CN1457869A - Chinese medicine composition for treating oral cavity and throat diseases and its preparing method - Google Patents
Chinese medicine composition for treating oral cavity and throat diseases and its preparing method Download PDFInfo
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- CN1457869A CN1457869A CN 03137148 CN03137148A CN1457869A CN 1457869 A CN1457869 A CN 1457869A CN 03137148 CN03137148 CN 03137148 CN 03137148 A CN03137148 A CN 03137148A CN 1457869 A CN1457869 A CN 1457869A
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Abstract
The Chinese medicine composition for treating oral cavity and throat diseases is prepared with 12 kinds of Chinese medicinal materials including watermelon frost, skullcap root, blackberry lily rhizome, tonkini sophora root, honeysuckle, etc. The preparation process includes distillation, decoction and alcohol of the materials to extract the effective components in the materials fully. The quality control method of component identification and content measurement is also provided. The Chinese medicine composition of the present invention has high functions of resisting acute inflammation, clearing away heat, stopping pain, resisting bacteria, resist virus, eliminating phlegm and strengthening immunity and has no obvious side effect.
Description
Invention field
The present invention relates to a kind of Chinese medicine composition, particularly be used for the treatment of the Chinese medicine composition of oral cavity and throat diseases, relate to preparation method, purposes and the method for quality control of said composition simultaneously.
Background technology
Throat and oral cavity diseases belongs to traditional Chinese medical science categories such as " tonsillitis, sore throat, aphonia due to throat disease ", be subordinate to ability to speak, larynx section, diseases such as the said acute/chronic pharyngitis laryngitis of modern medicine, acute tonsillitis, oral ulcer, stomatitis, gingival swelling and pain, pathogeny Chinese medicine is thought " all diseases of throat all belong to fire ", mainly be body diseases caused by exogenous pathogenic factor pyretic toxicity and cause on the pathogenic fire scorchingly, or cause exopathogen because oral cavity and throat is unclean and invade.Moreover be exactly that plain body loses void, and cause hyperactivity of deficient fire.Modern medicine study thinks that the scorching card of oral cavity and throat disease mainly is an infected by microbes such as antibacterial, virus and causing, or body immunity is low, and antibacterial, virus are in the pathogenic microorganism growth imbalance of oral cavity and throat and cause infection.Also have due to the mechanical damage simultaneously, or excessively take place with throat.This disease can repeatedly take place, and can repeatedly take place.
The tradition Chinese medicine has much the commentary treatise of oral cavity throat disease, has also put down in writing many prescriptions, and as Yangyin Qingfei Tang, BINGPENG SAN etc., these prescriptions are to adopt according to concrete symptom, are the important component parts of Chinese medicine content.Ancient Chinese medicine medicine or Chinese medicine among the people are fully being summed up, excavating or utilized to the modern Chinese medicine theory also.Just introduce the many proved recipes of control oral cavity and throat diseases, typical prescription as Chinese medicine institution of higher learning teaching material " traditional Chinese medical science otolaryngology ", the control oral cavity and throat diseases is had directive function preferably.
According to the needs in market, according to traditional Chinese medicine theory, in conjunction with modern pharmaceutical science and technology, the present invention has released the sick Chinese medicine of a kind of treatment oral cavity and throat, and this curative effect of medication is definite, and is quality controllable, the no obvious toxic-side effects of safety, and cutting agent novelty, it is convenient to use, and dosage is little.
Summary of the invention
One object of the present invention is to disclose a kind of Chinese medicine composition of new treatment oral cavity and throat diseases; Another object of the present invention is the method for the Chinese medicine composition of a kind of new treatment oral cavity and throat diseases of open preparation.The object of the invention also is to disclose a kind of method of quality control of new Chinese medicine composition.
The crude drug of pharmaceutical composition of the present invention is formed and proportioning following (by weight):
Watermelon crystal 20-60 weight portion Radix Scutellariae 75-220 weight portion Rhizoma Belamcandae 75-220 weight portion
Radix Sophorae Tonkinensis 50-150 weight portion Flos Lonicerae 80-240 weight portion Radix Saposhnikoviae 40-120 weight portion
Mentholum 1-4 weight portion Borneolum Syntheticum 1-4 weight portion Borax 10-50 weight portion
Radix Scrophulariae 40-120 weight portion 40-120 Radix Ophiopogonis weight portion Radix Glycyrrhizae 40-120 weight portion.
Above Chinese medicine composition can add adjuvant and make any dosage form on the pharmaceutics meaning, contains spray, tablet, capsule, syrup, granule, drop pill, pill, paster etc., preferred spray.
The present composition can add following adjuvant and make spray:
Steviosin 1-5 weight portion Polysorbate 15-90 parts by volume 95% ethanol 6-25 parts by volume.
