CN101623439B - Method for detecting cough quick-relieving capsule - Google Patents
Method for detecting cough quick-relieving capsule Download PDFInfo
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- CN101623439B CN101623439B CN2009103059190A CN200910305919A CN101623439B CN 101623439 B CN101623439 B CN 101623439B CN 2009103059190 A CN2009103059190 A CN 2009103059190A CN 200910305919 A CN200910305919 A CN 200910305919A CN 101623439 B CN101623439 B CN 101623439B
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Abstract
The invention discloses a method for detecting the a cough quick-relieving capsule, which increases the assaying of morphia in poppy capsules on the basis of the prior quality standards, thereby greatly improving the monitor level of the quality of the cough quick-relieving capsule. The invention not only facilitates production monitoring by manufacturers and supervisory and management departments, but also can provide a better guarantee for medical institutions and treatment of patients.
Description
Technical field
The invention belongs to the pharmaceutical technology field, relate to a kind of capsular detection method, particularly a kind of detection method of treating the capsule (adopted name or nomenclature of drug cough quick-relieving capsule) of cough.
Background technology
Cough quick-relieving capsule has boosting qi and nourishing yin, nourishing the lung to arrest cough, and the effect of reinforcing stomach reg fluid can be used for catching a cold and disease such as cough that acute and chronic bronchitis causes, dry pharynx, expectoration, asthma.Herba Reineckeae Carneae, Radix Platycodonis, Cortex Mori, Herba Ephedrae and Pericarpium Papaveris are respectively the characteristic index compositions of cough quick-relieving capsule.In existing cough quick-relieving capsule quality standard, morphine content in the Pericarpium Papaveris is not control effectively, be unfavorable for that manufacturer and superintendent office are to controllable quality.For the quality that further guarantees this product and more help supervision, management to this product quality, thus be necessary the detection method of this medicine is improved, thus further guarantee the quality and the curative effect of this product.
Summary of the invention
The objective of the invention is: the detection method that a kind of cough quick-relieving capsule is provided.The present invention is on initial quality control basis; Increased the method that can effectively detect to the main pharmaceutical compositions of cough quick-relieving capsule; Remedied the deficiency of proper mass control procedure, improved the quality monitoring level of product, also helped administration section product monitoring.
The object of the invention can be realized through following technical proposal:, the detection method of this cough quick-relieving capsule; Calculate according to weight, cough quick-relieving capsule is to process 1000 capsules finished products with Herba Reineckeae Carneae 500g, Rhizoma Polygonati 450g, Herba Aletridis Khasianae 375g, Radix Platycodonis 375g, Herba Saxifragae 250g, Folium Eriobotryae 375g, Herba Ephedrae 200g, Cortex Mori 200g and Pericarpium Papaveris 125g; It is characterized in that this detection method may further comprise the steps:
Character: these article (cough quick-relieving capsule) are capsule, and content is pale brown color to tan granule and a powder; Feeble QI, mildly bitter flavor.
Differentiate: these article content 6g is got in (1), and porphyrize adds 70% ethanol 70ml, and reflux 1.5 hours filters; The filtrating evaporate to dryness, residue adds water 25ml slight fever makes dissolving, moves in the conical flask, adds hydrochloric acid 8ml, reflux 2.5 hours; Put coldly, filter, filtrating is extracted 3 times with the chloroform jolting, at every turn 30ml; Combined chloroform liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Other gets Herba Reineckeae Carneae control medicinal material 4g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B); Draw each 8 μ l of above-mentioned two kinds of solution; Put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with chloroform-ethyl acetate-formic acid (8: 5: 0.2), launch, take out; Dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(2) get these article content 1g, porphyrize adds 7% ethanol solution of sulfuric acid-water (10: 30) mixed liquor 20ml, reflux 3 hours; Put coldly, filter, filtrating is extracted 2 times with the chloroform jolting, at every turn 20ml; Combined chloroform liquid, water 30ml washing discards washing liquid, and chloroform solution is used an amount of anhydrous sodium sulfate dehydration; Filter, the filtrating evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Platycodonis control medicinal material 1g, shines medical material solution in pairs with legal system.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5 μ l～10 μ l of above-mentioned 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 chloroform-ether (1: 1) is developing solvent; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(3) get these article content 3g, add saturated sodium carbonate solution 30ml, supersound process 30 minutes filters; Filtrating is regulated pH value to 1～2 with hydrochloric acid, places 30 minutes, extracts 2 times with the ethyl acetate jolting, each 20ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Mori control medicinal material 2g, shines medical material solution in pairs with legal system, according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draws each 6 μ l of above-mentioned two kinds of solution; Put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with petroleum ether (30～60 ℃)-ethyl acetate (3: 2), launch, take out; Dry, spray is put under the ultra-violet lamp (365nm) and is inspected with 5% sodium hydroxide solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
In the above-mentioned cough quick-relieving capsule detection method, also comprise:
Inspection: should meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2005 L) relevant under the capsule item.
