CN101028348A - Chinese medicinal capsule, its production and quality controlling method - Google Patents
Chinese medicinal capsule, its production and quality controlling method Download PDFInfo
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- CN101028348A CN101028348A CN 200710098387 CN200710098387A CN101028348A CN 101028348 A CN101028348 A CN 101028348A CN 200710098387 CN200710098387 CN 200710098387 CN 200710098387 A CN200710098387 A CN 200710098387A CN 101028348 A CN101028348 A CN 101028348A
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Abstract
A Chinese medicine in the form of capsule for treating fever, swollen and painful throat, toothache, dizziness, constipation, etc is prepared from isatis leaf, rhubarb, gypsum and menthol. Its preparing process and quality control method are also disclosed.
Description
[technical field]
The invention belongs to technical field of Chinese medicines, be specifically related to a kind of Chinese medicinal capsule and preparation method thereof and method of quality control.
[background technology]
Radix Et Rhizoma Rhei is crucial simply Chinese medicine, also is the good medicine that Tibetan medicine, Mongolian medicine use always simultaneously.Radix Et Rhizoma Rhei nature and flavor bitter cold, the property of medicine is high strong, have the title of " general ".Radix Et Rhizoma Rhei contains glycoside and the tannic acid and the related substances thereof of two kinds of opposite composition-anthraquinone derivatives.The former can stimulate enterokinesia and cause rushing down down, and the latter has astriction and energy antidiarrheal.It rushes down performance down giving birth to having under, a large amount of, the short situation of frying in shallow oil, but system with, in a small amount, under the situation of frying in shallow oil for a long time, rush down down that performance weakens, the antidiarrheal performance appears simultaneously.According to pharmacological evaluation, Radix Et Rhizoma Rhei has the effect of heat-clearing and toxic substances removing, anti-inflammation, purging fire and cooling blood, promoting the function of the gallbladder to alleviate jaundice, clots absorbing removing mass, blood pressure lowering hemostasis.
Emodin and chrysophanol all are the chemical compounds that Radix Et Rhizoma Rhei contains.Emodin (Emodin, molecular formula C wherein
15H
10O
5) be the antibacterial that derives from plant.Emodin can suppress the biosynthesis of bacterial nucleic acid and respiratory and have antibacterial activity.Its mechanism of action mainly is the oxidation and the dehydrogenation of antibacterial sugar and carbohydrate metabolism intermediate product, suppresses assimilation and amino acid whose oxidation, dehydrogenation and the deamination of ammonia nitrogen, Profilin matter and nucleic acid synthetic.To breathing, nucleic acid and proteinic synthesize of staphylococcus aureus in culture medium having the obvious suppression effect, emodin is difficult for developing immunity to drugs, also very sensitive to streptococcus.Secondly to diphtheria, hay, charcoal and bacillus, and pay typhoid fever and dysentery bacterium also effective.Chrysophanol has antibacterial activity; Can shorten blood coagulation time, excitor nerve, paralysis muscle; And have cough-relieving, diuresis and an antitumaous effect.
Gypsum Fibrosum: clearing away lung-heat, rush down stomach-fire, relieving restlessness is quenched the thirst: be used for hyperpyrexia, thirsty, irritated, the headache that lung-heat cough with asthma and stomach-fire cause, toothache.
The central high fever that a variety of causes causes, clinical manifestation are that body temperature continues more than 39 ℃, and body surface is lossless, relative infrequent pulse can occur, or the routine blood test leukocyte is normal, the Applied Physics cooling, and it is invalid mostly to reach the general solution medicine of a warm nature and glucocorticoids medicine.At this moment use heavy dose of Gypsum Fibrosum, Radix Et Rhizoma Rhei, the heat-clearing and toxic substances removing removing heat by catharsis expells the pathogenic heat not only can effectively be brought down a fever, and can reduce complication, improves patient's life quality.
Mentholum is colourless needle-like or prism-shaped crystallization or white crystalline powder; Herba Menthae fragrance is arranged, and the just scorching hot back of flavor is refrigerant, volatile, and it is neutral that alcoholic solution is.At ethanol, chloroform, ether, very easily dissolving in liquid Paraffin or the volatile oil, dissolving is atomic in water.Mentholum and glucuronic acid form conjugate and discharge in urine and bile, and various isomers do not combine with glucuronic acid with commensurability.In Canis familiaris L. and rat body, produce the molecular degradation reaction.It can the menthone metabolite form exist.The Herba Menthae brain-capacity optionally stimulates the Cold receptor of human body skin or mucosa, produces sense of cold reflection and creeping chill, causes the skin mucosa vasoconstriction, also can cause the blood vessel of deep tissue and shrink and produce therapeutical effect.External can antiinflammatory, pain relieving, and antipruritic, blood circulation promoting alleviates edema etc.; For oral administration can alleviate local inflammation in the compound preparation: pharyngolaryngitis and treatment flu, and have and be good for the stomach the wind dispelling effect.External is used for local analgesia, and is antipruritic, and headache is dizzy, mosquito bite; Collunarium is used for the cold nasal obstruction, sucks or spray to be used for pharyngolaryngitis; Oral can being good for the stomach.
[summary of the invention]
The object of the present invention is to provide a kind of Chinese medicinal capsule.
Another object of the present invention is to provide the preparation method of Chinese medicinal capsule.