The method that the present composition prepares spray is:
The above present composition 12 flavors, Flos Lonicerae, Radix Saposhnikoviae two flavors add the water distillation, collect the about 180-220 parts by volume of distillate, and the aqueous solution after the distillation filters, and device is preserved in addition; 6 flavors such as medicinal residues and Radix Scutellariae, Rhizoma Belamcandae, Radix Sophorae Tonkinensis, Radix Scrophulariae, Radix Ophiopogonis, Radix Glycyrrhizae decoct with water three times, each 0.5-3 hour, collecting decoction filtered, filtrate and above-mentioned aqueous solution merge, being concentrated into 40-90 ℃ of relative density is 1.05-1.40, adds 40-95% ethanol and makes and contain alcohol and reach 40-80%, fully stirs, left standstill 12-36 hour, get supernatant and filter, filtrate recycling ethanol, the clear paste that to be concentrated into 40-90 ℃ of relative density be 1.05-1.40; Mentholum, Borneolum Syntheticum add an amount of 70-95% dissolve with ethanol, after addition polymerization Pyrusussuriensis ester stirs evenly again, slowly add in the above-mentioned distillate, and the limit edged stirs, and adds above-mentioned clear paste again and stirs evenly; Watermelon crystal, Borax add an amount of hot water dissolving, filter; Steviosin adds an amount of hot water dissolving, is chilled to room temperature, adds in the above-mentioned medicinal liquid, adds water to 1000 parts by volume, stirs evenly, and filters, and fill promptly gets spray.
Above institute weight portion/state volume is corresponding with g/ml.
The method of quality control that the present composition is made spray comprises discriminating and/or assay.
Discrimination method comprises a kind of and/or several in the following method:
A. get this product 2ml, add barium chloride test solution 1ml, promptly generate white precipitate; Separate, be deposited in the hydrochloric acid and do not dissolve;
B. get this product 10ml, put in the water-bath and steam to thick, add sulphuric acid 2ml, after the mixing, add methanol 8ml, ignition promptly generates the boundary zone green flame;
C. get this product 10ml, add 20～70 ℃ of petroleum ether 20ml, jolting is extracted gently, leaves standstill, and gets supernatant, volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Borneolum Syntheticum, Mentholum reference substance, adds dehydrated alcohol respectively and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 7-10: 1-2: 1-3 petroleum ether (20～70 ℃)-ethyl acetate-benzene is developing solvent, launch, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. get this product 10ml, add strong ammonia solution 0.3ml, extract 1-3 time with the chloroform jolting, each 10ml, combined chloroform liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, and chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 2 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 9-12: 0.8-1.5: 0.1-0.4 ethyl acetate-methanol-strong ammonia solution is developing solvent, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
E. get this product 30ml, extract 1-3 time with 50～90 ℃ of petroleum ether joltings, each 15ml discards petroleum ether liquid, aqueous solution stirs with 2mol/L hydrochloric acid solution adjust pH to 2, and is centrifugal, filters, taking precipitate, oven dry grinds, and adds chloroform 30ml, hydrochloric acid 3ml, reflux 1-2 hour, put coldly, filter, divide and get chloroform solution, water 10ml washing discards water lotion, and chloroform solution adds anhydrous sodium sulfate and dewaters in right amount, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance adds dehydrated alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution in addition; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 3～5 μ l, reference substance solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 9-12: 18-25: 8-12: 0.3-0.7 petroleum ether (30～60 ℃)-benzene-ethyl acetate-glacial acetic acid is developing solvent, launches, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to speckle colour developing at 105-115 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D), chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 45-55: 45-55: the 0.1-0.4 methanol-water-phosphoric acid is a mobile phase; The detection wavelength is 277nm; Theoretical cam curve is calculated by the baicalin peak should be not less than 3500; The preparation of reference substance solution, precision take by weighing at 50-70 ℃ of vacuum drying 3-5 hour baicalin reference substance an amount of, add methanol and make the solution that every 1ml contains 60 μ g, promptly get reference substance solution; This product 0.5ml is measured in the preparation of need testing solution, precision, puts in the 50ml measuring bottle, adds 45-60% methanol and is diluted to scale, shakes up, and filters, and promptly gets 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, that is and: the every 1ml of this product contains Radix Scutellariae with baicalin (C
21H
18O
11) meter, must not be less than 5.8-6.6mg.
Present composition preparation has good anti-acute inflammation, analgesic, analgesia, antibiotic, antiviral, eliminate the phlegm and raise immunity effect and having no side effect.
The result of following experimental example can further specify the present invention.
Experimental example 1Present composition preparation (white a kind of reed mentioned in ancient books pharynx nebula for treating) pharmacodynamics test
1, by mice ear method, the evidence of mice acetic acid peritonitis method, this product can obviously suppress mice auricle swelling and the mice capillary permeability increases, and illustrates that this product has good antiinflammatory action.
2, this product has significant refrigeration function to heating due to the rat skin lower injection yeast.
3, the mouse writhing method test shows that this product has significant analgesic activity.
4, this product has good anti-golden yellow Portugal fungus ball bacterium, escherichia coli, Cray uncle pneumobacillus, streptococcus pneumoniae, beta hemolysis type streptococcus, alpha streptococcus, and the effect of adenovirus through in vitro tests proof.The mice in vivo test proves to have pharmacological actions such as anti-beta hemolysis type streptococcus, influenza virus.
5, this product has the macrophage phagocytic of enhancing ability to the mice of the immunologic hypofunction of caused by cyclophosphamide, increases immune organ weight such as thymus and spleen, strengthens the effect of humoral immune function.
6, can increase the phenol red bronchus excretion of mice amount, illustrate to have obvious phlegm-dispelling functions.
Experimental example 2The toxicity test acute toxicity test:
1, acute toxicity test: the mice maximum tolerated dose is 120g/kg, is with daily dose 1200 times of clinical plan.
