preparation of the present invention contains Ramulus Cinnamomi with cinnamic acid C 9H 8O 2Meter must not be less than 0.020mg.
Embodiment 18: the method for quality control of honey refining agent
Discrimination method: A, the content soft extract with bee honey preparation of getting among the embodiment 11 30 restrain, and add the 30ml water dissolution, add the jolting extraction gently of 30ml ether, place layering, divide and get ether solution, put in 40 ℃ of water-baths and fling to ether, and residue adds the 2ml dissolve with ethanol, as need testing solution; Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the solution that every 1ml contains 10 μ l, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with 60～90 ℃ of petroleum ether-ethyl acetate ratio be 17: 3 as developing solvent, launch, take out, dry, spray is with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
B, the content soft extract with bee honey preparation of getting among the embodiment 11 30 restrain, and add ethanol 60ml, and room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill about 10 minutes, divides and gets ethanol liquid; Get 30ml ethanol liquid, water-bath is steamed to about 2ml, adds water 20ml, extract three times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, the water 15ml saturated with n-butyl alcohol washs once, discard water liquid, n-butyl alcohol liquid adds active carbon 0.5 gram, stirs evenly, filter, filtrate water bath method, residue add ethanol 1ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 6 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid ratio is 40: 5: 10: 0.2 as developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
Assay in the method for quality control is as follows:
The test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica, acetonitrile-0.1% phosphoric acid solution ratio be 30: 70 as mobile phase, the detection wavelength is 285nm, number of theoretical plate should be not less than 2000 by the calculating of cinnamic acid peak; The preparation of reference substance solution, precision takes by weighing through the cinnamic acid reference substance 10mg of phosphorus pentoxide drying under reduced pressure to constant weight, put in the brown measuring bottle of 100ml, add 50% dissolve with methanol and be diluted to scale, shake up, precision is measured 0.7ml, put in the 10ml measuring bottle, add 50% methanol to scale, shake up, promptly get reference substance solution; Content soft extract with bee honey preparation 10 grams among the embodiment 11 are got in the preparation of need testing solution, and accurate the title decides, and adds water 20ml, stirs, and makes dissolving fully, and add chloroform and extract three times, each 20ml, placement is 30 minutes after the jolting, divides and gets chloroform solution; Combined chloroform liquid adds the 20g anhydrous sodium sulfate, jolting 10 minutes, filter, with 25ml chloroform washing container and filtering residue, washing liquid is incorporated in the filtrate, evaporate to dryness, filtering residue add 50% dissolve with methanol, move in the 50ml measuring bottle, add 50% methanol to scale, shake up, filter, get subsequent filtrate, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Algoscopy, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; The every 1g of soft extract with bee honey preparation contains Ramulus Cinnamomi with cinnamic acid C 9H 8O 2Meter must not be less than 0.020mg.

Claims (22)

1. pharmaceutical composition for the treatment of acute/chronic bronchitis, bronchial asthma and merging emphysema thereof, pulmonary heart disease is characterized in that the crude drug of this pharmaceutical composition consists of:
Ramulus Cinnamomi 5-20 weight portion Radix Glycyrrhizae 3-9 weight portion Os Draconis 10-30 weight portion
Concha Ostreae 10-30 weight portion Radix Paeoniae Alba 5-20 weight portion Rhizoma Pinelliae 6-15 weight portion
Pericarpium Trichosanthis 5-20 weight portion Semen Armeniacae Amarum 6-15 weight portion Rhizoma Coptidis 0.5-5 weight portion.
2. pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug of this pharmaceutical composition consists of:
Ramulus Cinnamomi 10 weight portion Radix Glycyrrhizae Preparatas 6 weight portion Os Draconis 20 weight portions
The Concha Ostreae 20 weight portion Radix Paeoniae Albas 10 weight portion Rhizoma Pinelliae Preparatum 9 weight portions
Pericarpium Trichosanthis 10 weight portion Semen Armeniacae Amarum (parched) 9 weight portion Rhizoma Coptidis 2 weight portions.
3. pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug of this pharmaceutical composition consists of:
Ramulus Cinnamomi 6 weight portion Radix Glycyrrhizae Preparatas 8 weight portion Os Draconis 12 weight portions
The Concha Ostreae 28 weight portion Radix Paeoniae Albas 8 weight portion Rhizoma Pinelliae Preparatum 14 weight portions
Pericarpium Trichosanthis 7 weight portion Semen Armeniacae Amarum (parched) 14 weight portion Rhizoma Coptidis 1 weight portion.
4. pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug of this pharmaceutical composition consists of:
Ramulus Cinnamomi 18 weight portion Radix Glycyrrhizae Preparatas 4 weight portion Os Draconis 28 weight portions
The Concha Ostreae 12 weight portion Radix Paeoniae Albas 15 weight portion Rhizoma Pinelliae Preparatum 7 weight portions
Pericarpium Trichosanthis 19 weight portion Semen Armeniacae Amarum (parched) 7 weight portion Rhizoma Coptidis 4 weight portions.
5. as claim 1,2,3 or 4 described pharmaceutical compositions, it is characterized in that this pharmaceutical composition also adds following bulk drugs: Rhizoma Zingiberis Recens 5-15 weight portion Fructus Jujubae 5-15 weight portion.
6. pharmaceutical composition as claimed in claim 5 is characterized in that the crude drug of this pharmaceutical composition is: Rhizoma Zingiberis Recens 10 weight portion Fructus Jujubaes 10 weight portions.
7. pharmaceutical composition as claimed in claim 5 is characterized in that the crude drug of this pharmaceutical composition is: Rhizoma Zingiberis Recens 14 weight portions, Fructus Jujubae 8 weight portions.
8. pharmaceutical composition as claimed in claim 5 is characterized in that the crude drug of this pharmaceutical composition is: Rhizoma Zingiberis Recens 6 weight portions, Fructus Jujubae 14 weight portions.
9. as claim 1,2,3,4,6,7 or 8 described pharmaceutical compositions, it is characterized in that this pharmaceutical composition adds conventional adjuvant, be prepared into capsule, pill, tablet, granule, soft extract with bee honey agent, oral liquid or injection according to common process.
10. the preparation method of pharmaceutical composition soft extract with bee honey preparation as claimed in claim 9 is characterized in that this method is: getting Ramulus Cinnamomi by percolation, is that solvent carries out percolation with 90% ethanol, collects percolate; Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug are decocted with water 2-4 time, and each 0.5-2 hour, collecting decoction filtered the clear paste that it is 1.25-1.33 that filtrate is concentrated into 80 ℃ of relative densities; Get sucrose 350-400 weight portion, add Mel 35-40 weight portion, after adding water boil and dissolving, boil and transform 2-4 hour; Add 320-380 weight portion liquid glucose, mixing; Add above-mentioned clear paste again, stir evenly, boil, get 100 ℃ of thick pastes that relative density is 1.33-1.39; Constantly stir and make cooling, when waiting to be chilled to 45-55 ℃, add Ramulus Cinnamomi percolate and 0.5-1 ‰ essence, receive cream, promptly.
11. the preparation method of pharmaceutical composition soft extract with bee honey preparation as claimed in claim 10 is characterized in that this method is: getting Ramulus Cinnamomi according to the percolation under the fluid extract item, is that solvent carries out percolation with 90% ethanol, collects percolate; Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug are decocted with water three times, and 2 hours for the first time, 1 hour for the second time, 0.5 hour for the third time, collecting decoction filtered the clear paste that it is 1.28-1.3 that filtrate is concentrated into 80 ℃ of relative densities; Get sucrose 380 weight portions, add Mel 38 weight portions, after adding water boil and dissolving, boil and transform 3 hours; Add 350 weight portion liquid glucoses, mixing; Add above-mentioned clear paste again, stir evenly, boil, get 100 ℃ of thick pastes that relative density is 1.34-1.38; Constantly stir and make cooling, when waiting to be chilled to 50 ℃, add Ramulus Cinnamomi percolate and 0.75 ‰ essence, receive cream, promptly.