Another object of the present invention is to provide the method for quality control of Chinese medicinal capsule.
Specifically, Chinese medicinal capsule of the present invention is made by pharmaceutically available adjuvant and following medicine: Folium Isatidis 400-1000 weight portion, Radix Et Rhizoma Rhei 100-300 weight portion, Gypsum Fibrosum 50-150 weight portion, Mentholum 0.5-3 weight portion.
Preferred Chinese medicinal capsule of the present invention is made by pharmaceutically available adjuvant and following medicine: Folium Isatidis 500-1000 weight portion, Radix Et Rhizoma Rhei 100-200 weight portion, Gypsum Fibrosum 50-100 weight portion, Mentholum 0.5-1.5 weight portion.
Preferred Chinese medicinal capsule of the present invention is made by pharmaceutically available adjuvant and following medicine: Folium Isatidis 800 weight portions, Radix Et Rhizoma Rhei 200 weight portions, Gypsum Fibrosum 100 weight portions, Mentholum 1.3 weight portions.
Preferred Chinese medicinal capsule of the present invention is made by pharmaceutically available adjuvant and following medicine: made by pharmaceutically available adjuvant and following medicine: Folium Isatidis 600 weight portions, Radix Et Rhizoma Rhei 200 weight portions, Gypsum Fibrosum 100 weight portions, Mentholum 1.0 weight portions.
The preparation method of above-mentioned Chinese medicinal capsule also can for: described Radix Et Rhizoma Rhei, Gypsum Fibrosum powder are broken into fine powder, sieve.Folium Isatidis decocts with water 2 times, 1-3 hour for the first time, adds water 8-12 doubly, 0.5-1.5 hour for the second time, add water 6-10 doubly, merging filtrate, filter, filtrate is concentrated into the clear paste that relative density is about 1.15-1.55, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying gets mixed powder, with the Mentholum dissolve with ethanol, spray adds in the mixed powder, the fill capsule, promptly.
The method of quality control of above-mentioned Chinese medicinal capsule is: when high performance liquid chromatography detects with emodin as detection material.
The method of quality control of above-mentioned Chinese medicinal capsule is: when high performance liquid chromatography detects with chrysophanol as detection material.
The method of quality control of above-mentioned Chinese medicinal capsule is: the mobile phase when high performance liquid chromatography detects is: methanol-0.1 mol phosphoric acid solution (85: 15); Flow velocity is: 1 ml/min, the detection wavelength is 254nm.
The preparation method of above-mentioned Chinese medicinal capsule is preferably: Radix Et Rhizoma Rhei, Gypsum Fibrosum powder are broken into fine powder, sieve.Folium Isatidis decocts with water 2 times, 2 hours for the first time, adds 10 times in water, 1 hour for the second time, add 8 times in water, merging filtrate, filter, filtrate is concentrated into relative density and is about 1.25 clear paste, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying gets mixed powder, with the Mentholum dissolve with ethanol, spray adds in the mixed powder, the fill capsule, promptly.。
The method of quality control of above-mentioned Chinese medicinal capsule is: get content 0.5 gram of Chinese medicinal capsule of the present invention, add 10 milliliters of methanol, supersound process 20 minutes, filter, filtrate evaporate to dryness, residue add water makes dissolving for 10 milliliters, add 1 milliliter of hydrochloric acid again, put in the water-bath and heated 30 minutes, cooling is immediately extracted 2 times with the chloroform jolting, each 10 milliliters, merge chloroform liquid, be concentrated into about 1 milliliter, as need testing solution.Other gets Radix Et Rhizoma Rhei control medicinal material 0.2 gram, shines medical material solution in pairs with legal system.Get the emodin reference substance again, add chloroform and make per 1 milliliter of solution that contains 0.5 milligram, product solution in contrast.Test according to thin layer chromatography (appendix VI B), draw above-mentioned each 3-5 microlitre of three kinds of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with petroleum ether (60-90 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Put in the ammonia steam smoked after, inspect under the daylight, speckle becomes redness.
The method of quality control of above-mentioned Chinese medicinal capsule also can for: get content 1 gram of Chinese medicinal capsule of the present invention, add 5 milliliters of petroleum ether (60-90 ℃), close plug, jolting number minute was placed 30 minutes, filtration, filtrate is as need testing solution.Other gets the Mentholum reference substance, adds petroleum ether and makes per 1 milliliter of solution that contains 0.5 milligram, product solution in contrast.Test according to thin layer chromatography (appendix VI B), draw above-mentioned each 5-10 microlitre of two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-ethyl acetate (10: 0.5) is developing solvent, launch, take out, dry, spray is with the anisaldehyde test solution, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
The method of quality control of above-mentioned Chinese medicinal capsule also can be content 1 gram of getting Chinese medicinal capsule of the present invention, add 10 milliliters of chloroform, reflux 30 minutes filters, the filtrate evaporate to dryness, residue adds 1% sodium hydroxide makes dissolving for 10 milliliters, extracts 2 times each 10 milliliters with the chloroform jolting, merge chloroform liquid, evaporate to dryness, residue add chloroform makes dissolving for 1 milliliter, as need testing solution.Other gets the indirubin reference substance, adds chloroform and makes per 1 milliliter of solution that contains 1 milligram, product solution in contrast.According to thin layer chromatography (appendix VI B) test, draw need testing solution 10 microlitres, reference substance solution 5 microlitres, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-chloroform-acetone (5: 4: 1) is developing solvent, launch, take out, dry.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical light violet magenta speckle.