2, skin anaphylactic test: this product does not have sensitivity response to guinea pig skin.
3, mucomembranous pungency test: this product is to oral cavity, throat and tunica mucosa tracheae nonirritant.Long term toxicity test:
Rat is retained animal and continues to observe for two weeks with this product 6g/kg (clinical plan is with 60 times of daily dose) gastric infusion 30 days continuously, there is no the toxicity that outward appearance, body weight gain, hematological indices, hepatic and renal function and organs and tissues appear in animal and changes.Point out this medicine life-time service toxicity little, safety coefficient is big.Retain animal and continue to observe for two weeks, above-mentioned every index toxicity also do not occur and changes.
Result of the test shows that this product is safe with the dosage and the course of treatment in clinical practice by plan.
Experimental example 3Clinical experiment
II clinical trial phase: according to the requirement of national relevant laws and regulations and technology, according to Ministry of Public Health clinical trial method, adopt parallel control, demixing zone group at random, the method for double blinding dual analog, multiple center trial, observe this product and treat wind-heat syndrome of acute pharyngitis clinical efficacy, toxic and side effects and untoward reaction, its effectiveness and safety are made evaluation.200 routine patients are observed in this test altogether, and wherein, test group is 100 examples, and matched group is 100 examples.Two groups of patient's background informations and clinical physical data have comparability (only there were significant differences between the average year age group).Clinical test results shows: the clinical recovery rate of this spray treatment wind-heat syndrome of acute pharyngitis is 52%, and obvious effective rate is 26%, and total effective rate is 78%, and matched group is respectively 51%, 23%, 74%; This product has no side effect substantially, and the heart, liver, renal function, blood system no abnormality seen are changed.
The III clinical trial phase: according to the requirement of national relevant laws and regulations and technology, according to Ministry of Public Health clinical trial method, adopt parallel control, demixing zone group at random, the method for multiple center trial, estimate the effectiveness and the safety of this product treatment wind-heat syndrome of acute pharyngitis.471 routine patients are observed in this test altogether, and wherein, test group is 356 examples, and matched group is 115 examples.Clinical test results shows: test group to pharyngalgia, dry pharynx is scorching hot and pharyngeal mucous membrane, the outstanding bullate improvement of Yong Hong significantly are better than matched group.Positive symptom sign disappearance rate relatively aspect, test group pharyngalgia, dry pharynx are scorching hot, the 6th day disappearance rate of pharyngeal mucous membrane congestion and edema and pharynx rear wall lymph follicle significantly is better than matched group.Primary symptom integration and total mark all significantly descend after two groups of treatments.The drop-out value test group of treatment back primary symptom integration and total mark significantly is better than matched group.Meet scheme collection test group cure rate 42.13%, obvious effective rate 29.78%, total effective rate 71.91%, matched group is respectively 23.48%, 31.30%, and 54.78%.Comprehensive therapeutic effect, cure rate and the total effective rate of test group treatment wind-heat syndrome of acute pharyngitis all significantly are better than matched group; Trial drug is not observed in this test has anomalous effects to the heart, liver, renal function, blood system.
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment 1Spray
Watermelon crystal 30g Radix Scutellariae 100g Rhizoma Belamcandae 80g Radix Sophorae Tonkinensis 100g
Flos Lonicerae 150g Radix Saposhnikoviae 70g Mentholum 2g Borneolum Syntheticum 1.5g
Borax 20g Radix Scrophulariae 85g 69.5g Radix Ophiopogonis Radix Glycyrrhizae 55g
Adjuvant:
Steviosin 3.5g Polysorbate 30ml 95% ethanol 20ml
More than 12 flavors, Flos Lonicerae, Radix Saposhnikoviae two flavors add the water distillation, collect the about 190ml of distillate, the aqueous solution after the distillation filters, device preservation in addition; 6 flavors such as medicinal residues and Radix Scutellariae, Rhizoma Belamcandae, Radix Sophorae Tonkinensis, Radix Scrophulariae, Radix Ophiopogonis, Radix Glycyrrhizae decoct with water three times, each 2 hours, collecting decoction filtered, filtrate and above-mentioned aqueous solution merge, being concentrated into 80 ℃ of relative densities is 1.25, adds 70% ethanol and makes and contain alcohol and reach 78%, fully stirs, left standstill 15 hours, get supernatant and filter, filtrate recycling ethanol is concentrated into 75 ℃ of relative densities and is 1.26 clear paste.Mentholum, Borneolum Syntheticum add an amount of 78% dissolve with ethanol, after addition polymerization Pyrusussuriensis ester 85ml stirs evenly again, slowly add in the above-mentioned distillate, and the limit edged stirs, and adds above-mentioned clear paste again and stirs evenly.Watermelon crystal, Borax add an amount of hot water dissolving, filter; Steviosin adds an amount of hot water dissolving, is chilled to room temperature, adds in the above-mentioned medicinal liquid, adds water to 1000ml, stirs evenly, filter, and fill, promptly.Function is in curing mainly: have heat-clearing and toxic substances removing, dispelling wind reduces phlegm, and the function of detumescence sore-throat relieving is used for exuberant lung-stomach heat, and wind heat is violated the pharyngalgia sore throat due to the table.Usage and dosage: be sprayed on the affected part, press for one time 5,12 times on the one.
