CN101361869B - Quality control method of tables for treating asthma - Google Patents
Quality control method of tables for treating asthma Download PDFInfo
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- CN101361869B CN101361869B CN2008101985931A CN200810198593A CN101361869B CN 101361869 B CN101361869 B CN 101361869B CN 2008101985931 A CN2008101985931 A CN 2008101985931A CN 200810198593 A CN200810198593 A CN 200810198593A CN 101361869 B CN101361869 B CN 101361869B
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Abstract
The invention discloses a quality control method for Xiaochuanning Pian (a tablet for treating asthma), to which drug identification and content determination are added. The method can identify the active compositions of Chinese ephedra, fructus schisandrae chinensis and radix polygalae and determine the content of Chinese ephedra to improve the exclusiveness and effectiveness of the quality control, thus being beneficial for the effective quality control of the finished Xiaochuanning Pian.
Description
Technical field
The present invention relates to a kind of method of quality control of tables for treating asthma.
Background technology
Tables for treating asthma is a kind of bronchial astehma, chronic cough of being used for the treatment of, Chinese medicine out of breath, this product is included in the 4th the 148th page in Drug Standard of Ministry of Public Health of the Peoples Republic of China Chinese traditional patent formulation preparation, by arisaema cum bile 150g, and gypsum 125g, Radix Glycyrrhizae 75g, datura flower 50g, fruit of Chinese magnoliavine 400g, polygala root (system) 150g, radix pseudostellariae 400g, eight flavor medicinal materials such as Chinese ephedra (honey is processed) 200g are made.Because the part medicinal material does not have reference substance, or because prescription is big, composition is difficult to separate, said preparation proper mass control criterion is comparatively simple, only has proterties to check item, and no medicine is differentiated and content assaying method, be not enough to control the quality of finished product, thereby influence its clinical efficacy and use.
Summary of the invention
The method of quality control that the purpose of this invention is to provide a kind of tables for treating asthma, having increased medicine differentiates and content assaying method, can differentiate and assay the effective constituent of tables for treating asthma, specificity and validity with the control that improves the quality, thereby help improving the quality control of tables for treating asthma, guarantee the quality and the clinical efficacy of this medicine.
Method of quality control of the present invention mainly comprise differentiate and the assay project in partly or entirely, wherein differentiate the thin-layer chromatography discriminating that comprises the Chinese ephedra in the preparation, the fruit of Chinese magnoliavine, polygala root, assay is the assay to the contained ephedrine of the Chinese ephedra in the preparation.
The discrimination method of its epheday intermedia is to be contrast with the ephedrine hydrochloride reference substance, and the toluene-chloroform-methanol that with the volume ratio is 5:20:2 is the thin-layered chromatography of developping agent; The discrimination method of the fruit of Chinese magnoliavine is to be contrast with fruit of Chinese magnoliavine control medicinal material and schizandrin A reference substance respectively, the toluene-ethyl acetate that with the volume ratio is 9:1 be developping agent thin-layered chromatography; The polygala root discrimination method is to be contrast with the polygala root control medicinal material, and the chloroform-acetone-normal hexane-acetate that with the volume ratio is 15:3:0.3:0.5 is the thin-layered chromatography of developping agent.
