CN101890095A - Method for controlling quality of dioxopromethazine tablets - Google Patents
Method for controlling quality of dioxopromethazine tablets Download PDFInfo
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- CN101890095A CN101890095A CN2009100397246A CN200910039724A CN101890095A CN 101890095 A CN101890095 A CN 101890095A CN 2009100397246 A CN2009100397246 A CN 2009100397246A CN 200910039724 A CN200910039724 A CN 200910039724A CN 101890095 A CN101890095 A CN 101890095A
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Abstract
The invention discloses a method for controlling the quality of dioxopromethazine tablets, which controls the content of three main active ingredients including Chinese ephedra, liquorice and poppy capsule according to a higher standard at the same time by the following five steps of determining the content of ephedrine hydrochloride and pseudoephedrinehydrochloride by using high performance liquid chromatography (HPLC), determining morphine content by using the HPLC, identifying an ephedrine hydrochloride film, identifying a poppy capsule film and identifying a glycyrrhetinic acid film. Thus, the high quality of the dioxopromethazine tablets is guaranteed.
Description
[technical field]
The present invention relates to a kind of method of quality control of cough-relieving tablets.
[background technology]
Cough-relieving tablets is made up of Chinese medicine Herba Ephedrae, Pericarpium Papaveris, Radix Glycyrrhizae, Semen Armeniacae Amarum, Radix Platycodonis, Semen Raphani, Gypsum Fibrosum, wherein preceding four flavors are MAXINGSHIGAN TANG, originally be the good recipe of treatment lung-heat excess-dyspnea, by the modern science processes, " make mutually with material, abnormal smells from the patient is in harmony mutually ", change its original intention, deposit it and become second nature, thereby widened the scope of application; Radix Platycodonis is opened the sharp key of lung, and the evacuation of pus of eliminating the phlegm is the special medicine of " removing food stagnancy gathers sputum "; Pericarpium Papaveris nature and flavor acid is flat, the solid and gas of astringing the lung, Compendium of Material Medica cloud " all diseases of coughing were both of a specified duration, and not receive the pulmonary distension pain acute and then gas looses ", thus at " root of preventing or cure a disease " afterwards, when should with its puckery it, admittedly it, receive it, hold back it; Pericarpium Papaveris compatibility Herba Ephedrae again, a surname one holds back, and opens the harmony of pathogen and holds back, the dissipation of convergence lung; Pericarpium Papaveris and Radix Glycyrrhizae compatibility then have the magical effect of sour and sweet drugs can transforme into YIN; All medicines share the effect of playing cough-relieving altogether, relieving asthma, eliminating the phlegm; Clinical practice and observe to confirm KEKE JIAONANG to respiratory system commonly encountered diseases, the caused cough of frequently-occurring disease, cough up phlegm, symptoms such as asthma, uncomfortable in chest, chest pain, itching throat all have tangible curative effect, especially to cough, expectorant, to breathe heavily three primary symptom effects remarkable.
Ephedrine hydrochloride, pseudoephedrine hydrochloride, morphine are the main component of anesthesia cough-relieving in the cough-relieving tablets; Ephedrine hydrochloride and pseudoephedrine hydrochloride can directly act on two kinds of receptors of α, β, the effect of performance adrenomimetic drug, also can impel the adrenergic nerve tip to discharge chemical mediator, bring into play the adrenomimetic drug effect indirectly, with epinephrine relatively, to bronchial smooth muscle influence ephedrine to the relexation of bronchial smooth muscle than epinephrine a little less than and lasting; Morphine can suppress the activity of brain respiratory center and coughing centre, breathing is slowed down and produce suppression to cough effect; The present invention is the deficiency that overcomes existing method of quality control, improve the quality control standard of cough-relieving tablets, when the thin layer chromatography of three flavor principal agent Herba Ephedraes, Radix Glycyrrhizae, Pericarpium Papaveris is differentiated in having guaranteed preparation, control above-mentioned 3 kinds of main content of effective simultaneously with higher standard, thereby guaranteed this preparation higher quality control level.
[summary of the invention]
The objective of the invention is to overcome the deficiencies in the prior art part, provide a kind of by effective process 3 kinds of main content of effective of three flavor principal agent Herba Ephedraes, Radix Glycyrrhizae, Pericarpium Papaveris in the preparation are controlled simultaneously with higher standard, thereby guaranteed that cough-relieving tablets has the method for quality control of better quality.