Embodiment 2Tablet
Watermelon crystal 40g Radix Scutellariae 200g Rhizoma Belamcandae 180g Radix Sophorae Tonkinensis 130g
Flos Lonicerae 200g Radix Saposhnikoviae 100g Mentholum 3g Borneolum Syntheticum 3g
Borax 40g Radix Scrophulariae 100g 100g Radix Ophiopogonis Radix Glycyrrhizae 100g
More than 12 flavors, Flos Lonicerae, Radix Saposhnikoviae two flavors add the water distillation, collect the about 200ml of distillate, the aqueous solution after the distillation filters, device preservation in addition; 6 flavors such as medicinal residues and Radix Scutellariae, Rhizoma Belamcandae, Radix Sophorae Tonkinensis, Radix Scrophulariae, Radix Ophiopogonis, Radix Glycyrrhizae decoct with water three times, each 2 hours, collecting decoction filtered, filtrate and above-mentioned aqueous solution merge, being concentrated into 70 ℃ of relative densities is 1.20, adds 60% ethanol and makes and contain alcohol and reach 70%, fully stirs, left standstill 26 hours, get supernatant and filter, filtrate recycling ethanol is concentrated into 70 ℃ of relative densities and is 1.20 clear paste.Mentholum, Borneolum Syntheticum add an amount of 80% dissolve with ethanol, after addition polymerization Pyrusussuriensis ester 85ml stirs evenly again, slowly add in the above-mentioned distillate, and the limit edged stirs, and adds above-mentioned clear paste again and stirs evenly.Watermelon crystal, Borax add an amount of hot water dissolving, filter; Make tablet through conventional technology.Function is in curing mainly: have heat-clearing and toxic substances removing, dispelling wind reduces phlegm, and the function of detumescence sore-throat relieving is used for exuberant lung-stomach heat, and wind heat is violated the pharyngalgia sore throat due to the table.Usage and dosage: oral, a 2-5 sheet, 3 times on the one.
Embodiment 3Capsule
Watermelon crystal 30g Radix Scutellariae 150g Rhizoma Belamcandae 130g Radix Sophorae Tonkinensis 80g
Flos Lonicerae 150g Radix Saposhnikoviae 60g Mentholum 3g Borneolum Syntheticum 3g
Borax 30g Radix Scrophulariae 60g 80g Radix Ophiopogonis Radix Glycyrrhizae 80g
More than 12 flavors, Flos Lonicerae, Radix Saposhnikoviae two flavors add the water distillation, collect the about 200ml of distillate, the aqueous solution after the distillation filters, device preservation in addition; 6 flavors such as medicinal residues and Radix Scutellariae, Rhizoma Belamcandae, Radix Sophorae Tonkinensis, Radix Scrophulariae, Radix Ophiopogonis, Radix Glycyrrhizae decoct with water three times, each 2 hours, collecting decoction filtered, filtrate and above-mentioned aqueous solution merge, being concentrated into 70 ℃ of relative densities is 1.20, adds 60% ethanol and makes and contain alcohol and reach 70%, fully stirs, left standstill 26 hours, get supernatant and filter, filtrate recycling ethanol is concentrated into 70 ℃ of relative densities and is 1.20 clear paste.Mentholum, Borneolum Syntheticum add an amount of 80%7 alcohol dissolvings, after addition polymerization Pyrusussuriensis ester 85ml stirs evenly again, slowly add in the above-mentioned distillate, and the limit edged stirs, and adds above-mentioned clear paste again and stirs evenly.Watermelon crystal, Borax add an amount of hot water dissolving, filter; Make capsule through conventional technology.
Embodiment 4The method of quality control of spray of the present invention
Differentiate: A. gets this product 2ml, adds barium chloride test solution 1ml, promptly generates white precipitate; Separate, be deposited in the hydrochloric acid and do not dissolve;
B. get this product 10ml, put in the water-bath and steam to thick, add sulphuric acid 2ml, after the mixing, add methanol 8ml, ignition promptly generates the boundary zone green flame;
C. get this product 10ml, add 30～60 ℃ of petroleum ether 20ml, jolting is extracted gently, leaves standstill, and gets supernatant, volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Borneolum Syntheticum, Mentholum reference substance, adds dehydrated alcohol respectively and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 9: 1: 2 petroleum ether (30～60 ℃)-ethyl acetate-benzene was developing solvent, launch, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. get this product 10ml, add strong ammonia solution 0.3ml, extract 2 times with the chloroform jolting, each 10ml, combined chloroform liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, and chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 2 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 10: 1: 0.2 ethyl acetate-methanol-strong ammonia solutions was developing solvent, launched, and took out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
E. get this product 30ml, extract 2 times with 60～90 ℃ of petroleum ether joltings, each 15ml discards petroleum ether liquid, aqueous solution stirs with 2mol/L hydrochloric acid solution adjust pH to 2, and is centrifugal, filters, taking precipitate, oven dry grinds, and adds chloroform 30ml, hydrochloric acid 3ml, reflux 1 hour is put coldly, filters, divide and get chloroform solution, water 10ml washing discards water lotion, and chloroform solution adds anhydrous sodium sulfate and dewaters in right amount, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance adds dehydrated alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution in addition; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 3～5 μ l, reference substance solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent, with the sodium carboxymethyl cellulose with 10: 20: 10: 0.5 petroleum ether (30～60 ℃)-benzene-ethyl acetate-glacial acetic acid is developing solvent, launches, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D), chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 50: 50: 0.2 methanol-water-phosphoric acid are mobile phase; The detection wavelength is 277nm; Theoretical cam curve is calculated by the baicalin peak should be not less than 3500; The preparation of reference substance solution, precision take by weighing at 4 hours baicalin reference substance of 60 ℃ of vacuum dryings an amount of, add methanol and make the solution that every 1ml contains 60 μ g, promptly get reference substance solution; This product 0.5ml is measured in the preparation of need testing solution, precision, puts in the 50ml measuring bottle, adds 50% methanol and is diluted to scale, shakes up, and filters, and promptly gets 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, that is and: the every 1ml of this product contains Radix Scutellariae with baicalin (C
21H
18O
11) meter, must not be less than 5.8mg.