Determination of Ephedrine Hydrochloride is measured, and measures according to HPLC (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; 0.01mol/L (regulating pH value to 2.5 with phosphoric acid)-methanol (94: 6) is mobile phase to potassium dihydrogen phosphate; The detection wavelength is 210nm.Number of theoretical plate calculates by the ephedrine hydrochloride peak should be not less than 2000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the ephedrine hydrochloride reference substance, adds 0.1% methanol hydrochloride solution and process the solution that every 1ml contains 40 μ g, promptly gets.
The preparation of need testing solution: get the content under these article content uniformity item, porphyrize is got 1g, and accurate the title decides, and puts in the tool plug conical flask, adds strong ammonia solution 1.5ml; Airtight, make fully moisteningly, the accurate chloroform 50ml that adds claims to decide weight, supersound process (250W, 40KHz) 30 minutes; Be placed to room temperature and claim to decide weight again, supply the weight that subtracts mistake with chloroform, filter, discard filtrating just, precision is measured subsequent filtrate 25ml; Add 0.1% methanol hydrochloride solution 2ml, shake up, volatilize, residue adds 0.1% methanol hydrochloride solution makes dissolving, moves in the 10ml measuring bottle; Add 0.1% methanol hydrochloride solution and be diluted to scale, shake up, centrifugal, get supernatant, promptly get.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get.
Every of these article contain Herba Ephedrae with ephedrine hydrochloride (C
10H
15NOHCL) meter must not be less than 0.30mg.
The assay of morphine is measured according to HPLC (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; With methanol-0.5% ammonium acetate-1% triethylamine (23: 76.5: 0.5) is mobile phase, and the detection wavelength is 220nm.Number of theoretical plate calculates by the morphine peak should be not less than 3000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the morphine reference substance, adds methanol and process the solution that every 1ml contains 20 μ g, promptly gets.
The preparation of need testing solution: get the content under these article content uniformity item, porphyrize is got 0.5g, and accurate the title decides, and puts in the tool plug conical flask, adds ammonia 1ml, chloroform 50ml successively; Supersound process (250W, 40KHz) 30 minutes, put to room temperature, filter, residue is with minimum of chloroform washing 3 times; Filter, merging filtrate is put water-bath and is volatilized, and residue adds methanol makes dissolving, and moves in the 10ml measuring bottle; Add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly get with 0.45 μ m filter membrane.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get.
Every of these article contain Pericarpium Papaveris with morphine (C
17H
190
3N) meter should be 0.01mg～0.24mg.
In the aforesaid cough quick-relieving capsule detection method, cough quick-relieving capsule is processed according to following method:
Get Radix Platycodonis 250g and be ground into fine powder, residue Radix Platycodonis and Rhizoma Polygonati, Herba Aletridis Khasianae, Radix Platycodonis, Herba Saxifragae, Folium Eriobotryae, Herba Ephedrae, Cortex Mori, this eight flavors decocte with water secondary of Pericarpium Papaveris, each 2 hours, merging filtrate; Filter, leave standstill, get supernatant, being concentrated into relative density is the clear paste of 1.25～1.30 (80 ℃); Add Radix Platycodonis fine powder and appropriate amount of starch, stir, process granule; Drying incapsulates, and promptly gets.
Compared with prior art, the present invention has increased the assay of morphine in the Pericarpium Papaveris on existing quality standard basis.Can more effectively control the main ingredient of cough quick-relieving capsule, make the quality monitoring level of cough quick-relieving capsule be greatly improved.Application of the present invention, both more help manufacturer and supervisory and management department to the monitoring of product quality, also can better guarantee be provided for medical department and patient's treatment.