[specific embodiment]
Embodiment 1
[prescription] Folium Isatidis 800 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1.3 grams
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis decocts with water 2 times, and 2 hours for the first time, add 10 times in water, 1 hour for the second time, add 8 times in water, merging filtrate filters, and filtrate is concentrated into the clear paste that relative density is about 1.25 (60 ℃), adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying is pulverized; With the Mentholum dissolve with ethanol, spray adds in the extract powder, mixing, and granulation, fill incapsulate, and make 1000, promptly.
Embodiment 2
[prescription] Folium Isatidis 800 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1.3 grams
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis decocts with water 2 times, and 2 hours for the first time, add 10 times in water, 1 hour for the second time, add 8 times in water, merging filtrate filters, and filtrate is concentrated into the clear paste that relative density is about 1.25 (60 ℃), adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying is pulverized; With the Mentholum dissolve with ethanol, spray adds in the extract powder, mixing, and granulation, fill incapsulate, and make 1000, promptly.
Embodiment 3
[prescription] Folium Isatidis 800 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1.3 grams
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis decocts with water 2 times, and each water yield is 12/10 times of medical material amount, extracts respectively 3/1.5 hour, and merge extractive liquid, promptly gets the capsular extracting solution of the present invention.The capsular extracting solution of the invention described above is filtered, and filtrate is by macroporous resin, with 20% ethanol elution, collects eluent earlier, and decompression recycling ethanol is not to there being the alcohol flavor, extracting solution, spray drying gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying, pulverizing; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Embodiment 4
[prescription] Folium Isatidis 800 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1.3 grams
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis adds water supersound extraction (ultrasonic power is 500W) 2 times, and each water yield is 8/6 times of medical material amount, extracts respectively 1/0.5 hour.Merge extractive liquid, reclaims ethanol to there not being the alcohol flavor, promptly gets the capsular extracting solution of the present invention.Extracting solution is by macroporous resin, with 20% ethanol elution, collects eluent earlier, and decompression recycling ethanol is not to there being the alcohol flavor, and spray drying gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying, pulverizing; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Embodiment 5
[prescription] Folium Isatidis 800 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 1 00 gram Mentholums 1.3 grams
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis extracting in water 2 times, each water yield is 8/6 times of medical material amount, extracts respectively 2/1 hour, merge extractive liquid, promptly gets the capsular extracting solution of the present invention.The capsular extracting solution of the invention described above is filtered, and filtrate discards with 5 times of water gaging eluents earlier by macroporous resin, and reuse adds 5 times of eluting of 65% ethanol, the collection eluent, and decompression recycling ethanol gets extracting solution to there not being the alcohol flavor.Spray drying adopts membrane separation technique further refining, and the model made from extra care used film is FLT-YL, gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, and drying is pulverized; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Embodiment 6
[prescription] Folium Isatidis 800 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1.3 grams
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis extracting in water 2 times, each water yield is 8/6 times of medical material amount, extracts respectively 2/1 hour, merge extractive liquid, promptly gets the capsular extracting solution of the present invention.The capsular extracting solution of the invention described above is filtered, and filtrate is by macroporous resin, with 20% ethanol elution, collects eluent earlier, and decompression recycling ethanol is not to there being the alcohol flavor, extracting solution, spray drying gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying, pulverizing; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Embodiment 7
[prescription] Folium Isatidis 800 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1.3 grams
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis extracting in water (ultrasonic power is 500W) 2 times, each water yield is 8/6 times of medical material amount, the water yield is 8 times of medical material amount.Merge extractive liquid, reclaims ethanol to there not being the alcohol flavor, promptly gets the capsular extracting solution of the present invention.Extracting solution is by macroporous resin, with 20% ethanol elution, collects eluent earlier, and decompression recycling ethanol is not to there being the alcohol flavor, and spray drying gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying, pulverizing; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Embodiment 8
[prescription] Folium Isatidis 800 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1.3 grams
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis extracting in water 2 times, each water yield is 8/6 times of medical material amount, extracts respectively 2/1 hour, merge extractive liquid, promptly gets the capsular extracting solution of the present invention.The capsular extracting solution of the invention described above is filtered, and filtrate discards with 5 times of water gaging eluents earlier by macroporous resin, and reuse adds 5 times of eluting of 65% ethanol, the collection eluent, and decompression recycling ethanol gets extracting solution to there not being the alcohol flavor.Spray drying adopts membrane separation technique further refining, and the model made from extra care used film is FLT-YL, gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, and drying is pulverized; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Embodiment 9
[prescription] Folium Isatidis 1000 gram Radix Et Rhizoma Rhei 300 gram Gypsum Fibrosum 150 gram Mentholums 3 grams
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis decocts with water 2 times, and 2 hours for the first time, add 10 times in water, 1 hour for the second time, add 8 times in water, merging filtrate filters, and filtrate is concentrated into the clear paste that relative density is about 1.25 (60 ℃), adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying is pulverized; With the Mentholum dissolve with ethanol, spray adds in the extract powder, mixing, and granulation, fill incapsulate, and make 1500, promptly.