Claims (14)
1, a kind of Chinese medicine composition for the treatment of oral cavity and throat diseases is characterized in that this Chinese medicine composition made by following raw material medicaments:
Watermelon crystal 20-60 weight portion Radix Scutellariae 75-220 weight portion Rhizoma Belamcandae 75-220 weight portion
Radix Sophorae Tonkinensis 50-150 weight portion Flos Lonicerae 80-240 weight portion Radix Saposhnikoviae 40-120 weight portion
Mentholum 1-4 weight portion Borneolum Syntheticum 1-4 weight portion Borax 10-50 weight portion
Radix Scrophulariae 40-120 weight portion 40-120 Radix Ophiopogonis weight portion Radix Glycyrrhizae 40-120 weight portion.
2, Chinese medicine composition as claimed in claim 1 is characterized in that this Chinese medicine composition made by following raw material medicaments:
Watermelon crystal 50 weight portion Radix Scutellariaes 80 weight portion Rhizoma Belamcandae 100 weight portions
Radix Sophorae Tonkinensis 95 weight portion Flos Loniceraes 120 weight portion Radix Saposhnikoviaes 65.5 weight portions
Mentholum 3.5 weight portion Borneolum Syntheticums 2.5 weight portion Boraxs 25 weight portions
Radix Scrophulariae 85 weight portion 62.5 weight portion Radix Glycyrrhizaes Radix Ophiopogonis 75 weight portions.
3, Chinese medicine composition as claimed in claim 1 or 2 is characterized in that this Chinese medicine composition can add adjuvant and make spray, tablet, capsule, syrup, granule, drop pill, pill, paster, preferred spray.
4, Chinese medicine composition as claimed in claim 3 is characterized in that this Chinese medicine composition can add adjuvant steviosin 1-5 weight portion, Polysorbate 15-90 parts by volume, 95% ethanol 6-25 parts by volume and make spray.
5, Chinese medicine composition as claimed in claim 4 is characterized in that this Chinese medicine composition can add adjuvant steviosin 4 weight portions, Polysorbate 30 parts by volume, 95% ethanol, 12 parts by volume and make spray.
6, as claim 4 or 5 described Chinese medicine composition spray preparing process, it is characterized in that this method is: Flos Lonicerae, Radix Saposhnikoviae two flavors add the water distillation, collect the about 180-220 parts by volume of distillate, and the aqueous solution after the distillation filters, and device is preserved in addition; 6 flavors such as medicinal residues and Radix Scutellariae, Rhizoma Belamcandae, Radix Sophorae Tonkinensis, Radix Scrophulariae, Radix Ophiopogonis, Radix Glycyrrhizae decoct with water three times, each 0.5-3 hour, collecting decoction filtered, filtrate and above-mentioned aqueous solution merge, being concentrated into 40-90 ℃ of relative density is 1.05-1.40, adds 40-95% ethanol and makes and contain alcohol and reach 40-80%, fully stirs, left standstill 12-36 hour, get supernatant and filter, filtrate recycling ethanol, the clear paste that to be concentrated into 40-90 ℃ of relative density be 1.05-1.40; Mentholum, Borneolum Syntheticum add an amount of 70-95% dissolve with ethanol, after addition polymerization Pyrusussuriensis ester stirs evenly again, slowly add in the above-mentioned distillate, and the limit edged stirs, and adds above-mentioned clear paste again and stirs evenly; Watermelon crystal, Borax add an amount of hot water dissolving, filter; Steviosin adds an amount of hot water dissolving, is chilled to room temperature, adds in the above-mentioned medicinal liquid, adds water to 1000 parts by volume, stirs evenly, and filters, and fill promptly gets spray.
7, Chinese medicine composition spray preparing process as claimed in claim 6 is characterized in that this method is: Flos Lonicerae, Radix Saposhnikoviae two flavors add the water distillation, collect about 190 parts by volume of distillate, and the aqueous solution after the distillation filters, and device is preserved in addition; 6 flavors such as medicinal residues and Radix Scutellariae, Rhizoma Belamcandae, Radix Sophorae Tonkinensis, Radix Scrophulariae, Radix Ophiopogonis, Radix Glycyrrhizae decoct with water three times, each 2 hours, collecting decoction filtered, filtrate and above-mentioned aqueous solution merge, being concentrated into 80 ℃ of relative densities is 1.25, adds 70% ethanol and makes and contain alcohol and reach 78%, fully stirs, left standstill 15 hours, get supernatant and filter, filtrate recycling ethanol is concentrated into 75 ℃ of relative densities and is 1.26 clear paste; Mentholum, Borneolum Syntheticum add an amount of 78% dissolve with ethanol, after addition polymerization Pyrusussuriensis ester stirs evenly again, slowly add in the above-mentioned distillate, and the limit edged stirs, and adds above-mentioned clear paste again and stirs evenly; Watermelon crystal, Borax add an amount of hot water dissolving, filter; Steviosin adds an amount of hot water dissolving, is chilled to room temperature, adds in the above-mentioned medicinal liquid, adds water to 1000 parts by volume, stirs evenly, and filters, and fill promptly gets spray.