Discrimination method comprises in the following project one or multinomial:
(1), get 15 of tables for treating asthma finished products, porphyrize adds 20 of strong ammonia solutions, adds chloroform 10ml again, reflux 1 hour filters, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Thin-layered chromatography test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, in with the pre-saturated expansion cylinder of dense ammonia test, be developping agent with toluene-chloroform-methanol of 5:20:2, launch, take out, dry, spray is with ninhydrin solution, and 105 ℃ to be heated to spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2), get 15 of tables for treating asthma finished products, porphyrize adds chloroform 20ml, reflux 30 minutes filters, filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Get fruit of Chinese magnoliavine control medicinal material 1g and shine medicinal material solution in pairs with legal system; Get the schizandrin A reference substance again, chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test of an appendix VIB record of Chinese Pharmacopoeia version in 2005, draw each 5 μ l of above-mentioned three kinds of solution, put in same silica G F respectively
254On the thin layer plate, be developping agent, launch, take out, dry, put under the uviol lamp of 254nm and inspect with toluene-ethyl acetate of 9:1; In the test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color;
(3), get 20 of this product, porphyrize, the hydrochloric acid ethanol solution 30ml of adding 10%, water-bath reflux 30 minutes, taking-up, put coldly, filter, filtrate adds water 45ml, with chloroform extraction 2 times, and each 30ml, combined chloroform liquid, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets polygala root control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; Thin-layered chromatography test according to an appendix VIB record of Chinese Pharmacopoeia version in 2005, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, chloroform-acetone-normal hexane-acetate with 15:3:0.3:0.5 is developping agent, launch, take out, dry, spray is mixed with the solution that forms with the ethanol solution of sulfuric acid of 8% vanillic aldehyde ethanol solution and 70% in the ratio of 1:10,105 ℃ are dried by the fire to clear spot, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical pansy spot.
The content assaying method of Chinese ephedra epheday intermedia alkali is to be contrast with the ephedrine hydrochloride reference substance, is the high performance liquid chromatography of moving phase with the 0.02mol/L potassium dihydrogen phosphate that contains 0.1% triethylamine and 0.1% phosphoric acid and acetonitrile with the ratio of 95:5.The content assaying method of ephedrine is:
Get the tables for treating asthma finished product under the weight differential item, porphyrize is got 1.0g, and accurate the title decides, put in the 50ml tool plug conical flask, accurate adding strong ammonia solution 1ml makes moistening, and the accurate again 25ml methylene chloride that adds claims to decide weight, sonicated 30 minutes, put coldly, claim to decide weight, supply the weight that subtracts mistake with methylene chloride, filter, get subsequent filtrate 10ml, put in the 25ml evaporating dish, add 5% the ethanol solution hydrochloride of 1ml, the low temperature evaporate to dryness, residue adds 5% ethanol solution hydrochloride makes dissolving in right amount, is transferred in the 25ml volumetric flask, adds 0.1mol/L HCl solution washing container and is diluted to scale, shake up, with the aperture is the miillpore filter filtration of 0.45 μ m, gets subsequent filtrate, promptly gets for test agent solution; It is an amount of that precision takes by weighing the ephedrine hydrochloride reference substance, adds 0.1mol/L HCl solution and make the solution that every 1ml contains 10 μ g, promptly gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, are filling agent with octadecylsilane chemically bonded silica; Is moving phase with the 0.02mol/L potassium dihydrogen phosphate that contains 0.1% triethylamine and 0.1% phosphoric acid and acetonitrile with the ratio of 95:5; The detection wavelength is 207nm; Theoretical cam curve is calculated by the ephedrine hydrochloride peak should be not less than 3000, measures, promptly;
This product contains Chinese ephedra with ephedrine hydrochloride C
10H
15NOHCl calculates, and every setting value is more than or equal to 0.2mg.
Above-mentioned steps does not need sequencing to carry out, and can also carry out conventional sense simultaneously, and as the observation of shape, this tables for treating asthma is the taupe sheet, the little raw meat of gas, and it is salty, bitter to distinguish the flavor of.This finished product also should meet relevant every regulation under 11 pages of tablet items of Chinese Pharmacopoeia appendix.
The tables for treating asthma finished product that meets above-mentioned condition is qualified.
The present invention has improved the quality check step in the existing tables for treating asthma, having increased medicine differentiates and the assay step, can differentiate and assay the effective constituent of tables for treating asthma, specificity and validity with the control that improves the quality help the tables for treating asthma end product quality is control effectively.
Embodiment:
Further specify the present invention by the following examples, but not as limitation of the present invention.