The specific embodiment
The detection method of this cough quick-relieving capsule; Calculate according to weight, cough quick-relieving capsule is to process 1000 capsules finished products with Herba Reineckeae Carneae 500g, Rhizoma Polygonati 450g, Herba Aletridis Khasianae 375g, Radix Platycodonis 375g, Herba Saxifragae 250g, Folium Eriobotryae 375g, Herba Ephedrae 200g, Cortex Mori 200g, Pericarpium Papaveris 125g; It is characterized in that this detection method may further comprise the steps:
Character: these article are capsule, and content is pale brown color to tan granule and a powder; Feeble QI, mildly bitter flavor;
Differentiate: these article content 6g is got in (1), and porphyrize adds 70% ethanol 70ml, and reflux 1.5 hours filters; The filtrating evaporate to dryness, residue adds water 25ml slight fever makes dissolving, moves in the conical flask, adds hydrochloric acid 8ml, reflux 2.5 hours; Put coldly, filter, filtrating is extracted 3 times with the chloroform jolting, at every turn 30ml; Combined chloroform liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Other gets Herba Reineckeae Carneae control medicinal material 4g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B); Draw each 8 μ l of above-mentioned two kinds of solution; Put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with chloroform-ethyl acetate-formic acid (8: 5: 0.2), launch, take out; Dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(2) get these article content 1g, porphyrize adds 7% ethanol solution of sulfuric acid-water (10: 30) mixed liquor 20ml, reflux 3 hours; Put coldly, filter, filtrating is extracted 2 times with the chloroform jolting, at every turn 20ml; Combined chloroform liquid, water 30ml washing discards washing liquid, and chloroform solution is used an amount of anhydrous sodium sulfate dehydration; Filter, the filtrating evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Platycodonis control medicinal material 1g, shines medical material solution in pairs with legal system.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5 μ l～10 μ l of above-mentioned 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 chloroform-ether (1: 1) is developing solvent; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(3) get these article content 3g, add saturated sodium carbonate solution 30ml, supersound process 30 minutes filters; Filtrating is regulated pH value to 1～2 with hydrochloric acid, places 30 minutes, extracts 2 times with the ethyl acetate jolting, each 20ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Mori control medicinal material 2g, shines medical material solution in pairs with legal system, according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draws each 6 μ l of above-mentioned two kinds of solution; Put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with petroleum ether (30～60 ℃)-ethyl acetate (3: 2), launch, take out; Dry, spray is put under the ultra-violet lamp (365nm) and is inspected with 5% sodium hydroxide solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
Inspection: should meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2005 L) relevant under the capsule item.
Determination of Ephedrine Hydrochloride is measured, and measures according to HPLC (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; 0.01mol/L (regulating pH value to 2.5 with phosphoric acid)-methanol (94: 6) is mobile phase to potassium dihydrogen phosphate; The detection wavelength is 210nm.Number of theoretical plate calculates by the ephedrine hydrochloride peak should be not less than 2000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the ephedrine hydrochloride reference substance, adds 0.1% methanol hydrochloride solution and process the solution that every 1ml contains 40 μ g, promptly gets.
The preparation of need testing solution: get the content under these article content uniformity item, porphyrize is got 1g, and accurate the title decides, and puts in the tool plug conical flask, adds strong ammonia solution 1.5ml; Airtight, make fully moisteningly, the accurate chloroform 50ml that adds claims to decide weight, supersound process (250W, 40KHz) 30 minutes; Be placed to room temperature and claim to decide weight again, supply the weight that subtracts mistake with chloroform, filter, discard filtrating just, precision is measured subsequent filtrate 25ml; Add 0.1% methanol hydrochloride solution 2ml, shake up, volatilize, residue adds 0.1% methanol hydrochloride solution makes dissolving, moves in the 10ml measuring bottle; Add 0.1% methanol hydrochloride solution and be diluted to scale, shake up, centrifugal, get supernatant, promptly get.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get.
Every of these article contain Herba Ephedrae with ephedrine hydrochloride (C
10H
15NOHCL) meter must not be less than 0.30mg.