The object of the present invention is achieved like this:
A kind of method of quality control of cough-relieving tablets, described by weight cough-relieving tablets is made by following medical material: the Chinese crude drug Herba Ephedrae
Part, Pericarpium Papaveris
Part, Radix Glycyrrhizae
Part, Semen Armeniacae Amarum
Part, Radix Platycodonis
Part, Semen Raphani
Part, Gypsum Fibrosum
Part, it is characterized in that this method comprises the following steps:
(1) with the content of measuring ephedrine hydrochloride and pseudoephedrine hydrochloride in the HPLC method while cough-relieving tablets:
A, chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With the proportioning is 5-10: 100 acetonitrile-0.02mol/l potassium dihydrogen phosphate (transferring pH1-5) is mobile phase; The detection wavelength is 210 ± 2nm;
The preparation of b, reference substance solution: get the ephedrine hydrochloride reference substance respectively and the pseudoephedrine hydrochloride reference substance is an amount of, the accurate title, decide, add 0.1% hydrochloric acid methanol and make the mixing reference substance solution of the hydrochloric ephedrine 0.05-1.00mg of every 1ml, pseudoephedrine hydrochloride 10-100 μ g, promptly;
The preparation of c, need testing solution: sample thief, porphyrize, mixing, get about 0.1-5g, the accurate title, decide, and puts in the tool plug conical flask, add strong ammonia solution 0.5-5ml, fully moistening, precision adds chloroform 20-100ml, claims to decide weight, supersound process 20-50 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with chloroform, shake up, filter, precision is measured subsequent filtrate 10-50ml, evaporate to dryness, residue adds 0.1% dilute hydrochloric acid methanol solution makes dissolving in right amount, be transferred in the measuring bottle and be diluted to scale, shake up, promptly;
D, assay method: accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, per unit preparation contain Herba Ephedrae in ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C10H15NOHCl) total amount, must not be less than 0.5mg;
(2) use the HPLC method to measure the content of morphine in the cough-relieving tablets:
A, chromatographic condition: with octyl silane group silica gel is filler; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (30-50: 20-40: 20-40) be mobile phase; The detection wavelength is 220 ± 2nm;
The preparation of b, reference substance solution: it is an amount of that precision takes by weighing the morphine reference substance, adds the methanol solution that contains 5% acetic acid and make the solution that every 1ml contains 20-80 μ g, promptly;
The preparation of c, need testing solution: sample thief, porphyrize is got powder 0.2-2g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol solution 10-100ml that contains acetic acid that adds, close plug claims to decide weight, supersound process 20-50 minute, put coldly, claim decide weight again, usefulness contains acetate methanol solution and supplies the weight that subtracts mistake, shake up, filter, get subsequent filtrate, promptly;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, whenever take unit formulation and contain Pericarpium Papaveris with morphine (C17H19O
3N) meter must not be less than 0.2mg;
(3) thin layer of ephedrine hydrochloride is differentiated in the cough-relieving tablets:
The preparation of a, reference substance solution: get the ephedrine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 2mg, make reference substance solution;
The preparation of b, need testing solution: it is an amount of to get this product, and porphyrize adds ammonia solution number droplet, mixes thoroughly, add the chloroform merceration and spend the night, filter, filtrate is put in the separatory funnel, extracts 1-2 time with the hydrochloric acid solution jolting, divide and get the sour water layer, evaporate to dryness, residue add methanol makes dissolving, makes test sample solution;
C, thin layer chromatography are differentiated: draw need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-strong ammonia solution (50-150: 10-30: 0.5-5) be developing solvent, launch, take out, dry, spray is with 0.3% 1,2,3-indantrione monohydrate butanol solution-acetic acid mixed solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(4) thin layer of Pericarpium Papaveris is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get Pericarpium Papaveris control medicinal material 1g, it is an amount of to add methanol, and heating and refluxing extraction filters, the filtrate evaporate to dryness, and residue adds dissolve with methanol, makes control medicinal material solution;
The preparation of b, need testing solution: sample thief is an amount of, and porphyrize adds ammonia solution number droplet, mixes thoroughly, add chloroform reagent merceration and spend the night, filter, filtrate is put in the separatory funnel, extracts 1-2 time with the hydrochloric acid solution jolting, divide and get the sour water layer, evaporate to dryness, residue adds dissolve with methanol, makes test sample solution;
C, thin layer are differentiated: draw control medicinal material solution and need testing solution, put respectively on same alkaline silica gel G lamellae, with toluene-acetone-ethanol-strong ammonia solution (10-30: 10-30: 1-5: 0.5-5) be developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(5) thin layer of enoxolone is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: extracting liquorice subacid reference substance adds ethanol and makes control medicinal material solution in right amount;
The preparation of b, need testing solution: sample thief is an amount of, and porphyrize adds mineral acid and chloroform for extracting reagent, and heating and refluxing extraction is put coldly, filters, and filtrate evaporate to dryness, residue add ethanol makes dissolving, makes need testing solution;
C, thin layer are differentiated: draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether-toluene-ethyl acetate-glacial acetic acid (5-20: 10-30: 2-15: 0.5-5) be developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating colour developings; 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 aforesaid a kind of cough-relieving tablets, described by weight cough-relieving tablets is made by following medical material: 3.2 parts in Chinese crude drug Herba Ephedrae, 3.2 parts of Pericarpium Papaveriss, 3.2 parts in Radix Glycyrrhizae, 3.2 parts of Semen Armeniacae Amarums, 1 part of Radix Platycodonis, 1 part of Semen Raphani, 1 part in Gypsum Fibrosum; It is characterized in that this method comprises the following steps:
(1) measure the content of ephedrine hydrochloride and pseudoephedrine hydrochloride in the cough-relieving tablets simultaneously with the HPLC method:
A, chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With proportioning is that acetonitrile-0.02mol/l potassium dihydrogen phosphate (transfer pH3.0) of 5: 100 is a mobile phase; The detection wavelength is 210nm;
The preparation of b, reference substance solution: get the ephedrine hydrochloride reference substance respectively and the pseudoephedrine hydrochloride reference substance is an amount of, the accurate title, decide, add 0.1% hydrochloric acid methanol and make the mixing reference substance solution of the hydrochloric ephedrine 0.1mg of every 1ml, pseudoephedrine hydrochloride 40 μ g, promptly;