Embodiment 1:
The method of quality control of a kind of tables for treating asthma in the present embodiment comprises:
Differentiate:
(1), get 15 of tables for treating asthma finished products, porphyrize adds 20 of strong ammonia solutions, adds chloroform 10ml again, reflux 1 hour filters, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Thin-layered chromatography test according to an appendix VIB record of Chinese Pharmacopoeia version in 2005, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, in with the pre-saturated expansion cylinder of dense ammonia test, be developping agent with toluene-chloroform-methanol of 5:20:2, launch, take out, dry, spray is with ninhydrin solution, and 105 ℃ to be heated to spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2), get 15 of tables for treating asthma finished products, porphyrize adds chloroform 20ml, reflux 30 minutes filters, filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Get fruit of Chinese magnoliavine control medicinal material 1g and shine medicinal material solution in pairs with legal system; Get the schizandrin A reference substance again, chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned three kinds of solution, put in same silica G F respectively
254On the thin layer plate, be developping agent, launch, take out, dry, put under the uviol lamp of 254nm and inspect with toluene-ethyl acetate of 9:1; In the test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color;
(3), get 20 of this product, porphyrize adds 10% hydrochloric acid ethanol solution 30ml, water-bath reflux 30 minutes is taken out, put coldly, filter, filtrate adds water 45ml, with chloroform extraction 2 times, and each 30ml, combined chloroform liquid, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets polygala root control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; Thin-layered chromatography test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, chloroform-acetone-normal hexane-acetate with 15:3:0.3:0.5 is developping agent, launch, take out, dry, spray is mixed with the solution that forms with the ethanol solution of sulfuric acid of 8% vanillic aldehyde ethanol solution and 70% in the ratio of 1:10,105 ℃ are dried by the fire to clear spot, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical pansy spot.
Assay:
Get the tables for treating asthma finished product under the weight differential item, porphyrize is got 1.0g, and accurate the title decides, put in the 50ml tool plug conical flask, accurate adding strong ammonia solution 1ml makes moistening, and the accurate again 25ml methylene chloride that adds claims to decide weight, sonicated 30 minutes, put coldly, claim to decide weight, supply the weight that subtracts mistake with methylene chloride, filter, get subsequent filtrate 10ml, put in the 25ml evaporating dish, add the ethanol solution hydrochloride of 1ml5%, the low temperature evaporate to dryness, residue adds 5% ethanol solution hydrochloride makes dissolving in right amount, is transferred in the 25ml volumetric flask, adds 0.1mol/L HCl solution washing container and is diluted to scale, shake up, with the aperture is the miillpore filter filtration of 0.45 μ m, gets subsequent filtrate, promptly gets for test agent solution; It is an amount of that precision takes by weighing the ephedrine hydrochloride reference substance, adds 0.1mol/L HCl solution and make the solution that every 1ml contains 10 μ g, promptly gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, are filling agent with octadecylsilane chemically bonded silica; Is moving phase with the 0.02mol/L potassium dihydrogen phosphate that contains 0.1% triethylamine and 0.1% phosphoric acid and acetonitrile with the ratio of 95:5; The detection wavelength is 207nm; Theoretical cam curve is calculated by the ephedrine hydrochloride peak should be not less than 3000, measures, promptly.
This product contains Chinese ephedra with ephedrine hydrochloride C
10H
15NOHCl calculates, and every content is not less than 0.2mg.
Above-mentioned steps does not need sequencing to carry out, and can also carry out conventional sense simultaneously, and as the observation of shape, this tables for treating asthma is the taupe sheet, the little raw meat of gas, and it is salty, bitter to distinguish the flavor of.This finished product also should meet relevant every regulation under 11 pages of tablet items of Chinese Pharmacopoeia appendix.
The tables for treating asthma finished product that meets above-mentioned condition is qualified.