12. the preparation method of medicament composition granule agent as claimed in claim 9 is characterized in that this method is: getting Ramulus Cinnamomi according to percolation, is that solvent carries out percolation with 90% ethanol, collects percolate; With the Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug, decoct with water 2-4 time, each 0.5-2 hour, collecting decoction, filter, relative density was the clear paste of 1.20-1.38 when filtrate was concentrated into 60 ℃, added the Ramulus Cinnamomi percolate, mixing adds conventional adjuvant, makes granule.
13. the preparation method of medicament composition granule agent as claimed in claim 12 is characterized in that this method is: getting Ramulus Cinnamomi according to percolation, is that solvent carries out percolation with 90% ethanol, collects percolate; With the Ramulus Cinnamomi medicinal residues behind the percolation and all the other crude drug, decoct with water three times, 2 hours for the first time, 1 hour for the second time, 0.5 hour for the third time, collecting decoction filters, and relative density was the clear paste of 1.25-1.33 when filtrate was concentrated into 60 ℃, add the Ramulus Cinnamomi percolate, mixing adds conventional adjuvant, makes granule.
14. the preparation method of medicament composition capsule agent as claimed in claim 9, it is characterized in that this method is: the Radix Paeoniae Alba of getting Ramulus Cinnamomi and half weight portion is ground into fine powder, sieves mixing; The remaining Radix Paeoniae Alba and all the other crude drug decoct with water 2-4 time, and each 0.5-2 hour, collecting decoction filtered, and it is 1.23-1.32 that filtrate decompression is concentrated into 60 ℃ of relative densities, add above-mentioned fine powder, mixing, cold drying is ground into fine powder, sieve, mixing incapsulates, promptly.
15. the preparation method of medicament composition capsule agent as claimed in claim 14, it is characterized in that this method is: the Radix Paeoniae Alba of getting Ramulus Cinnamomi and half weight portion is ground into fine powder, sieves mixing; The remaining Radix Paeoniae Alba and all the other crude drug decoct with water three times, and 2 hours for the first time, 1 hour for the second time, for the third time half an hour, collecting decoction filters, it is 1.25-1.30 that filtrate decompression is concentrated into 60 ℃ of relative densities, adds above-mentioned fine powder, mixing, cold drying, be ground into fine powder, sieve, mixing, incapsulate, promptly.
16. the method for quality control as the soft extract with bee honey preparation of claim 1,2,3,4,6,7 or 8 described pharmaceutical compositions is characterized in that this method comprises following discriminating and/or assay:
Differentiate: A, get pharmaceutical composition soft extract with bee honey preparation 30 grams of the present invention, add the 30ml water dissolution, add the 25-35ml ether gently jolting extract, place layering, divide and get ether solution, put in 40 ℃ of water-baths and fling to ether, residue adds the 2ml dissolve with ethanol, as need testing solution; Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the solution that every 1ml contains 10 μ l, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with 60～90 ℃ of petroleum ether-ethyl acetate ratio be 15-20: 1-5 as developing solvent, launch, take out, dry, spray is with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
B, get pharmaceutical composition soft extract with bee honey preparation of the present invention 30 grams, add ethanol 60ml, room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill 10 minutes, divides and gets ethanol liquid; Get 20ml ethanol liquid, water-bath is steamed to thick, cooling, and residue adds 2ml ethanol, stirs dipping 10 minutes, leaves standstill, and gets supernatant as need testing solution; Other gets berberine hydrochloride and palmatine hydrochloride reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg respectively, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, putting respectively on same silica gel g thin-layer plate, is 5-9 with n-butyl alcohol-glacial acetic acid-water ratio: 1: 1-3 launches as developing solvent, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the fluorescence speckle of same color;