The assay of morphine: measure according to HPLC (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; With methanol-0.5% ammonium acetate-1% triethylamine (23: 76.5: 0.5) is mobile phase, and the detection wavelength is 220nm.Number of theoretical plate calculates by the morphine peak should be not less than 3000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the morphine reference substance, adds methanol and process the solution that every 1ml contains 20 μ g, promptly gets.
The preparation of need testing solution: get the content under these article content uniformity item, porphyrize is got 0.5g, and accurate the title decides, and puts in the tool plug conical flask, adds ammonia 1ml, chloroform 50ml successively; Supersound process (250W, 40KHz) 30 minutes, put to room temperature, filter, residue is with minimum of chloroform washing 3 times; Filter, merging filtrate is put water-bath and is volatilized, and residue adds methanol makes dissolving, and moves in the 10ml measuring bottle; Add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly get with 0.45 μ m filter membrane.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get.
Every of these article contain Pericarpium Papaveris with morphine (C
17H
19O
3N) meter should be 0.01mg～0.24mg.
Described cough quick-relieving capsule is processed according to following method:
Get Radix Platycodonis 250g and be ground into fine powder, residue Radix Platycodonis and Rhizoma Polygonati, Herba Aletridis Khasianae, Radix Platycodonis, Herba Saxifragae, Folium Eriobotryae, Herba Ephedrae, Cortex Mori, this eight flavors decocte with water secondary of Pericarpium Papaveris, each 2 hours, merging filtrate; Filter, leave standstill, get supernatant, being concentrated into relative density is the clear paste of 1.25～1.30 (80 ℃); Add Radix Platycodonis fine powder and appropriate amount of starch, stir, process granule; Drying incapsulates, and promptly gets.
Claims (2)
1. the detection method of cough quick-relieving capsule; Calculate according to weight, cough quick-relieving capsule is to process 1000 capsules finished products with Herba Reineckeae Carneae 500g, Rhizoma Polygonati 450g, Herba Aletridis Khasianae 375g, Radix Platycodonis 375g, Herba Saxifragae 250g, Folium Eriobotryae 375g, Herba Ephedrae 200g, Cortex Mori 200g and Pericarpium Papaveris 125g; It is characterized in that this detection method may further comprise the steps:
Character: these article are capsule, and content is pale brown color to tan granule and a powder; Feeble QI, mildly bitter flavor;
Differentiate: these article content 6g is got in (1), and porphyrize adds 70% ethanol 70ml, and reflux 1.5 hours filters; The filtrating evaporate to dryness, residue adds water 25ml slight fever makes dissolving, moves in the conical flask, adds hydrochloric acid 8ml, reflux 2.5 hours; Put coldly, filter, filtrating is extracted 3 times with the chloroform jolting, at every turn 30ml; Combined chloroform liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Herba Reineckeae Carneae control medicinal material 4g, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 8 μ l of above-mentioned 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 chloroform-ethyl acetate of 8: 5: 0.2-formic acid is developing solvent; Launch, take out, dry, put under the ultra-violet lamp that wavelength is 365nm and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(2) get these article content 1g, porphyrize adds 7% ethanol solution of sulfuric acid-water mixed liquid 20ml of 10: 30, reflux 3 hours; Put coldly, filter, filtrating is extracted 2 times with the chloroform jolting, at every turn 20ml; Combined chloroform liquid, water 30ml washing discards washing liquid, and chloroform solution is used an amount of anhydrous sodium sulfate dehydration; Filter, the filtrating evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Radix Platycodonis control medicinal material 1g, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 5 μ l～10 μ l of above-mentioned 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 1: 1 chloroform-ether was developing solvent; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(3) get this product content 3g, add saturated sodium carbonate solution 30ml, sonicated 30 minutes filters, and filtrating is used salt acid for adjusting pH value to 1～2; Placed 30 minutes, and extracted 2 times, each 20ml, combined ethyl acetate liquid, evaporate to dryness with the ethyl acetate jolting; Residue adds methyl alcohol 1ml makes dissolving, and as need testing solution, other gets root bark of white mulberry control medicinal material 2g, shines medicinal material solution in pairs with legal system; According to thin-layered chromatography test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethylcellulose, be solvent with 30～60 ℃ of petroleum ether-ethyl acetates of 3: 2; Launch, take out, dry, spray is with 5% sodium hydroxide solution; Put under the ultraviolet lamp that wavelength is 365nm and inspect, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