Embodiment 2: the method for quality control of tables for treating asthma can comprise:
Differentiate:
(1), get 15 of tables for treating asthma finished products, porphyrize adds chloroform 20ml, reflux 30 minutes filters, filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Get fruit of Chinese magnoliavine control medicinal material 1g and shine medicinal material solution in pairs with legal system; Get the schizandrin A reference substance again, chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned three kinds of solution, put in same silica G F respectively
254On the thin layer plate, be developping agent, launch, take out, dry, put under the uviol lamp of 254nm and inspect with toluene-ethyl acetate of 9:1; In the test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color;
(2), get 20 of this product, porphyrize, the hydrochloric acid ethanol solution 30ml of adding 10%, water-bath reflux 30 minutes, taking-up, put coldly, filter, filtrate adds water 45ml, with chloroform extraction 2 times, and each 30ml, combined chloroform liquid, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets polygala root control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; Thin-layered chromatography test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, chloroform-acetone-normal hexane-acetate with 15:3:0.3:0.5 is developping agent, launch, take out, dry, spray is mixed with the solution that forms with the ethanol solution of sulfuric acid of 8% vanillic aldehyde ethanol solution and 70% in the ratio of 1:10,105 ℃ are dried by the fire to clear spot, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical pansy spot.
Assay:
Get the tables for treating asthma finished product under the weight differential item, porphyrize is got 1.0g, and accurate the title decides, put in the 50ml tool plug conical flask, accurate adding strong ammonia solution 1ml makes moistening, and the accurate again 25ml methylene chloride that adds claims to decide weight, sonicated 30 minutes, put coldly, claim to decide weight, supply the weight that subtracts mistake with methylene chloride, filter, get subsequent filtrate 10ml, put in the 25ml evaporating dish, add the ethanol solution hydrochloride of 1ml5%, the low temperature evaporate to dryness, residue adds 5% ethanol solution hydrochloride makes dissolving in right amount, is transferred in the 25ml volumetric flask, adds 0.1mol/L HCl solution washing container and is diluted to scale, shake up, with the aperture is the miillpore filter filtration of 0.45 μ m, gets subsequent filtrate, promptly gets for test agent solution; It is an amount of that precision takes by weighing the ephedrine hydrochloride reference substance, adds 0.1mol/L HCl solution and make the solution that every 1ml contains 10 μ g, promptly gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, are filling agent with octadecylsilane chemically bonded silica; Is moving phase with the 0.02mol/L potassium dihydrogen phosphate that contains 0.1% triethylamine and 0.1% phosphoric acid and acetonitrile with the ratio of 95:5; The detection wavelength is 207nm; Theoretical cam curve is calculated by the ephedrine hydrochloride peak should be not less than 3000, measures, promptly.
This product contains Chinese ephedra with ephedrine hydrochloride C
10H
15NOHCl calculates, and every content is not less than 0.2mg.
Above-mentioned steps does not need sequencing to carry out, and can also carry out conventional sense simultaneously, and as the observation of shape, this tables for treating asthma is the taupe sheet, the little raw meat of gas, and it is salty, bitter to distinguish the flavor of.This finished product also should meet relevant every regulation under 11 pages of tablet items of Chinese Pharmacopoeia appendix.
The tables for treating asthma finished product that meets above-mentioned condition is qualified.
Embodiment 3: the method for quality control of tables for treating asthma can comprise:
Differentiate:
Get 15 of tables for treating asthma finished products, porphyrize adds chloroform 20ml, and reflux 30 minutes filters, and filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Get fruit of Chinese magnoliavine control medicinal material 1g and shine medicinal material solution in pairs with legal system; Get the schizandrin A reference substance again, chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned three kinds of solution, put in same silica G F respectively
254On the thin layer plate, be developping agent, launch, take out, dry, put under the uviol lamp of 254nm and inspect with toluene-ethyl acetate of 9:1; In the test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color;
Assay:
Get the tables for treating asthma finished product under the weight differential item, porphyrize is got 1.0g, and accurate the title decides, put in the 50ml tool plug conical flask, accurate adding strong ammonia solution 1ml makes moistening, and the accurate again 25ml methylene chloride that adds claims to decide weight, sonicated 30 minutes, put coldly, claim to decide weight, supply the weight that subtracts mistake with methylene chloride, filter, get subsequent filtrate 10ml, put in the 25ml evaporating dish, add the ethanol solution hydrochloride of 1ml5%, the low temperature evaporate to dryness, residue adds 5% ethanol solution hydrochloride makes dissolving in right amount, is transferred in the 25ml volumetric flask, adds 0.1mol/L HCl solution washing container and is diluted to scale, shake up, with the aperture is the miillpore filter filtration of 0.45 μ m, gets subsequent filtrate, promptly gets for test agent solution; It is an amount of that precision takes by weighing the ephedrine hydrochloride reference substance, adds 0.1mol/L HCl solution and make the solution that every 1ml contains 10 μ g, promptly gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, are filling agent with octadecylsilane chemically bonded silica; Is moving phase with the 0.02mol/L potassium dihydrogen phosphate that contains 0.1% triethylamine and 0.1% phosphoric acid and acetonitrile with the ratio of 95:5; The detection wavelength is 207nm; Theoretical cam curve is calculated by the ephedrine hydrochloride peak should be not less than 3000, measures, promptly.