C, get pharmaceutical composition soft extract with bee honey preparation of the present invention 30 grams, add ethanol 60ml, room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill 10 minutes, divides and gets ethanol liquid; Get 30ml ethanol liquid, water-bath is steamed to 2ml, adds water 20ml, extract three times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, the water 15ml saturated with n-butyl alcohol washs once, discard water liquid, n-butyl alcohol liquid adds active carbon 0.3-0.8 gram, stirs evenly, filter, filtrate water bath method, residue add ethanol 1ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 6 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid ratio is 38-42: 4-6: 8-12: 0.1-0.3 is as developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
Assay: chromatographic condition and system suitability test, with octadecylsilane chemically bonded silica is filler, acetonitrile-0.1% phosphoric acid solution ratio be 25-35: 65-75 as mobile phase, the detection wavelength is 285nm, number of theoretical plate calculates by the cinnamic acid peak and should be not less than 2000; The preparation of reference substance solution, precision takes by weighing through the cinnamic acid reference substance 10mg of phosphorus pentoxide drying under reduced pressure to constant weight, put in the brown measuring bottle of 100ml, add 50% dissolve with methanol and be diluted to scale, shake up, precision is measured 0.7ml, put in the 10ml measuring bottle, add 50% methanol to scale, shake up, promptly get reference substance solution; Drug regimen soft extract with bee honey preparation 10 grams of the present invention are got in the preparation of need testing solution, and accurate the title decides, and adds water 20ml, stirs, and makes dissolving fully, and add chloroform and extract three times, each 20ml, placement is 30 minutes after the jolting, divides and gets chloroform solution; Combined chloroform liquid adds the 20g anhydrous sodium sulfate, jolting 10 minutes, filter, with 20-30ml chloroform washing container and filtering residue, washing liquid is incorporated in the filtrate, evaporate to dryness, filtering residue add 50% dissolve with methanol, move in the 50ml measuring bottle, add 50% methanol to scale, shake up, filter, get subsequent filtrate, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Algoscopy, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; The every 1g of pharmaceutical composition soft extract with bee honey preparation of the present invention contains Ramulus Cinnamomi with cinnamic acid C 9H 8O 2Meter must not be less than 0.020mg.
17. the method for quality control of pharmaceutical composition soft extract with bee honey preparation as claimed in claim 16 is characterized in that this method comprises following discriminating and/or assay:
Differentiate: A, get pharmaceutical composition soft extract with bee honey preparation 30 grams of the present invention, add the 30ml water dissolution, add the 30ml ether gently jolting extract, place layering, divide and get ether solution, put in 40 ℃ of water-baths and fling to ether, residue adds the 2ml dissolve with ethanol, as need testing solution; Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the solution that every 1ml contains 10 μ l, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with 60-90 ℃ of petroleum ether-ethyl acetate ratio be 17: 3 as developing solvent, launch, take out, dry, spray is with the dinitrophenylhydrazine test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
B, get pharmaceutical composition soft extract with bee honey preparation of the present invention 30 grams, add ethanol 60ml, room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill 10 minutes, divides and gets ethanol liquid; Get 20ml ethanol liquid, water-bath is steamed to thick, cooling, and residue adds 2ml ethanol, stirs dipping 10 minutes, leaves standstill, and gets supernatant as need testing solution; Other gets berberine hydrochloride and palmatine hydrochloride reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg respectively, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol-glacial acetic acid-water ratio be 7: 1: 2 as developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the fluorescence speckle of same color;
C, get pharmaceutical composition soft extract with bee honey preparation of the present invention 30 grams, add ethanol 60ml, room temperature dipping 30 minutes constantly stirs and makes dispersion, leaves standstill 10 minutes, divides and gets ethanol liquid; Get 30ml ethanol liquid, water-bath is steamed to 2ml, adds water 20ml, extract three times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, the water 15ml saturated with n-butyl alcohol washs once, discard water liquid, n-butyl alcohol liquid adds active carbon 0.5 gram, stirs evenly, filter, filtrate water bath method, residue add ethanol 1ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 6 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid ratio is 40: 5: 10: 0.2 as developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