This detection method also comprises:
Inspection should meet each item regulation relevant under the capsule item;
Determination of Ephedrine Hydrochloride is measured, according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; The 0.01mol/L potassium dihydrogen phosphate-methanol that uses phosphoric acid to regulate pH value to 2.5 with 94: 6 is mobile phase; The detection wavelength is 210nm; Number of theoretical plate calculates by the ephedrine hydrochloride peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the ephedrine hydrochloride reference substance, adds 0.1% methanol hydrochloride solution and process the solution that every 1ml contains 40 μ g, promptly gets;
The preparation of need testing solution: get the content under these article content uniformity item, porphyrize is got 1g, and accurate the title decides, and puts in the tool plug conical flask, adds strong ammonia solution 1.5ml; Airtight, make fully moisteningly, the accurate chloroform 50ml that adds claims to decide weight, the supersound process through 250W, 40KHz 30 minutes; Be placed to room temperature and claim to decide weight again, supply the weight that subtracts mistake with chloroform, filter, discard filtrating just, precision is measured subsequent filtrate 25ml; Add 0.1% methanol hydrochloride solution 2ml, shake up, volatilize, residue adds 0.1% methanol hydrochloride solution makes dissolving, moves in the 10ml measuring bottle; Add 0.1% methanol hydrochloride solution and be diluted to scale, shake up, centrifugal, get supernatant, promptly get;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get;
Every of these article contain Herba Ephedrae with ephedrine hydrochloride (C
10H
15NOHCL) meter must not be less than 0.30mg;
The assay of morphine is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; With 23: 76.5: 0.5 methanol-0.5% ammonium acetate-1% triethylamine is mobile phase, and the detection wavelength is 220nm; Number of theoretical plate calculates by the morphine peak should be not less than 3000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the morphine reference substance, adds methanol and process the solution that every 1ml contains 20 μ g, promptly gets;
The preparation of need testing solution: get the content under this product content uniformity item, porphyrize is got 0.5g, and accurate the title decides, and puts in the tool plug conical flask, adds ammoniacal liquor 1ml, chloroform 50ml successively; By 250W, the sonicated of 40KHz 30 minutes is put to room temperature, filters, and residue washs 3 times with minimum of chloroform; Filter, merging filtrate is put water-bath and is volatilized, and residue adds methyl alcohol makes dissolving, and moves in the 10ml measuring bottle; Add methyl alcohol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly get with 0.45 μ m filter membrane;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get;
Every of these article contain Pericarpium Papaveris with morphine (C
17H
19O
3N) meter should be 0.01mg～0.24mg.
2. the detection method of cough quick-relieving capsule according to claim 1 is characterized in that, described cough quick-relieving capsule is processed according to following method:
Get Radix Platycodonis 250g and be ground into fine powder, this eight flavors decocte with water secondary of residue Radix Platycodonis and Rhizoma Polygonati, Herba Aletridis Khasianae, Radix Platycodonis, Herba Saxifragae, Folium Eriobotryae, Herba Ephedrae, Cortex Mori and Pericarpium Papaveris, each 2 hours, merging filtrate; Filter, leave standstill, get supernatant, relative density is 1.25～1.30 clear paste when being concentrated into 80 ℃; Add Radix Platycodonis fine powder and appropriate amount of starch, stir, process granule; Drying incapsulates, and promptly gets.
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| CN104844720B (en) * | 2015-06-19 | 2016-11-09 | 贵州师范学院 | A kind of separating and extracting process of hundred tail gracilis polysaccharides |
| CN106198842A (en) * | 2016-08-31 | 2016-12-07 | 天津中新药业研究中心 | A kind of method of quality control of removing heat from the lung and dissipating phlegm antitussive medicine |
| CN106324161B (en) * | 2016-10-24 | 2017-11-14 | 广州康臣药物研究有限公司 | Treat the quality determining method of the Chinese medicine composition of diabetic nephropathy |
| CN111337599A (en) * | 2018-12-18 | 2020-06-26 | 新疆维吾尔药业有限责任公司 | Pretreatment method, morphine detection method and application |
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Non-Patent Citations (1)
| Title |
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| 国家药品监督管理局.《咳速停胶囊》.《国家药品中药标准 内科 肺系（1）分册》.2002,505. * |
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