This product contains Chinese ephedra with ephedrine hydrochloride C
10H
15NOHCl calculates, and every content is not less than 0.2mg.
Above-mentioned steps does not need sequencing to carry out, and can also carry out conventional sense simultaneously, and as the observation of shape, this tables for treating asthma is the taupe sheet, the little raw meat of gas, and it is salty, bitter to distinguish the flavor of.This finished product also should meet relevant every regulation under 11 pages of tablet items of Chinese Pharmacopoeia appendix.
The tables for treating asthma finished product that meets above-mentioned condition is qualified.
Embodiment 4: the method for quality control of tables for treating asthma can comprise:
Differentiate:
(1), get 15 of tables for treating asthma finished products, porphyrize adds 20 of strong ammonia solutions, adds chloroform 10ml again, reflux 1 hour filters, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Thin-layered chromatography test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, in with the pre-saturated expansion cylinder of dense ammonia test, be developping agent with toluene-chloroform-methanol of 5:20:2, launch, take out, dry, spray is with ninhydrin solution, and 105 ℃ to be heated to spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2), get 15 of tables for treating asthma finished products, porphyrize adds chloroform 20ml, reflux 30 minutes filters, filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Get fruit of Chinese magnoliavine control medicinal material 1g and shine medicinal material solution in pairs with legal system; Get the schizandrin A reference substance again, chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned three kinds of solution, put in same silica G F respectively
254On the thin layer plate, be developping agent, launch, take out, dry, put under the uviol lamp of 254nm and inspect with toluene-ethyl acetate of 9:1; In the test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color;
Above-mentioned steps does not need sequencing to carry out, and can also carry out conventional sense simultaneously, and as the observation of shape, this tables for treating asthma is the taupe sheet, the little raw meat of gas, and it is salty, bitter to distinguish the flavor of.This finished product also should meet relevant every regulation under 11 pages of tablet items of Chinese Pharmacopoeia appendix.
The tables for treating asthma finished product that meets above-mentioned condition is qualified.
Claims (5)
1. the analytical approach of a tables for treating asthma, it is characterized in that: described analytical approach mainly comprise differentiate and the assay project in partly or entirely, the discrimination method of its epheday intermedia is to be contrast with the ephedrine hydrochloride reference substance, is that toluene-chloroform-methanol of 5: 20: 2 is the thin-layered chromatography of developping agent with volume ratio; The discrimination method of the fruit of Chinese magnoliavine is to be contrast with fruit of Chinese magnoliavine control medicinal material and schizandrin A reference substance respectively, with volume ratio be toluene-ethyl acetate of 9: 1 be developping agent thin-layered chromatography; The polygala root discrimination method is to be contrast with the polygala root control medicinal material, with volume ratio is 15: 3: 0.3: chloroform-acetone of 0.5-normal hexane-acetate is the thin-layered chromatography of developping agent, assay is the assay to the contained ephedrine of the Chinese ephedra in the preparation, with ephedrine hydrochloride C
10H
15NOHCl calculates, and every setting value is more than or equal to 0.2mg.