The preparation of c, need testing solution: get 20 of this product, the accurate title, decided porphyrize, mixing is got about 0.6g, and accurate the title decides, put in the tool plug conical flask, add strong ammonia solution 2ml, jolting makes abundant moistening, precision adds chloroform 50ml, claims to decide weight, supersound process 30 minutes, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with chloroform, filter, precision is measured subsequent filtrate 25ml, adds 0.1% methanol hydrochloride solution 2ml, evaporate to dryness, residue adds 0.1% methanol hydrochloride solution makes dissolving in right amount, be transferred in the 10ml measuring bottle and be diluted to scale, shake up, promptly;
D, assay method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, every of this product contain Herba Ephedrae in ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C10H15NOHCl) total amount, must not be less than 0.5mg;
(2) use the HPLC method to measure the content of morphine in the cough-relieving tablets:
A, chromatographic condition: with octyl silane group silica gel is filler; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (40: 30: 30) is mobile phase; The detection wavelength is 220nm;
The preparation of b, reference substance solution: it is an amount of that precision takes by weighing the morphine reference substance, adds 20% methanol solution that contains 5% acetic acid and make the solution that every 1ml contains 40 μ g, promptly;
The preparation of c, need testing solution: get 10 of this product, remove coating, the accurate title, decided porphyrize, get the about 0.75g of powder, the accurate title, decide, and puts in the tool plug conical flask, the accurate 20% methanol solution 25ml that contains 5% acetic acid that adds, close plug claims to decide weight, supersound process (power 250W, frequency 40kHz) 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake, shake up with 20% methanol solution that contains 5% acetic acid, filter, get subsequent filtrate, promptly;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, whenever take unit formulation and contain Pericarpium Papaveris with morphine (C17H19O
3N) meter must not be less than 0.2mg;
(3) thin layer of ephedrine hydrochloride is differentiated in the cough-relieving tablets:
The preparation of a, reference substance solution: get the ephedrine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 2mg, make reference substance solution;
The preparation of b, need testing solution: get 6 of this product, remove coating, porphyrize, add ammonia solution number droplet, mix thoroughly, add chloroform 20ml, merceration spends the night, and filters, and filtrate is put in the separatory funnel, extract 2 (10ml with hydrochloric acid (3 → 10) solution jolting, 10ml), branch is got sour water layer, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution;
C, thin layer chromatography are differentiated: draw need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-strong ammonia solution (100: 20: 1) is developing solvent, launch, take out, dry, spray is with 0.3% 1,2,3-indantrione monohydrate butanol solution-acetic acid (19: 1) mixed solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(4) thin layer of Pericarpium Papaveris is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get Pericarpium Papaveris control medicinal material 1g, add methanol 20ml, reflux 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution;
The preparation of b, need testing solution: get 6 of this product, remove coating, porphyrize, add ammonia solution number droplet, mix thoroughly, add chloroform 20ml, merceration spends the night, and filters, and filtrate is put in the separatory funnel, extract 2 (10ml with hydrochloric acid (3 → 10) solution jolting, 10ml), branch is got sour water layer, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution;
C, thin layer are differentiated: draw control medicinal material solution and each 10ul of need testing solution, put respectively on the silica gel g thin-layer plate of same usefulness 2% sodium hydroxide solution preparation, with toluene-acetone-ethanol-strong ammonia solution (20: 20: 3: 1) be developing solvent, 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 speckle of same color;
(5) thin layer of enoxolone is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: extracting liquorice subacid reference substance adds ethanol and makes the solution that every 1ml contains 2mg, in contrast product solution;
The preparation of b, need testing solution: get 4 of this product, remove coating, porphyrize adds hydrochloric acid 1ml and chloroform 20ml, puts in the water-bath reflux 1 hour, puts coldly, filters, and filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution;
C, thin layer differentiate: draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30～60 ℃)-toluene-ethyl acetate-glacial acetic acid (10: 20: 7: 0.5) be developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
The present invention adopts the HPLC method to measure the content of ephedrine hydrochloride and pseudoephedrine hydrochloride simultaneously; Measure the content of morphine with the HPLC method; The thin layer of ephedrine hydrochloride is differentiated; The thin layer of Pericarpium Papaveris is differentiated; Five kinds of processing steps of thin layer discriminating of enoxolone are controlled with higher standard simultaneously to 3 kinds of main content of effective of three flavor principal agent Herba Ephedraes, Radix Glycyrrhizae, Pericarpium Papaveris, thereby have guaranteed that cough-relieving tablets has higher quality.
[specific embodiment]
Embodiment 1: described by weight cough-relieving tablets is made by following medical material: the Chinese crude drug Herba Ephedrae
Part, Pericarpium Papaveris
Part, Radix Glycyrrhizae
Part, Semen Armeniacae Amarum
Part, Radix Platycodonis
Part, Semen Raphani
Part, Gypsum Fibrosum
Part; Above-mentioned raw materials seven flavors, Herba Ephedrae and Pericarpium Papaveris are ground into fine powder, sieve, stay fine powder standby, the residue coarse powder decocts secondary, each 2 hours with acidic aqueous solution (with about 10% hydrochloric acid solution adjust pH to 5), filter, filtrate is with 10% sodium hydroxide solution adjust pH to 7, and medicinal liquid is standby; The five tastes such as all the other Radix Glycyrrhizaes decoct with water secondary, and each 1 hour, filter, filtrate and above-mentioned solution merge, and are concentrated into the thick paste shape, add Herba Ephedrae and Pericarpium Papaveris fine powder, and mixing 60～70 ℃ of dryings, is ground into fine powder, adds adjuvant, tablet forming.Get cough-relieving tablets, detect by following condition:
(1) measure the content of ephedrine hydrochloride and pseudoephedrine hydrochloride in the cough-relieving tablets simultaneously with HPLC method (high performance liquid chromatography):
A, chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-0.02mol/l potassium dihydrogen phosphate (transferring pH to 2.7) (5: 100) is mobile phase; The detection wavelength is 208nm.Number of theoretical plate calculates by the ephedrine hydrochloride peak should be not less than 3000.