8, require the method for quality control of the described Chinese medicine composition composition spray of 3-5 as profit, it is characterized in that discrimination method in this method comprises one or more in the following discriminating:
A. get this product 2ml, add barium chloride test solution 1ml, promptly generate white precipitate; Separate, be deposited in the hydrochloric acid and do not dissolve;
B. get this product 10ml, put in the water-bath and steam to thick, add sulphuric acid 2ml, after the mixing, add methanol 8ml, ignition promptly generates the boundary zone green flame;
C. get this product 10ml, add 20～70 ℃ of petroleum ether 20ml, jolting is extracted gently, leaves standstill, and gets supernatant, volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Borneolum Syntheticum, Mentholum reference substance, adds dehydrated alcohol respectively and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 7-10: 1-2: 20～70 ℃-ethyl acetate-benzene of 1-3 petroleum ether is developing solvent, launch, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. get this product 10ml, add strong ammonia solution 0.3ml, extract 1-3 time with the chloroform jolting, each 10ml, combined chloroform liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, and chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 2 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 9-12: 0.8-1.5: 0.1-0.4 ethyl acetate-methanol-strong ammonia solution is developing solvent, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
E. get this product 30ml, extract 1-3 time with 50～90 ℃ of petroleum ether joltings, each 15ml discards petroleum ether liquid, aqueous solution stirs with 2mol/L hydrochloric acid solution adjust pH to 2, and is centrifugal, filters, taking precipitate, oven dry grinds, and adds chloroform 30ml, hydrochloric acid 3ml, reflux 1-2 hour, put coldly, filter, divide and get chloroform solution, water 10ml washing discards water lotion, and chloroform solution adds anhydrous sodium sulfate and dewaters in right amount, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance adds dehydrated alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution in addition; Test according to thin layer chromatography, draw need testing solution 3～5 μ l, reference substance solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 9-12: 18-25: 8-12: 30～60 ℃-benzene-ethyl acetate of 0.3-0.7 petroleum ether-glacial acetic acid is developing solvent, launches, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to speckle colour developing at 105-115 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
9, require the method for quality control of 8 described Chinese medicine composition composition sprays as profit, it is characterized in that discrimination method in this method comprises one or more in the following discriminating:
A. get this product 2ml, add barium chloride test solution 1ml, promptly generate white precipitate; Separate, be deposited in the hydrochloric acid and do not dissolve;
B. get this product 10ml, put in the water-bath and steam to thick, add sulphuric acid 2ml, after the mixing, add methanol 8ml, ignition promptly generates the boundary zone green flame;
C. get this product 10ml, add 30～60 ℃ of petroleum ether 20ml, jolting is extracted gently, leaves standstill, and gets supernatant, volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Borneolum Syntheticum, Mentholum reference substance, adds dehydrated alcohol respectively and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 30～60 ℃-ethyl acetate-benzene of 9: 1: 2 petroleum ether is developing solvent, launch, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. get this product 10ml, add strong ammonia solution 0.3ml, extract 2 times with the chloroform jolting, each 10ml, combined chloroform liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, and chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 2 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 10: 1: 0.2 ethyl acetate-methanol-strong ammonia solutions was developing solvent, launched, and took out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
E. get this product 30ml, extract 2 times with 60～90 ℃ of petroleum ether joltings, each 15ml discards petroleum ether liquid, aqueous solution stirs with 2mol/L hydrochloric acid solution adjust pH to 2, and is centrifugal, filters, taking precipitate, oven dry grinds, and adds chloroform 30ml, hydrochloric acid 3ml, reflux 1 hour is put coldly, filters, divide and get chloroform solution, water 10ml washing discards water lotion, and chloroform solution adds anhydrous sodium sulfate and dewaters in right amount, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance adds dehydrated alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution in addition; Test according to thin layer chromatography, draw need testing solution 3～5 μ l, reference substance solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent, with the sodium carboxymethyl cellulose with 10: 20: 10: 30～60 ℃-benzene-ethyl acetate of 0.5 petroleum ether-glacial acetic acid is developing solvent, launches, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
10, require the method for quality control of the described Chinese medicine composition composition spray of 3-5 as profit, it is characterized in that the content assaying method in this method is: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 45-55: 45-55: the 0.1-0.4 methanol-water-phosphoric acid is a mobile phase; The detection wavelength is 277nm; Theoretical cam curve is calculated by the baicalin peak should be not less than 3500; The preparation of reference substance solution, precision take by weighing at 50-70 ℃ of vacuum drying 3-5 hour baicalin reference substance an amount of, add methanol and make the solution that every 1ml contains 60 μ g, promptly get reference substance solution; This product 0.5ml is measured in the preparation of need testing solution, precision, puts in the 50ml measuring bottle, adds 45-60% methanol and is diluted to scale, shakes up, and filters, and promptly gets 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, that is and: the every 1ml of this product contains Radix Scutellariae in baicalin, must not be less than 5.8-6.6mg.