2. the analytical approach of tables for treating asthma according to claim 1 is characterized in that: discrimination method comprises in the following project one or multinomial:
(1), get 15 of tables for treating asthma finished products, porphyrize adds 20 of strong ammonia solutions, adds chloroform 10ml again, reflux 1 hour filters, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Thin-layered chromatography test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, in with the pre-saturated expansion cylinder of dense ammonia test, be developping agent with toluene-chloroform-methanols of 5: 20: 2, launch, take out, dry, spray is with ninhydrin solution, and 105 ℃ to be heated to spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2), get 15 of tables for treating asthma finished products, porphyrize adds chloroform 20ml, reflux 30 minutes filters, filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Get fruit of Chinese magnoliavine control medicinal material 1g and shine medicinal material solution in pairs with legal system; Get the schizandrin A reference substance again, chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned three kinds of solution, put in same silica G F respectively
254On the thin layer plate, be developping agent, launch, take out, dry, put under the uviol lamp of 254nm and inspect with toluene-ethyl acetate of 9: 1; In the test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color;
(3), get 20 of this product, porphyrize, the hydrochloric acid ethanol solution 30ml of adding 10%, water-bath reflux 30 minutes, taking-up, put coldly, filter, filtrate adds water 45ml, with chloroform extraction 2 times, and each 30ml, combined chloroform liquid, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets polygala root control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; Thin-layered chromatography test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 15: 3: 0.3: chloroform-acetone of 0.5-normal hexane-acetate was developping agent, launch, take out, dry, spray is mixed with the solution that forms with the ethanol solution of sulfuric acid of 8% vanillic aldehyde ethanol solution and 70% in 1: 10 ratio, 105 ℃ are dried by the fire to clear spot, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical pansy spot.
3. the analytical approach of tables for treating asthma according to claim 1, it is characterized in that: the content assaying method of Chinese ephedra epheday intermedia alkali is to be contrast with the ephedrine hydrochloride reference substance, is the high performance liquid chromatography of moving phase with the 0.02mol/L potassium dihydrogen phosphate that contains 0.1% triethylamine and 0.1% phosphoric acid and acetonitrile with 95: 5 ratio.
4. according to the analytical approach of claim 1 or 3 described tables for treating asthma, it is characterized in that: the content assaying method of ephedrine is:
Get the tables for treating asthma finished product under the weight differential item, porphyrize is got 1.0g, and accurate the title decides, put in the 50ml tool plug conical flask, accurate adding strong ammonia solution 1ml makes moistening, and the accurate again 25ml methylene chloride that adds claims to decide weight, sonicated 30 minutes, put coldly, claim to decide weight, supply the weight that subtracts mistake with methylene chloride, filter, get subsequent filtrate 10ml, put in the 25ml evaporating dish, add 5% the ethanol solution hydrochloride of 1ml, the low temperature evaporate to dryness, residue adds 5% ethanol solution hydrochloride makes dissolving in right amount, is transferred in the 25ml volumetric flask, adds 0.1mol/L HCl solution washing container and is diluted to scale, shake up, with the aperture is the miillpore filter filtration of 0.45 μ m, gets subsequent filtrate, promptly gets for test agent solution; It is an amount of that precision takes by weighing the ephedrine hydrochloride reference substance, adds 0.1mol/L HCl solution and make the solution that every 1ml contains 10 μ g, promptly gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, are filling agent with octadecylsilane chemically bonded silica; Is moving phase with the 0.02mol/L potassium dihydrogen phosphate that contains 0.1% triethylamine and 0.1% phosphoric acid and acetonitrile with 95: 5 ratio; The detection wavelength is 207nm; Theoretical cam curve is calculated by the ephedrine hydrochloride peak should be not less than 3000, measures, promptly;
This product contains Chinese ephedra with ephedrine hydrochloride C
10H
15NOHCl calculates, and every setting value is more than or equal to 0.2mg.