Embodiment 10
[prescription] Folium Isatidis 400 gram Radix Et Rhizoma Rhei 100 gram Gypsum Fibrosum 50 gram Mentholums 0.5 gram
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis decocts with water 2 times, and 2 hours for the first time, add 10 times in water, 1 hour for the second time, add 8 times in water, merging filtrate filters, and filtrate is concentrated into the clear paste that relative density is about 1.25 (60 ℃), adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying is pulverized; With the Mentholum dissolve with ethanol, spray adds in the extract powder, mixing, and granulation, fill incapsulate, and make 500, promptly.
Embodiment 11
[prescription] Folium Isatidis 1000 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1.5 grams
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis decocts with water 2 times, and each water yield is 12/10 times of medical material amount, extracts respectively 3/1.5 hour, and merge extractive liquid, promptly gets the capsular extracting solution of the present invention.The capsular extracting solution of the invention described above is filtered, and filtrate is by macroporous resin, with 20% ethanol elution, collects eluent earlier, and decompression recycling ethanol is not to there being the alcohol flavor, extracting solution, spray drying gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying, pulverizing; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 800 of capsules.
Embodiment 12
[prescription] Folium Isatidis 500 gram Radix Et Rhizoma Rhei 100 gram Gypsum Fibrosum 50 gram Mentholums 0.5 gram
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis adds water supersound extraction (ultrasonic power is 500W) 2 times, and each water yield is 8/6 times of medical material amount, extracts respectively 1/0.5 hour.Merge extractive liquid, reclaims ethanol to there not being the alcohol flavor, promptly gets the capsular extracting solution of the present invention.Extracting solution is by macroporous resin, with 20% ethanol elution, collects eluent earlier, and decompression recycling ethanol is not to there being the alcohol flavor, and spray drying gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying, pulverizing; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Embodiment 13
[prescription] Folium Isatidis 600 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1 gram
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis extracting in water 2 times, each water yield is 8/6 times of medical material amount, extracts respectively 2/1 hour, merge extractive liquid, promptly gets the capsular extracting solution of the present invention.The capsular extracting solution of the invention described above is filtered, and filtrate discards with 5 times of water gaging eluents earlier by macroporous resin, and reuse adds 5 times of eluting of 65% ethanol, the collection eluent, and decompression recycling ethanol gets extracting solution to there not being the alcohol flavor.Spray drying adopts membrane separation technique further refining, and the model made from extra care used film is FLT-YL, gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, and drying is pulverized; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Embodiment 14
[prescription] Folium Isatidis 600 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1 gram
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis extracting in water 2 times, each water yield is 8/6 times of medical material amount, extracts respectively 2/1 hour, merge extractive liquid, promptly gets the capsular extracting solution of the present invention.The capsular extracting solution of the invention described above is filtered, and filtrate is by macroporous resin, with 20% ethanol elution, collects eluent earlier, and decompression recycling ethanol is not to there being the alcohol flavor, extracting solution, spray drying gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying, pulverizing; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Embodiment 15
[prescription] Folium Isatidis 600 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1 gram
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis extracting in water (ultrasonic power is 500W) 2 times, each water yield is 8/6 times of medical material amount, the water yield is 8 times of medical material amount.Merge extractive liquid, reclaims ethanol to there not being the alcohol flavor, promptly gets the capsular extracting solution of the present invention.Extracting solution is by macroporous resin, with 20% ethanol elution, collects eluent earlier, and decompression recycling ethanol is not to there being the alcohol flavor, and spray drying gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying, pulverizing; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Embodiment 16
[prescription] Folium Isatidis 600 gram Radix Et Rhizoma Rhei 200 gram Gypsum Fibrosum 100 gram Mentholums 1 gram
[method for making] above four Chinese medicine material is got Radix Et Rhizoma Rhei earlier, Gypsum Fibrosum powder is broken into fine powder, sieves.Folium Isatidis extracting in water 2 times, each water yield is 8/6 times of medical material amount, extracts respectively 2/1 hour, merge extractive liquid, promptly gets the capsular extracting solution of the present invention.The capsular extracting solution of the invention described above is filtered, and filtrate discards with 5 times of water gaging eluents earlier by macroporous resin, and reuse adds 5 times of eluting of 65% ethanol, the collection eluent, and decompression recycling ethanol gets extracting solution to there not being the alcohol flavor.Spray drying adopts membrane separation technique further refining, and the model made from extra care used film is FLT-YL, gets extract powder, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, and drying is pulverized; With the Mentholum dissolve with ethanol, spray adds in the extract powder, and mixing is granulated, and fill gets 1000 of capsules.
Experimental example 1-method of quality control of the present invention
Chinese medicinal capsule of the present invention is made up of Folium Isatidis, Radix Et Rhizoma Rhei, Gypsum Fibrosum and Mentholum.Folium Isatidis index composition is liposoluble constituent-indirubin and indigo, extracts because Folium Isatidis is a decocting, so be difficult for measuring liposoluble constituent indirubin and indigo; It is anthraquinone analog compounds such as emodin and chrysophanol that Radix Et Rhizoma Rhei cures mainly relevant main effective ingredient with this product function, and the total amount of emodin and chrysophanol is as quality control standard among mensuration the present invention, and the row method of going forward side by side is learned research.Relevant research contents is as follows:
1, instrument and reagent
High performance liquid chromatograph comprises Waters 1525 pumps, 2487 dual pathways UV-detector, Waters column oven, Breeze liquid chromatograph work station, Brasson ultrasonic cleaning instrument.Emodin and chrysophanol: the assay reference substance, available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number: emodin: 0756-200110; Chrysophanol: 0796-200005.Methanol is U.S. Tedia chromatographically pure, and water is ultra-pure water, and other reagent is analytical pure.