11, require the method for quality control of 10 described Chinese medicine composition composition sprays as profit, it is characterized in that the content assaying method in this method is: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 50: 50: 0.2 methanol-water-phosphoric acid are mobile phase; The detection wavelength is 277nm; Theoretical cam curve is calculated by the baicalin peak should be not less than 3500; The preparation of reference substance solution, precision take by weighing at 4 hours baicalin reference substance of 60 ℃ of vacuum dryings an amount of, add methanol and make the solution that every 1ml contains 60 μ g, promptly get reference substance solution; This product 0.5ml is measured in the preparation of need testing solution, precision, puts in the 50ml measuring bottle, adds 50% methanol and is diluted to scale, shakes up, and filters, and promptly gets 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, that is and: the every 1ml of this product contains Radix Scutellariae in baicalin, must not be less than 5.8mg.
12, require the method for quality control of the described Chinese medicine composition composition spray of 3-5 as profit, it is characterized in that this method may further comprise the steps:
Differentiate: A. gets this product 2ml, adds barium chloride test solution 1ml, promptly generates white precipitate; Separate, be deposited in the hydrochloric acid and do not dissolve;
B. get this product 10ml, put in the water-bath and steam to thick, add sulphuric acid 2ml, after the mixing, add methanol 8ml, ignition promptly generates the boundary zone green flame;
C. get this product 10ml, add 20～70 ℃ of petroleum ether 20ml, jolting is extracted gently, leaves standstill, and gets supernatant, volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Borneolum Syntheticum, Mentholum reference substance, adds dehydrated alcohol respectively and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 7-10: 1-2: 20～70 ℃-ethyl acetate-benzene of 1-3 petroleum ether is developing solvent, launch, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. get this product 10ml, add strong ammonia solution 0.3ml, extract 1-3 time with the chloroform jolting, each 10ml, combined chloroform liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, and chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 2 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 9-12: 0.8-1.5: 0.1-0.4 ethyl acetate-methanol-strong ammonia solution is developing solvent, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
E. get this product 30ml, extract 1-3 time with 50～90 ℃ of petroleum ether joltings, each 15ml discards petroleum ether liquid, aqueous solution stirs with 2mol/L hydrochloric acid solution adjust pH to 2, and is centrifugal, filters, taking precipitate, oven dry grinds, and adds chloroform 30ml, hydrochloric acid 3ml, reflux 1-2 hour, put coldly, filter, divide and get chloroform solution, water 10ml washing discards water lotion, and chloroform solution adds anhydrous sodium sulfate and dewaters in right amount, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance adds dehydrated alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution in addition; Test according to thin layer chromatography, draw need testing solution 3～5 μ l, reference substance solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 9-12: 18-25: 8-12: 30～60 ℃-benzene-ethyl acetate of 0.3-0.7 petroleum ether-glacial acetic acid is developing solvent, launches, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to speckle colour developing at 105-115 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 45-55: 45-55: the 0.1-0.4 methanol-water-phosphoric acid is a mobile phase; The detection wavelength is 277nm; Theoretical cam curve is calculated by the baicalin peak should be not less than 3500; The preparation of reference substance solution, precision take by weighing at 50-70 ℃ of vacuum drying 3-5 hour baicalin reference substance an amount of, add methanol and make the solution that every 1ml contains 60 μ g, promptly get reference substance solution; This product 0.5ml is measured in the preparation of need testing solution, precision, puts in the 50ml measuring bottle, adds 45-60% methanol and is diluted to scale, shakes up, and filters, and promptly gets 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, that is and: the every 1ml of this product contains Radix Scutellariae in baicalin, must not be less than 5.8-6.6mg.