The preparation of b, reference substance solution: get the ephedrine hydrochloride reference substance respectively and the pseudoephedrine hydrochloride reference substance is an amount of, the accurate title, decide, add 0.1% hydrochloric acid methanol and make the mixing reference substance solution of the hydrochloric ephedrine 0.05mg of every 1ml, pseudoephedrine hydrochloride 10 μ g, promptly;
The preparation of c, need testing solution: get 20 of this product, the accurate title, decide, porphyrize, and mixing gets about 0.1
G, the accurate title, decide, and puts in the tool plug conical flask, adds strong ammonia solution 0.5, fully moistening, precision adds chloroform 20ml, claims to decide weight, supersound process 20 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with chloroform, shake up, filter, precision is measured subsequent filtrate 10ml, and evaporate to dryness, residue add 0.1% dilute hydrochloric acid methanol solution makes dissolving in right amount, be transferred in the measuring bottle and be diluted to scale, shake up, promptly;
D, assay method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, per unit preparation contain Herba Ephedrae with ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C
10H15NOHCl) total amount meter must not be less than 0.5mg;
(2) use the HPLC method to measure the content of morphine in the cough-relieving tablets:
A, chromatographic condition: with octyl silane group silica gel is filler; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (30: 20: 20) is mobile phase; The detection wavelength is 218nm;
The preparation of b, reference substance solution: it is an amount of that precision takes by weighing the morphine reference substance, adds the methanol solution that contains 5% acetic acid and make the solution that every 1ml contains 20 μ g, promptly;
The preparation of c, need testing solution: get 10 of this product, remove coating, the accurate title, decide, porphyrize is got powder 0.2g, and accurate the title decides, put in the tool plug conical flask the accurate methanol solution 10ml that contains acetic acid, the close plug of adding, claim to decide weight, supersound process 20 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake, shake up with containing acetate methanol solution, filter, get subsequent filtrate, promptly;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, whenever take unit formulation and contain Pericarpium Papaveris with morphine (C17H19O
3N) meter must not be less than 0.2mg;
(3) thin layer of ephedrine hydrochloride is differentiated in the cough-relieving tablets:
The preparation of a, reference substance solution: get the ephedrine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 2mg, make reference substance solution;
The preparation of b, need testing solution: get 6 of this product, remove coating, porphyrize adds ammonia solution number droplet, mixes thoroughly, add the chloroform merceration and spend the night, filter, filtrate is put in the separatory funnel, extracts 1 time with the hydrochloric acid solution jolting, divide and get the sour water layer, evaporate to dryness, residue add methanol makes dissolving, makes test sample solution;
C, thin layer chromatography are differentiated: draw need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-strong ammonia solution (50: 10: 0.5) is developing solvent, launch, take out, dry, spray is with 0.3% 1,2,3-indantrione monohydrate butanol solution-acetic acid mixed solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(4) thin layer of Pericarpium Papaveris is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get Pericarpium Papaveris control medicinal material 1g, it is an amount of to add methanol, and heating and refluxing extraction filters, the filtrate evaporate to dryness, and residue adds dissolve with methanol, makes control medicinal material solution;
The preparation of b, need testing solution: get 6 of this product, remove coating, porphyrize adds ammonia solution number droplet, mixes thoroughly, add chloroform reagent merceration and spend the night, filter, filtrate is put in the separatory funnel, extracts 1 time with the hydrochloric acid solution jolting, divide and get the sour water layer, evaporate to dryness, residue adds dissolve with methanol, makes test sample solution;
C, thin layer are differentiated: draw control medicinal material solution and need testing solution, put respectively on same alkaline silica gel G lamellae, with toluene-acetone-ethanol-strong ammonia solution (10: 10: 1: 0.5) be developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(5) thin layer of enoxolone is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: extracting liquorice subacid reference substance adds ethanol and makes control medicinal material solution in right amount;
The preparation of b, need testing solution: get 4 of this product, remove coating, porphyrize adds mineral acid and chloroform for extracting reagent, and heating and refluxing extraction is put coldly, filters, and filtrate evaporate to dryness, residue add ethanol makes dissolving, makes need testing solution;
C, thin layer differentiate: draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether-toluene-ethyl acetate-glacial acetic acid (5: 10: 2: 0.5) be developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 2: cough-relieving tablets is made by following medical material by weight: the Chinese crude drug Herba Ephedrae
Part, Pericarpium Papaveris
Part, Radix Glycyrrhizae
Part, Semen Armeniacae Amarum
Part, 1 part of Radix Platycodonis, 1 part of Semen Raphani, 1 part in Gypsum Fibrosum.Above-mentioned raw materials seven flavors, Herba Ephedrae and Pericarpium Papaveris are ground into fine powder, sieve, stay fine powder standby, the residue coarse powder decocts secondary, each 2 hours with acidic aqueous solution (with about 10% hydrochloric acid solution adjust pH to 5), filter, filtrate is with 10% sodium hydroxide solution adjust pH to 7, and medicinal liquid is standby; The five tastes such as all the other Radix Glycyrrhizaes decoct with water secondary, and each 1 hour, filter, filtrate and above-mentioned solution merge, and are concentrated into the thick paste shape, add Herba Ephedrae and Pericarpium Papaveris fine powder, and mixing 60～70 ℃ of dryings, is ground into fine powder, adds adjuvant, tablet forming.Get cough-relieving tablets, detect by following condition:
(1) measure the content of ephedrine hydrochloride and pseudoephedrine hydrochloride in the cough-relieving tablets simultaneously with the HPLC method:
A, chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With proportioning is that acetonitrile-0.02mol/l potassium dihydrogen phosphate (transfer pH to 5) of 10: 100 is a mobile phase; The detection wavelength is 212nm;
The preparation of b, reference substance solution: get the ephedrine hydrochloride reference substance respectively and the pseudoephedrine hydrochloride reference substance is an amount of, the accurate title, decide, add 0.1% hydrochloric acid methanol and make the mixing reference substance solution of the hydrochloric ephedrine 1.00mg of every 1ml, pseudoephedrine hydrochloride 100 μ g, promptly;
The preparation of c, need testing solution: get 20 of this product, the accurate title, decide, porphyrize, and mixing,, get about 5
G, the accurate title, decide, and puts in the tool plug conical flask, adds strong ammonia solution 5ml, fully moistening, precision adds chloroform 100ml, claims to decide weight, supersound process 50 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with chloroform, shake up, filter, precision is measured subsequent filtrate 50ml, and evaporate to dryness, residue add 0.1% dilute hydrochloric acid methanol solution makes dissolving in right amount, be transferred in the measuring bottle and be diluted to scale, shake up, promptly;
D, assay method: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, per unit preparation contain Herba Ephedrae in ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C10H15NOHCl) total amount, must not be less than 0.5mg;
(2) use the HPLC method to measure the content of morphine in the cough-relieving tablets:
A, chromatographic condition: with octyl silane group silica gel is filler; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (50: 40: 40) is mobile phase; The detection wavelength is 222nm;
The preparation of b, reference substance solution: it is an amount of that precision takes by weighing the morphine reference substance, adds the methanol solution that contains 5% acetic acid and make the solution that every 1ml contains 80 μ g, promptly;
The preparation of c, need testing solution: get 10 of this product, remove coating, the accurate title, decide, porphyrize is got powder 2g, and accurate the title decides, put in the tool plug conical flask the accurate methanol solution 100ml that contains acetic acid, the close plug of adding, claim to decide weight, supersound process 50 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake, shake up with containing acetate methanol solution, filter, get subsequent filtrate, promptly;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, whenever take unit formulation and contain Pericarpium Papaveris with morphine (C17H19O
3N) meter must not be less than 0.2mg;
(3) thin layer of ephedrine hydrochloride is differentiated in the cough-relieving tablets:
The preparation of a, reference substance solution: get the ephedrine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 2mg, make reference substance solution;
The preparation of b, need testing solution: get 6 of this product, remove coating, porphyrize adds ammonia solution number droplet, mixes thoroughly, add the chloroform merceration and spend the night, filter, filtrate is put in the separatory funnel, extracts 2 times with the hydrochloric acid solution jolting, divide and get the sour water layer, evaporate to dryness, residue add methanol makes dissolving, makes test sample solution;
C, thin layer chromatography are differentiated: draw need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-strong ammonia solution (150: 30: 5) is developing solvent, launch, take out, dry, spray is with 0.3% 1,2,3-indantrione monohydrate butanol solution-acetic acid mixed solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(4) thin layer of Pericarpium Papaveris is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get Pericarpium Papaveris control medicinal material 1g, it is an amount of to add methanol, and heating and refluxing extraction filters, the filtrate evaporate to dryness, and residue adds dissolve with methanol, makes control medicinal material solution;
The preparation of b, need testing solution: get 6 of this product, remove coating, porphyrize adds ammonia solution number droplet, mixes thoroughly, add chloroform reagent merceration and spend the night, filter, filtrate is put in the separatory funnel, extracts 2 times with the hydrochloric acid solution jolting, divide and get the sour water layer, evaporate to dryness, residue adds dissolve with methanol, makes test sample solution;
C, thin layer are differentiated: draw control medicinal material solution and need testing solution, put respectively on same alkaline silica gel G lamellae, with toluene-acetone-ethanol-strong ammonia solution (30: 30: 5: 5) be developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(5) thin layer of enoxolone is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: extracting liquorice subacid reference substance adds ethanol and makes control medicinal material solution in right amount;
The preparation of b, need testing solution: get 4 of this product, remove coating, porphyrize adds mineral acid and chloroform for extracting reagent, and heating and refluxing extraction is put coldly, filters, and filtrate evaporate to dryness, residue add ethanol makes dissolving, makes need testing solution;
C, thin layer differentiate: draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether-toluene-ethyl acetate-glacial acetic acid (20: 30: 15: 5) be developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 3: cough-relieving tablets is made by following medical material by weight: the Chinese crude drug Herba Ephedrae
Part, Pericarpium Papaveris
Part, Radix Glycyrrhizae
Part, Semen Armeniacae Amarum
Part, Radix Platycodonis
Part, Semen Raphani
Part, Gypsum Fibrosum