2, chromatographic condition
Chromatographic column: Phenomenex Luna C18 (2), 4.6mm * 150mm, 5 μ m; Column temperature: 35 ℃; Mobile phase: methanol-0.1 mol phosphoric acid solution (85: 15); Flow velocity: 1 ml/min, the detection wavelength is 254nm.Theoretical cam curve is calculated by the emodin peak should be not less than 3000.
3, the preparation of reference substance solution
Precision takes by weighing 5.01 milligrams of emodin reference substances, 5.25 milligrams of chrysophanol reference substances, puts respectively in 50 milliliters of measuring bottles, with dissolve with methanol and be diluted to scale, shakes up; Precision is measured 1 milliliter of emodin solution, 2 milliliters of chrysophanol solution respectively, puts in 25 milliliters of measuring bottles, adds methanol to scale, shakes up, promptly.(per 1 milliliter contains emodin 4.008 micrograms, chrysophanol 8.4 micrograms)
4, the preparation of need testing solution
Get 5 of the capsules of the embodiment 1 under the content uniformity item, inclining content, porphyrize, get the about 0.25g of powder, the accurate title, decide, and puts in 50 milliliters of tool plug conical flasks, precision adds 25 milliliters of methanol, claims to decide weight, reflux 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured 5 milliliters of subsequent filtrates, put in 50 milliliters of round-bottomed flasks, fling to methanol, add 10 milliliters of 2.5 mol sulfuric acid solutions, supersound process 5 minutes adds 10 milliliters of chloroform again, reflux 1 hour, cooling is in the dislocation separatory funnel, with a small amount of chloroform washing container, incorporate in the separatory funnel, divide and get the chloroform layer, acid solution chloroform extraction 3 times, each 10 milliliters, merge chloroform liquid, decompression and solvent recovery is to doing, and residue adds methanol makes dissolving, be transferred in 10 milliliters of measuring bottles, add methanol to scale, shake up, filter, get subsequent filtrate, promptly.
5, linear relationship is investigated
Accurate reference substance solution (emodin 4.008 mcg/ml, chrysophanol 8.4 mcg/ml) 4.0,6.0,8.0,10.0,12.0 microlitres of drawing, injecting chromatograph of liquid, is abscissa with the sample size, and peak area is a vertical coordinate, set up working curve, the results are shown in Table 1.
The standard curve of table 1 emodin and chrysophanol
| Emodin | Chrysophanol | ||
| Sample size (microgram) | Peak area | Sample size (microgram) | Peak area |
| 0.016032 0.024048 0.032064 0.040080 0.048096 | 61854 92199 124111 154501 184989 | 0.0336 0.0504 0.0672 0.0840 0.1008 | 181698 268449 360645 448567 537829 |
| a＝102，b＝3849451，r＝0.9999 | a＝2485，b＝5311785，r＝0.9999 | ||
| Regression equation: Y=3849451X+102 | Y-5311785X+2485 | ||
| The range of linearity: 0.016032-0.048096 microgram | 0.0336-0.1008 microgram | ||
The result shows that emodin and chrysophanol have good linear relationship in the range of linearity of table 6.
6, the interferential investigation of negative test sample
The preparation method that need testing solution is pressed in the preparation of negative need testing solution takes by weighing the Chinese medicinal capsule sample of the present invention that lacks Radix Et Rhizoma Rhei, makes negative need testing solution (lacking Radix Et Rhizoma Rhei).
Draw each 5 microlitre of reference substance solution, need testing solution and negative need testing solution respectively, inject chromatograph of liquid, conclusion: emodin and chrysophanol reach baseline separation in the need testing solution, and negative need testing solution is noiseless, baseline stability, and method is feasible.
7, stability test
Accurate need testing solution 5 microlitres of drawing are measured once at regular intervals, and totally 5 times, the peak area of mensuration emodin and chrysophanol, RSD is respectively 0.44%, 0.76%, shows that test sample measurement result in 24 hours is stable, the results are shown in Table 2.
Table 2 stability test
| Sample injection time (hour) | 0 hour | 1 hour | 2 hours | 4 hours | 24 hours |
| The emodin peak area | 91208 | 91933 | 91644 | 90885 | 91464 |
| The chrysophanol peak area | 357876 | 360068 | 357159 | 352594 | 357285 |
8, precision test
Accurate need testing solution 5 microlitres of drawing inject chromatograph of liquid, measure the peak area of emodin and chrysophanol, repeat 5 times, the results are shown in Table 3.
The test of table 3 precision
| Measure number of times | 1 | 2 | 3 | 4 | 5 | RSD％ |
| The emodin peak area | 91208 | 91235 | 91836 | 92282 | 91933 | 0.51％ |
| The chrysophanol peak area | 357876 | 358394 | 36077 3 | 362303 | 360068 | 0.50％ |
9, repeatability experiment
According to the operation down of assay item, same batch sample (lot number: embodiment 1) is repeatedly measured, calculate relative standard deviation, the results are shown in Table 4.