Assay: the test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica, acetonitrile-0.1% phosphoric acid solution ratio be 30: 70 as mobile phase, the detection wavelength is 285nm, number of theoretical plate should be not less than 2000 by the calculating of cinnamic acid peak; The preparation of reference substance solution, precision takes by weighing through the cinnamic acid reference substance 10mg of phosphorus pentoxide drying under reduced pressure to constant weight, put in the brown measuring bottle of 100ml, add 50% dissolve with methanol and be diluted to scale, shake up, precision is measured 0.7ml, put in the 10ml measuring bottle, add 50% methanol to scale, shake up, promptly get reference substance solution; Pharmaceutical composition soft extract with bee honey preparation 10 grams of the present invention are got in the preparation of need testing solution, and accurate the title decides, and adds water 20ml, stirs, and makes dissolving fully, and add chloroform and extract three times, each 20ml, placement is 30 minutes after the jolting, divides and gets chloroform solution; Combined chloroform liquid adds the 20g anhydrous sodium sulfate, jolting 10 minutes, filter, with 25ml chloroform washing container and filtering residue, washing liquid is incorporated in the filtrate, evaporate to dryness, filtering residue add 50% dissolve with methanol, move in the 50ml measuring bottle, add 50% methanol to scale, shake up, filter, get subsequent filtrate, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Algoscopy, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; The every 1g of pharmaceutical composition soft extract with bee honey preparation of the present invention contains Ramulus Cinnamomi with cinnamic acid C 9H 8O 2Meter must not be less than 0.020mg.
18. pharmaceutical composition as claimed in claim 9 has treatment acute bronchitis, chronic bronchitis, bronchial asthma or merges application in the medicine of emphysema, pulmonary heart disease in preparation.
19. pharmaceutical composition as claimed in claim 5 preparation have the treatment acute/chronic bronchitis, bronchial asthma and merging emphysema or pulmonary heart disease medicine in application.
20., it is characterized in that wherein said treatment acute/chronic bronchitis, bronchial asthma and merging emphysema thereof, pulmonary heart disease are meant treatment cough, expectoration, pant, reduce leukocyte or pulmonary ventilation function improving as claim 18 or 19 described application.
21. pharmaceutical composition as claimed in claim 9 has relieving cough and resolving phlegm in preparation, the application in the medicine of lowering the adverse-rising QI to subdue asthma effect.
22. application as claimed in claim 21 is characterised in that the wherein said relieving cough and resolving phlegm that has, the lowering the adverse-rising QI to subdue asthma effect is meant treatment because cough, asthma or the accumulation and obstruction of sputum that wind and cold or accumulation of phlegm-damp in the lung cause.
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CN103071142A (en) * 2013-02-26 2013-05-01 栗明峰 Quick-acting external patch for tracheitis
CN105259295A (en) * 2015-11-17 2016-01-20 山东沃华医药科技股份有限公司 Quality detection method for ginseng, cassia twig and poria cocos oral solution
CN105816519A (en) * 2016-05-19 2016-08-03 万云鹏 Pharmaceutical composition for treating emphysema and preparation method thereof
CN106110280A (en) * 2016-08-28 2016-11-16 福州海王金象中药制药有限公司 Guilong kechuangning tablet preparation technology
CN113117039A (en) * 2020-01-13 2021-07-16 广西泰诺制药有限公司 Method for preparing Guilong Kechuanning tablet

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103071142A (en) * 2013-02-26 2013-05-01 栗明峰 Quick-acting external patch for tracheitis
CN105259295A (en) * 2015-11-17 2016-01-20 山东沃华医药科技股份有限公司 Quality detection method for ginseng, cassia twig and poria cocos oral solution
CN105259295B (en) * 2015-11-17 2017-05-17 山东沃华医药科技股份有限公司 Quality detection method for ginseng, cassia twig and poria cocos oral solution
CN105816519A (en) * 2016-05-19 2016-08-03 万云鹏 Pharmaceutical composition for treating emphysema and preparation method thereof
CN106110280A (en) * 2016-08-28 2016-11-16 福州海王金象中药制药有限公司 Guilong kechuangning tablet preparation technology
CN113117039A (en) * 2020-01-13 2021-07-16 广西泰诺制药有限公司 Method for preparing Guilong Kechuanning tablet

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