Part.Above-mentioned raw materials seven flavors, Herba Ephedrae and Pericarpium Papaveris are ground into fine powder, sieve, stay fine powder standby, the residue coarse powder decocts secondary, each 2 hours with acidic aqueous solution (with about 10% hydrochloric acid solution adjust pH to 5), filter, filtrate is with 10% sodium hydroxide solution adjust pH to 7, and medicinal liquid is standby; The five tastes such as all the other Radix Glycyrrhizaes decoct with water secondary, and each 1 hour, filter, filtrate and above-mentioned solution merge, and are concentrated into the thick paste shape, add Herba Ephedrae and Pericarpium Papaveris fine powder, and mixing 60～70 ℃ of dryings, is ground into fine powder, adds adjuvant, tablet forming.Get cough-relieving tablets, detect by following condition:
(1) the HPLC method is measured the content of ephedrine hydrochloride and pseudoephedrine hydrochloride in the cough-relieving tablets simultaneously:
A, chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With the proportioning is 5-10: 100 acetonitrile-0.02mol/l potassium dihydrogen phosphate (transferring pH to 3) is mobile phase; The detection wavelength is 2l0nm;
The preparation of b, reference substance solution: get the ephedrine hydrochloride reference substance respectively and the pseudoephedrine hydrochloride reference substance is an amount of, the accurate title, decide, add 0.1% hydrochloric acid methanol and make the mixing reference substance solution of the hydrochloric ephedrine 0.75mg of every 1ml, pseudoephedrine hydrochloride 50 μ g, promptly;
The preparation of c, need testing solution: get 20 of this product, the accurate title, decide, porphyrize, and mixing gets about 2.5
G, the accurate title, decide, and puts in the tool plug conical flask, adds strong ammonia solution 2.7ml, fully moistening, precision adds chloroform 60ml, claims to decide weight, supersound process 35 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with chloroform, shake up, filter, precision is measured subsequent filtrate 30ml, and evaporate to dryness, residue add 0.1% dilute hydrochloric acid methanol solution makes dissolving in right amount, be transferred in the measuring bottle and be diluted to scale, shake up, promptly;
D, assay method: accurate respectively reference substance solution and each 12 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, per unit preparation contain Herba Ephedrae in ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C10H15NOHCl) total amount, must not be less than 0.5mg;
(2) the HPLC method is measured the content of morphine in the cough-relieving tablets:
A, chromatographic condition: with octyl silane group silica gel is filler; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (40: 30: 30) is mobile phase; The detection wavelength is 220nm;
The preparation of b, reference substance solution: it is an amount of that precision takes by weighing the morphine reference substance, adds the methanol solution that contains 5% acetic acid and make the solution that every 1ml contains 50 μ g, promptly;
The preparation of c, need testing solution: get 10 of this product, remove coating, the accurate title, decide, porphyrize is got powder 1.1g, and accurate the title decides, put in the tool plug conical flask the accurate methanol solution 50ml that contains acetic acid, the close plug of adding, claim to decide weight, supersound process 35 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake, shake up with containing acetate methanol solution, filter, get subsequent filtrate, promptly;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 12 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, whenever take unit formulation and contain Pericarpium Papaveris with morphine (C17H19O
3N) meter must not be less than 0.2mg;
(3) thin layer of ephedrine hydrochloride is differentiated in the cough-relieving tablets:
The preparation of a, reference substance solution: get the ephedrine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 2mg, make reference substance solution;
The preparation of b, need testing solution: get 6 of this product, remove coating, porphyrize adds ammonia solution number droplet, mixes thoroughly, add the chloroform merceration and spend the night, filter, filtrate is put in the separatory funnel, extracts 1.5 times with the hydrochloric acid solution jolting, divide and get the sour water layer, evaporate to dryness, residue add methanol makes dissolving, makes test sample solution;
C, thin layer chromatography are differentiated: draw need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-strong ammonia solution (100: 20: 3) is developing solvent, launch, take out, dry, spray is with 0.3% 1,2,3-indantrione monohydrate butanol solution-acetic acid mixed solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(4) thin layer of Pericarpium Papaveris is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get Pericarpium Papaveris control medicinal material 1g, it is an amount of to add methanol, and heating and refluxing extraction filters, the filtrate evaporate to dryness, and residue adds dissolve with methanol, makes control medicinal material solution;
The preparation of b, need testing solution: get 6 of this product, remove coating, porphyrize adds ammonia solution number droplet, mixes thoroughly, add chloroform reagent merceration and spend the night, filter, filtrate is put in the separatory funnel, extracts 1.5 times with the hydrochloric acid solution jolting, divide and get the sour water layer, evaporate to dryness, residue adds dissolve with methanol, makes test sample solution;
C, thin layer are differentiated: draw control medicinal material solution and need testing solution, put respectively on same alkaline silica gel G lamellae, with toluene-acetone-ethanol-strong ammonia solution (20: 20: 3: 3) be developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(5) thin layer of enoxolone is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: extracting liquorice subacid reference substance adds ethanol and makes control medicinal material solution in right amount;
The preparation of b, need testing solution: get 4 of this product, remove coating, porphyrize adds mineral acid and chloroform for extracting reagent, and heating and refluxing extraction is put coldly, filters, and filtrate evaporate to dryness, residue add ethanol makes dissolving, makes need testing solution;