The test of table 4 repeatability
| Measure number of times | Emodin content (%) | Chrysophanol content (%) | Emodin and chrysophanol total amount (%) |
| 1 2 3 4 | 0.097 0.097 0.100 0.098 | 0.274 0.271 0.280 0.276 | 0.371 0.368 0.380 0.374 |
| 5 RSD％ | 0.098 1.25％ | 0.279 1.33％ | 0.377 1.27％ |
10, average recovery test
(embodiment 1 to get the Chinese medicinal capsule of the present invention of known emodin and chrysophanol content, 3.74 milligram/gram) content is about 125 milligrams, the accurate title, decide, accurately add a certain amount of emodin and chrysophanol reference substance solution (emodin: 0.1204 mg/ml, chrysophanol: 0.3216 mg/ml), according to the operation down of assay item, measure content, be calculated as follows the response rate, the results are shown in Table 5.
The test of table 5 average recovery
| Sample weighing (milligram) | Emodin and chrysophanol total amount (milligram) in the sample | Add reference substance (milliliter) | Be equivalent to emodin and chrysophanol total amount (milligram) | Measure emodin and chrysophanol total amount (milligram) | The response rate (%) |
| 121.3 115.1 125.2 129.8 128.4 118.6 | 0.4537 0.4305 0.4682 0.4855 0.4802 0.4436 | 0.8 0.8 1.0 1.0 1.2 1.2 | 0.3536 0.3536 0.4420 0.4420 0.5304 0.5304 | 0.8069 0.7750 0.9053 0.9201 0.9958 0.9622 | 99.9 97.4 98.9 98.3 97.2 97.8 |
11, the mensuration of emodin and chrysophanol total amount in the Chinese medicinal capsule of the present invention
According to content assaying method operation in the quality standard text, measured the total amount of emodin and chrysophanol in 6 batches of Chinese medicinal capsules of the present invention respectively, operation repetitive 2 times the results are shown in Table 6.
The mensuration of emodin and chrysophanol total amount in table 6 Chinese medicinal capsule of the present invention
| Lot number | Emodin and chrysophanol total amount (%) | Emodin and chrysophanol total amount (milligram/grain) | Average content (milligram/grain) |
| Embodiment 1 | 0.371 | 1.86 | 1.88 |
| 0.377 | 1.89 | ||
| Embodiment 2 | 0.362 | 1.81 | 1.8 3 |
| 0.369 | 1.85 | ||
| Embodiment 3 | 0.381 | 1.91 | 1.91 |
| 0.380 | 1.90 | ||
| Embodiment 4 | 0.417 | 2.09 | 2.08 |
| 0.414 | 2.07 | ||
| Embodiment 5 | 0.400 | 2.00 | 2.03 |
| 0.410 | 2.05 | ||
| Embodiment 6 | 0.440 | 2.20 | 2.18 |
| 0.429 | 2.15 |
According to the content assaying method of Chinese medicinal capsule of the present invention, 6 batch samples are measured, the results are shown in Table 6." Chinese pharmacopoeia version regulation in 2000 Radix Et Rhizoma Rhei is pressed dry product and is calculated, and contains emodin (C
15H
10O
5) and chrysophanol (C
15H
10O
4) total amount must not be less than 0.5%.Preparation prescription according to Chinese medicinal capsule of the present invention, in rhubarb medicinal material moisture by 10%, flour extraction is by 95%, then embodiment 1 every capsules total amount of containing emodin and chrysophanol should be: (200 * 90% * 95% * 0.5%) ÷ 1000=0.85 (milligram/grain), so tentative every of capsule of the present invention contains Radix Et Rhizoma Rhei with emodin (C
15H
10O
5) and chrysophanol (C
15H
10O
4) the total amount meter, must not be less than 0.85 milligram.
Experimental example 2-clinical observation of the present invention
1 data and method
1.1 physical data: select outpatient service and inpatient's Chinese medical discrimination be attack on the wind-fire, excessive heat in SAN JIAO person totally 53 examples, wherein male 27 examples, woman's 26 examples, minimum 30 years old of age, maximum 62 years old, the sick kind comprised toothache, sore throat, tonsillitis, constipation etc., is divided into treatment at random to organize 35 examples, matched group 18 examples, two groups all there not being significant difference (X checks P＞0.05) aspect sex, age, the course of disease, the sick kind, has comparability.
1.2 case is selected
1.2.1 Chinese medical discrimination standard primary symptom: (1) gingival swelling and pain; (2) aphtha of the mouth and tongue; (3) laryngopharynx swelling and pain; (4) otalgia; (5) epidemic hemorrhagic conjunctivitis; (6) constipation.Inferior disease: (1) tinnitus; (2) have a dizzy spell; (3) yellowish or reddish urine; (4) red tongue with yellow fur; (5) rapid pulse.
1.2.2 the case inclusion criteria possesses two of primary symptoms, inferior disease binomial person promptly can be used as the clinical observation case.