13, require the method for quality control of 12 described Chinese medicine composition composition sprays as profit, it is characterized in that this method may further comprise the steps:
Differentiate: A. gets this product 2ml, adds barium chloride test solution 1ml, promptly generates white precipitate; Separate, be deposited in the hydrochloric acid and do not dissolve;
B. get this product 10ml, put in the water-bath and steam to thick, add sulphuric acid 2ml, after the mixing, add methanol 8ml, ignition promptly generates the boundary zone green flame;
C. get this product 10ml, add 30～60 ℃ of petroleum ether 20ml, jolting is extracted gently, leaves standstill, and gets supernatant, volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Borneolum Syntheticum, Mentholum reference substance, adds dehydrated alcohol respectively and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 30～60 ℃-ethyl acetate-benzene of 9: 1: 2 petroleum ether is developing solvent, launch, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. get this product 10ml, add strong ammonia solution 0.3ml, extract 2 times with the chloroform jolting, each 10ml, combined chloroform liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, and chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 2 μ 1, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 10: 1: 0.2 ethyl acetate-methanol-strong ammonia solutions was developing solvent, launched, and took out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
E. get this product 30ml, extract 2 times with 60～90 ℃ of petroleum ether joltings, each 15ml discards petroleum ether liquid, aqueous solution stirs with 2mol/L hydrochloric acid solution adjust pH to 2, and is centrifugal, filters, taking precipitate, oven dry grinds, and adds chloroform 30ml, hydrochloric acid 3ml, reflux 1 hour is put coldly, filters, divide and get chloroform solution, water 10ml washing discards water lotion, and chloroform solution adds anhydrous sodium sulfate and dewaters in right amount, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance adds dehydrated alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution in addition; Test according to thin layer chromatography, draw need testing solution 3～5 μ l, reference substance solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent, with the sodium carboxymethyl cellulose with 10: 20: 10: 30～60 ℃-benzene-ethyl acetate of 0.5 petroleum ether-glacial acetic acid is developing solvent, launches, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear to be heated to speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 50: 50: 0.2 methanol-water-phosphoric acid are mobile phase; The detection wavelength is 277nm; Theoretical cam curve is calculated by the baicalin peak should be not less than 3500; The preparation of reference substance solution, precision take by weighing at 4 hours baicalin reference substance of 60 ℃ of vacuum dryings an amount of, add methanol and make the solution that every 1ml contains 60 μ g, promptly get reference substance solution; This product 0.5ml is measured in the preparation of need testing solution, precision, puts in the 50ml measuring bottle, adds 50% methanol and is diluted to scale, shakes up, and filters, and promptly gets 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, that is and: the every 1ml of this product contains Radix Scutellariae in baicalin, must not be less than 5.8mg.
14, the application of Chinese medicine composition as claimed in claim 1 or 2 in preparation treatment oral cavity and throat wind-heat syndrome medicine.
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| CN 03137148 CN1233378C (en) | 2003-06-05 | 2003-06-05 | Chinese medicine composition for treating oral cavity and throat diseases and its preparing method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299748C (en) * | 2004-10-13 | 2007-02-14 | 谭玉杰 | Fat reducing regulating Qi supplement bag |
| CN101396488B (en) * | 2008-10-29 | 2011-06-01 | 宗希阳 | Medicine for treating chronic faucitis |
| CN101332269B (en) * | 2008-07-10 | 2011-09-07 | 江汉大学 | Traditional Chinese medicine propellant for treating pharyngitis and preparation method thereof |
| CN102038747B (en) * | 2009-10-16 | 2012-03-07 | 刘新义 | Compound electuary for treating faucitis |
| CN105288305A (en) * | 2015-11-30 | 2016-02-03 | 延欣虹 | Pharmaceutical composition for curing oral excessive inflammation and gingival pain and swelling and preparation method of pharmaceutical composition |
| CN107536947A (en) * | 2016-06-28 | 2018-01-05 | 桂林三金药业股份有限公司 | A kind of application of Chinese medicine composition in the medicine for preparing prevention and/or treatment hand-foot-and-mouth disease |
| CN110354247A (en) * | 2019-08-12 | 2019-10-22 | 马晟利 | A kind of streptocin compound preparation and preparation method thereof for treating thrush |
| CN110927321A (en) * | 2019-11-06 | 2020-03-27 | 桂林三金药业股份有限公司 | Quality detection method of throat soothing spray |
| CN111289630A (en) * | 2018-12-07 | 2020-06-16 | 桂林三金药业股份有限公司 | Method for measuring content of menthol in traditional Chinese medicine composition by gas chromatography |
-
2003
- 2003-06-05 CN CN 03137148 patent/CN1233378C/en not_active Expired - Lifetime
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299748C (en) * | 2004-10-13 | 2007-02-14 | 谭玉杰 | Fat reducing regulating Qi supplement bag |
| CN101332269B (en) * | 2008-07-10 | 2011-09-07 | 江汉大学 | Traditional Chinese medicine propellant for treating pharyngitis and preparation method thereof |
| CN101396488B (en) * | 2008-10-29 | 2011-06-01 | 宗希阳 | Medicine for treating chronic faucitis |
| CN102038747B (en) * | 2009-10-16 | 2012-03-07 | 刘新义 | Compound electuary for treating faucitis |
| CN105288305A (en) * | 2015-11-30 | 2016-02-03 | 延欣虹 | Pharmaceutical composition for curing oral excessive inflammation and gingival pain and swelling and preparation method of pharmaceutical composition |
| CN107536947A (en) * | 2016-06-28 | 2018-01-05 | 桂林三金药业股份有限公司 | A kind of application of Chinese medicine composition in the medicine for preparing prevention and/or treatment hand-foot-and-mouth disease |
| CN107536947B (en) * | 2016-06-28 | 2021-02-02 | 桂林三金药业股份有限公司 | Application of traditional Chinese medicine composition in preparation of medicine for preventing and/or treating hand-foot-and-mouth disease |
| CN111289630A (en) * | 2018-12-07 | 2020-06-16 | 桂林三金药业股份有限公司 | Method for measuring content of menthol in traditional Chinese medicine composition by gas chromatography |
| CN110354247A (en) * | 2019-08-12 | 2019-10-22 | 马晟利 | A kind of streptocin compound preparation and preparation method thereof for treating thrush |
| CN110927321A (en) * | 2019-11-06 | 2020-03-27 | 桂林三金药业股份有限公司 | Quality detection method of throat soothing spray |
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| Publication number | Publication date |
|---|---|
| CN1233378C (en) | 2005-12-28 |
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