C, thin layer differentiate: draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether-toluene-ethyl acetate-glacial acetic acid (12: 20: 8: 3) be developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Claims (2)
1. the method for quality control of a cough-relieving tablets, described by weight cough-relieving tablets is made by following medical material: the Chinese crude drug Herba Ephedrae
Part, Pericarpium Papaveris
Part, Radix Glycyrrhizae
Part, Semen Armeniacae Amarum
Part, Radix Platycodonis
Part, Semen Raphani
Part, Gypsum Fibrosum
Part, it is characterized in that this method comprises the following steps:
(1) with the content of measuring ephedrine hydrochloride and pseudoephedrine hydrochloride in the HPLC method while cough-relieving tablets:
A, chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With the proportioning is 5-10: 100 acetonitrile-0.02mol/l potassium dihydrogen phosphate (transferring pH1-5) is mobile phase; The detection wavelength is 210 ± 2nm;
The preparation of b, reference substance solution: get the ephedrine hydrochloride reference substance respectively and the pseudoephedrine hydrochloride reference substance is an amount of, the accurate title, decide, add 0.1% hydrochloric acid methanol and make the mixing reference substance solution of the hydrochloric ephedrine 0.05-1.00mg of every 1ml, pseudoephedrine hydrochloride 10-100 μ g, promptly;
The preparation of c, need testing solution: sample thief, porphyrize, mixing, get about 0.1-5g, the accurate title, decide, and puts in the tool plug conical flask, add strong ammonia solution 0.5-5ml, fully moistening, precision adds chloroform 20-100ml, claims to decide weight, supersound process 20-50 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with chloroform, shake up, filter, precision is measured subsequent filtrate 10-50ml, evaporate to dryness, residue adds 0.1% dilute hydrochloric acid methanol solution makes dissolving in right amount, be transferred in the measuring bottle and be diluted to scale, shake up, promptly;
D, assay method: accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, per unit preparation contain Herba Ephedrae in ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C10H15NOHCl) total amount, must not be less than 0.5mg;
(2) use the HPLC method to measure the content of morphine in the cough-relieving tablets:
A, chromatographic condition: with octyl silane group silica gel is filler; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (30-50: 20-40: 20-40) be mobile phase; The detection wavelength is 220 ± 2nm;
The preparation of b, reference substance solution: it is an amount of that precision takes by weighing the morphine reference substance, adds the methanol solution that contains 5% acetic acid and make the solution that every 1ml contains 20-80 μ g, promptly;
The preparation of c, need testing solution: sample thief, porphyrize is got powder 0.2-2g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol solution 10-100ml that contains acetic acid that adds, close plug claims to decide weight, supersound process 20-50 minute, put coldly, claim decide weight again, usefulness contains acetate methanol solution and supplies the weight that subtracts mistake, shake up, filter, get subsequent filtrate, promptly;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, whenever take unit formulation and contain Pericarpium Papaveris with morphine (C17H19O
3N) meter must not be less than 0.2mg;
(3) thin layer of ephedrine hydrochloride is differentiated in the cough-relieving tablets:
The preparation of a, reference substance solution: get the ephedrine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 2mg, make reference substance solution;
The preparation of b, need testing solution: it is an amount of to get this product, and porphyrize adds ammonia solution number droplet, mixes thoroughly, add the chloroform merceration and spend the night, filter, filtrate is put in the separatory funnel, extracts 1-2 time with the hydrochloric acid solution jolting, divide and get the sour water layer, evaporate to dryness, residue add methanol makes dissolving, makes test sample solution;
C, thin layer chromatography are differentiated: draw need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-strong ammonia solution (50-150: 10-30: 0.5-5) be developing solvent, launch, take out, dry, spray is with 0.3% 1,2,3-indantrione monohydrate butanol solution-acetic acid mixed solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(4) thin layer of Pericarpium Papaveris is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get Pericarpium Papaveris control medicinal material 1g, it is an amount of to add methanol, and heating and refluxing extraction filters, the filtrate evaporate to dryness, and residue adds dissolve with methanol, makes control medicinal material solution;
The preparation of b, need testing solution: sample thief is an amount of, and porphyrize adds ammonia solution number droplet, mixes thoroughly, add chloroform reagent merceration and spend the night, filter, filtrate is put in the separatory funnel, extracts 1-2 time with the hydrochloric acid solution jolting, divide and get the sour water layer, evaporate to dryness, residue adds dissolve with methanol, makes test sample solution;
C, thin layer are differentiated: draw control medicinal material solution and need testing solution, put respectively on same alkaline silica gel G lamellae, with toluene-acetone-ethanol-strong ammonia solution (10-30: 10-30: 1-5: 0.5-5) be developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(5) thin layer of enoxolone is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: extracting liquorice subacid reference substance adds ethanol and makes control medicinal material solution in right amount;
The preparation of b, need testing solution: sample thief is an amount of, and porphyrize adds mineral acid and chloroform for extracting reagent, and heating and refluxing extraction is put coldly, filters, and filtrate evaporate to dryness, residue add ethanol makes dissolving, makes need testing solution;
C, thin layer are differentiated: draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether-toluene-ethyl acetate-glacial acetic acid (5-20: 10-30: 2-15: 0.5-5) be developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