1.2.3 case exclusion standard (1) age is at under-18s, the over-65s person.(2) trimester of pregnancy and women breast-feeding their children.(3) be associated with serious primary disease person such as cardiovascular, Liver and kidney and hemopoietic system.(4) do not meet inclusion criteria, there is the factor that affects the treatment in not medication in accordance with regulations, and can't judge the infull person of curative effect or data.
1.3 Therapeutic Method
The treatment group: take inflammation-relieving capsule (embodiment 1), oral, one time 6,2 times on the one, 6 is a course of treatment;
Matched group: clearing capsule on the Rhizoma Coptidis, oral, one time 6,2 times on the one, 6 is a course of treatment;
All cases are all taken a course of treatment, do not take other medicines in the observation period.
1.4 observation index and recording method by the unified observation table of formulating before treatment and in the therapeutic process with symptom, sign, about lab testing and untoward reaction etc., itemized record on time.
1.5 criterion of therapeutical effect is with reference to card marquis scoring method in " new Chinese medicine clinical research guideline ", promptly the symptom of initiatively saying (have a dizzy spell, otalgia, tinnitus, constipation, yellowish or reddish urine) note is 4 minutes, the symptom got system significantly or continue the person of appearance and remember 3 fens, heavy or be interrupted and note 2 minutes occur when light during symptom, mild symptoms or appearance note once in a while 1 minute, asymptomatic note 0 minute.Gingival swelling and pain in the sign, aphtha of the mouth and tongue, laryngopharynx swelling and pain, each note of epidemic hemorrhagic conjunctivitis 6 minutes, the note that takes a turn for the better 3 minutes, the note that disappears 0 minute; Red tongue, yellow fur, rapid pulse are remembered 6 fens, the note that takes a turn for the better 3 minutes, the note that disappears 0 minute.Integrated value changes before and after observing treatment, calculates the total mark value of every example, judges according to the variation of integrated value.
2 therapeutic outcomes
2.1 efficacy analysis
2.1.1 two groups of cases treatments of two groups of efficacy analysis back symptoms are all obviously improved, treatment group total effective rate is 91.4%, the matched group total effective rate is 83.3%, and concrete outcome sees Table 1
The variation of card marquis integrated value before and after the table 1 liang group treatment (x ± s)
| Symptom | The treatment group | Matched group |
| Tooth pain | 2 | 3 |
| Aphtha of the mouth and tongue | 3 | 3 |
| Laryngopharynx swelling and pain | 2.5 | 2 |
| Epidemic hemorrhagic conjunctivitis | 2 | 2.5 |
| Constipation | 2 | 3 |
| Have a dizzy spell | 2.5 | 2 |
| Otalgia | 2 | 3 |
| Oliguria with reddish urine | 2 | 3 |
| Red tongue with yellow fur | 3 | 3 |
| Rapid pulse | 3 | 3 |
3. conclusion: inflammation-relieving capsule has clearing away heat and loosing the bowels, the effect of the wind pain relieving of loosing.
Claims (10)
1. Chinese medicinal capsule is characterized in that being made by pharmaceutically available adjuvant and following medicine: Folium Isatidis 400-1000 weight portion, Radix Et Rhizoma Rhei 100-300 weight portion, Gypsum Fibrosum 50-150 weight portion, Mentholum 0.5-3 weight portion.
2. the described Chinese medicinal capsule of claim 1 is characterized in that being made by pharmaceutically available adjuvant and following medicine: Folium Isatidis 500-1000 weight portion, Radix Et Rhizoma Rhei 100-200 weight portion, Gypsum Fibrosum 50-100 weight portion, Mentholum 0.5-1.5 weight portion.
3. the described Chinese medicinal capsule of claim 2 is characterized in that being made by pharmaceutically available adjuvant and following medicine: Folium Isatidis 800 weight portions, Radix Et Rhizoma Rhei 200 weight portions, Gypsum Fibrosum 100 weight portions, Mentholum 1.3 weight portions.
4. the described Chinese medicinal capsule of claim 2 is characterized in that being made by pharmaceutically available adjuvant and following medicine: Folium Isatidis 600 weight portions, Radix Et Rhizoma Rhei 200 weight portions, Gypsum Fibrosum 100 weight portions, Mentholum 1.0 weight portions.
5. the preparation method of the arbitrary described Chinese medicinal capsule of claim 1-4 is characterized in that described Radix Et Rhizoma Rhei, Gypsum Fibrosum powder are broken into fine powder, sieves.Folium Isatidis decocts with water 2 times, 1-3 hour for the first time, adds water 8-12 doubly, 0.5-1.5 hour for the second time, add water 6-10 doubly, merging filtrate, filter, filtrate is concentrated into the clear paste that relative density is about 1.15-1.55, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying gets mixed powder, with the Mentholum dissolve with ethanol, spray adds in the mixed powder, the fill capsule, promptly.
6. the preparation method of the described Chinese medicinal capsule of claim 5 is characterized in that described Radix Et Rhizoma Rhei, Gypsum Fibrosum powder are broken into fine powder, sieves.Folium Isatidis decocts with water 2 times, 2 hours for the first time, adds 10 times in water, 1 hour for the second time, add 8 times in water, merging filtrate, filter, filtrate is concentrated into relative density and is about 1.25 clear paste, adds Radix Et Rhizoma Rhei, Gypsum Fibrosum fine powder, mixing, drying gets mixed powder, with the Mentholum dissolve with ethanol, spray adds in the mixed powder, the fill capsule, promptly.