5. the analytical approach of tables for treating asthma according to claim 1, it is characterized in that: the analytical approach of described tables for treating asthma comprises:
Differentiate:
(1), get 15 of tables for treating asthma finished products, porphyrize adds 20 of strong ammonia solutions, adds chloroform 10ml again, reflux 1 hour filters, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Thin-layered chromatography test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, in with the pre-saturated expansion cylinder of dense ammonia test, be developping agent with toluene-chloroform-methanols of 5: 20: 2, launch, take out, dry, spray is with ninhydrin solution, and 105 ℃ to be heated to spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2), get 15 of tables for treating asthma finished products, porphyrize adds chloroform 20ml, reflux 30 minutes filters, filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Get fruit of Chinese magnoliavine control medicinal material 1g and shine medicinal material solution in pairs with legal system; Get the schizandrin A reference substance again, chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned three kinds of solution, put in same silica G F respectively
254On the thin layer plate, be developping agent, launch, take out, dry, put under the uviol lamp of 254nm and inspect with toluene-ethyl acetate of 9: 1; In the test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color;
(3), get 20 of this product, porphyrize, the hydrochloric acid ethanol solution 30ml of adding 10%, water-bath reflux 30 minutes, taking-up, put coldly, filter, filtrate adds water 45ml, with chloroform extraction 2 times, and each 30ml, combined chloroform liquid, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets polygala root control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; Thin-layered chromatography test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B record, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 15: 3: 0.3: chloroform-acetone of 0.5-normal hexane-acetate was developping agent, launch, take out, dry, spray is mixed with the solution that forms with the ethanol solution of sulfuric acid of 8% vanillic aldehyde ethanol solution and 70% in 1: 10 ratio, 105 ℃ are dried by the fire to clear spot, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical pansy spot;
Assay:
Get the tables for treating asthma finished product under the weight differential item, porphyrize is got 1.0g, and accurate the title decides, put in the 50ml tool plug conical flask, accurate adding strong ammonia solution 1ml makes moistening, and the accurate again 25ml methylene chloride that adds claims to decide weight, sonicated 30 minutes, put coldly, claim to decide weight, supply the weight that subtracts mistake with methylene chloride, filter, get subsequent filtrate 10ml, put in the 25ml evaporating dish, add 5% the ethanol solution hydrochloride of 1ml, the low temperature evaporate to dryness, residue adds 5% ethanol solution hydrochloride makes dissolving in right amount, is transferred in the 25ml volumetric flask, adds 0.1mol/L HCl solution washing container and is diluted to scale, shake up, with the aperture is the miillpore filter filtration of 0.45 μ m, gets subsequent filtrate, promptly gets for test agent solution; It is an amount of that precision takes by weighing the ephedrine hydrochloride reference substance, adds 0.1mol/L HCl solution and make the solution that every 1ml contains 10 μ g, promptly gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, are filling agent with octadecylsilane chemically bonded silica; Is moving phase with the 0.02mol/L potassium dihydrogen phosphate that contains 0.1% triethylamine and 0.1% phosphoric acid and acetonitrile with 95: 5 ratio; The detection wavelength is 207nm; Theoretical cam curve is calculated by the ephedrine hydrochloride peak should be not less than 3000, measures, promptly;
This product contains Chinese ephedra with ephedrine hydrochloride C
10H
15NOHCl calculates, and every setting value is more than or equal to 0.2mg.
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| CN102697959B (en) * | 2012-05-08 | 2014-06-04 | 广州市和生堂动物药业有限公司 | Veterinary drug of traditional Chinese veterinary drug for preventing and treating porcine respiratory disease syndrome |
| CN104777265B (en) * | 2015-04-24 | 2016-06-08 | 四川逢春制药有限公司 | The detection method of a kind of FUFANG CHUANBEIJING sheet |
| CN104777264B (en) * | 2015-04-24 | 2016-04-06 | 九寨沟天然药业集团有限责任公司 | The detection method of Chinese medicine preparation compound tablet of fritillary bulb |
| CN111735900B (en) * | 2020-07-01 | 2022-03-01 | 清华德人西安幸福制药有限公司 | Method for detecting effective components in Wuling capsules |
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