7. claim 1-4 states the method for quality control of Chinese medicinal capsule, it is characterized in that adopting one of following method:
(1), get content 0.5 gram of Chinese medicinal capsule of the present invention, add 10 milliliters of methanol, supersound process 20 minutes, filter, filtrate evaporate to dryness, residue add water makes dissolving for 10 milliliters, add 1 milliliter of hydrochloric acid again, put in the water-bath and heated 30 minutes, cooling is immediately extracted 2 times with the chloroform jolting, each 10 milliliters, merge chloroform liquid, be concentrated into about 1 milliliter, as need testing solution.Other gets Radix Et Rhizoma Rhei control medicinal material 0.2 gram, shines medical material solution in pairs with legal system.Get the emodin reference substance again, add chloroform and make per 1 milliliter of solution that contains 0.5 milligram, product solution in contrast.Test according to thin layer chromatography, draw above-mentioned each 3-5 microlitre of three kinds of solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with petroleum ether (60-90 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Put in the ammonia steam smoked after, inspect under the daylight, speckle becomes redness.
(2), get content 1 gram of Chinese medicinal capsule of the present invention, add 5 milliliters of petroleum ether (60-90 ℃), close plug, jolting number minute was placed 30 minutes, filtration, filtrate is as need testing solution; Other gets the Mentholum reference substance, adds petroleum ether and makes per 1 milliliter of solution that contains 0.5 milligram, product solution in contrast; Test according to thin layer chromatography (appendix VI B), draw above-mentioned each 5-10 microlitre of two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-ethyl acetate (10: 0.5) is developing solvent, launch, take out, dry, spray is with the anisaldehyde test solution, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3), get content 1 gram of Chinese medicinal capsule of the present invention, add 10 milliliters of chloroform, reflux 30 minutes filters, the filtrate evaporate to dryness, residue adds 1% sodium hydroxide makes dissolving for 10 milliliters, extracts 2 times each 10 milliliters with the chloroform jolting, merge chloroform liquid, evaporate to dryness, residue add chloroform makes dissolving for 1 milliliter, as need testing solution; Other gets the indirubin reference substance, adds chloroform and makes per 1 milliliter of solution that contains 1 milligram, product solution in contrast.According to thin layer chromatography test, draw need testing solution 10 microlitres, reference substance solution 5 microlitres, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-chloroform-acetone (5: 4: 1) is developing solvent, launch, take out, dry; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical light violet magenta speckle.
8. claim 1-4 states the method for quality control of Chinese medicinal capsule, it is characterized in that adopting following method: when high performance liquid chromatography detects with emodin as detection material.
9. claim 1-4 states the method for quality control of Chinese medicinal capsule, it is characterized in that adopting following method: when high performance liquid chromatography detects with chrysophanol as detection material.
10. claim 1-4 states the method for quality control of Chinese medicinal capsule, and it is characterized in that adopting following method: the mobile phase when high performance liquid chromatography detects is: methanol-0.1 mol phosphoric acid solution (85: 15); Flow velocity is: 1 ml/min, the detection wavelength is 254nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102772583A (en) * | 2012-07-20 | 2012-11-14 | 蚌埠丰原涂山制药有限公司 | Heat clearing tablet and preparation method thereof |
| CN107569464A (en) * | 2017-09-28 | 2018-01-12 | 承德医学院 | One kind is relieved inflammation or internal heat dripping pill and preparation method thereof |
| CN112946158A (en) * | 2020-11-06 | 2021-06-11 | 天地恒一制药股份有限公司 | Quality detection method of Yankening pills |
| WO2021253803A1 (en) * | 2020-06-18 | 2021-12-23 | 海南葫芦娃药业集团股份有限公司 | Preparation method for fire-purging tablet |
| CN114848729A (en) * | 2022-04-07 | 2022-08-05 | 江西药都仁和制药有限公司 | Method for preparing fire-clearing capsules by combining MVR concentration and single-effect concentration |
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2007
- 2007-04-24 CN CN 200710098387 patent/CN101028348A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102772583A (en) * | 2012-07-20 | 2012-11-14 | 蚌埠丰原涂山制药有限公司 | Heat clearing tablet and preparation method thereof |
| CN102772583B (en) * | 2012-07-20 | 2014-02-19 | 蚌埠丰原涂山制药有限公司 | Heat clearing tablet and preparation method thereof |
| CN107569464A (en) * | 2017-09-28 | 2018-01-12 | 承德医学院 | One kind is relieved inflammation or internal heat dripping pill and preparation method thereof |
| CN107569464B (en) * | 2017-09-28 | 2021-10-15 | 承德医学院 | Fire-clearing dropping pill and preparation method thereof |
| WO2021253803A1 (en) * | 2020-06-18 | 2021-12-23 | 海南葫芦娃药业集团股份有限公司 | Preparation method for fire-purging tablet |
| CN112946158A (en) * | 2020-11-06 | 2021-06-11 | 天地恒一制药股份有限公司 | Quality detection method of Yankening pills |
| CN114848729A (en) * | 2022-04-07 | 2022-08-05 | 江西药都仁和制药有限公司 | Method for preparing fire-clearing capsules by combining MVR concentration and single-effect concentration |
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