2. the method for quality control of a kind of cough-relieving tablets according to claim 1, described by weight cough-relieving tablets is made by following medical material: the Chinese crude drug Herba Ephedrae
Part, Pericarpium Papaveris
Part, Radix Glycyrrhizae
Part, Semen Armeniacae Amarum
Part, 1 part of Radix Platycodonis, 1 part of Semen Raphani, 1 part in Gypsum Fibrosum; It is characterized in that this method comprises the following steps:
(1) measure the content of ephedrine hydrochloride and pseudoephedrine hydrochloride in the cough-relieving tablets simultaneously with the HPLC method:
A, chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With proportioning is that acetonitrile-0.02mol/l potassium dihydrogen phosphate (transfer pH3.0) of 5: 100 is a mobile phase; The detection wavelength is 210nm;
The preparation of b, reference substance solution: get the ephedrine hydrochloride reference substance respectively and the pseudoephedrine hydrochloride reference substance is an amount of, the accurate title, decide, add 0.1% hydrochloric acid methanol and make the mixing reference substance solution of the hydrochloric ephedrine 0.1mg of every 1ml, pseudoephedrine hydrochloride 40 μ g, promptly;
The preparation of c, need testing solution: get 20 of this product, the accurate title, decided porphyrize, mixing is got about 0.6g, and accurate the title decides, put in the tool plug conical flask, add strong ammonia solution 2ml, jolting makes abundant moistening, precision adds chloroform 50ml, claims to decide weight, supersound process 30 minutes, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with chloroform, filter, precision is measured subsequent filtrate 25ml, adds 0.1% methanol hydrochloride solution 2ml, evaporate to dryness, residue adds 0.1% methanol hydrochloride solution makes dissolving in right amount, be transferred in the 10ml measuring bottle and be diluted to scale, shake up, promptly;
D, assay method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, every of this product contain Herba Ephedrae in ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C10H15NOHCl) total amount, must not be less than 0.5mg;
(2) use the HPLC method to measure the content of morphine in the cough-relieving tablets:
A, chromatographic condition: with octyl silane group silica gel is filler; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (40: 30: 30) is mobile phase; The detection wavelength is 220nm;
The preparation of b, reference substance solution: it is an amount of that precision takes by weighing the morphine reference substance, adds 20% methanol solution that contains 5% acetic acid and make the solution that every 1ml contains 40 μ g, promptly;
The preparation of c, need testing solution: get 10 of this product, remove coating, the accurate title, decided porphyrize, get the about 0.75g of powder, the accurate title, decide, and puts in the tool plug conical flask, the accurate 20% methanol solution 25ml that contains 5% acetic acid that adds, close plug claims to decide weight, supersound process (power 250W, frequency 40kHz) 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake, shake up with 20% methanol solution that contains 5% acetic acid, filter, get subsequent filtrate, promptly;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
E, whenever take unit formulation and contain Pericarpium Papaveris with morphine (C17H19O
3N) meter must not be less than 0.2mg;
(3) thin layer of ephedrine hydrochloride is differentiated in the cough-relieving tablets:
The preparation of a, reference substance solution: get the ephedrine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 2mg, make reference substance solution;
The preparation of b, need testing solution: get 6 of this product, remove coating, porphyrize, add ammonia solution number droplet, mix thoroughly, add chloroform 20ml, merceration spends the night, and filters, and filtrate is put in the separatory funnel, extract 2 (10ml with hydrochloric acid (3 → 10) solution jolting, 10ml), branch is got sour water layer, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution;
C, thin layer chromatography are differentiated: draw need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-strong ammonia solution (100: 20: 1) is developing solvent, launch, take out, dry, spray is with 0.3% 1,2,3-indantrione monohydrate butanol solution-acetic acid (19: 1) mixed solution, 105 ℃ of heating colour developings; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(4) thin layer of Pericarpium Papaveris is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get Pericarpium Papaveris control medicinal material 1g, add methanol 20ml, reflux 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution;
The preparation of b, need testing solution: get 6 of this product, remove coating, porphyrize, add ammonia solution number droplet, mix thoroughly, add chloroform 20ml, merceration spends the night, and filters, and filtrate is put in the separatory funnel, extract 2 (10ml with hydrochloric acid (3 → 10) solution jolting, 10ml), branch is got sour water layer, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution;
C, thin layer are differentiated: draw control medicinal material solution and each 10ul of need testing solution, put respectively on the silica gel g thin-layer plate of same usefulness 2% sodium hydroxide solution preparation, with toluene-acetone-ethanol-strong ammonia solution (20: 20: 3: 1) be developing solvent, 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 speckle of same color;
(5) thin layer of enoxolone is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: extracting liquorice subacid reference substance adds ethanol and makes the solution that every 1ml contains 2mg, in contrast product solution;
The preparation of b, need testing solution: get 4 of this product, remove coating, porphyrize adds hydrochloric acid 1ml and chloroform 20ml, puts in the water-bath reflux 1 hour, puts coldly, filters, and filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution;
C, thin layer differentiate: draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30～60 ℃)-toluene-ethyl acetate-glacial acetic acid (10: 20: 7: 0.5) be developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
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| CN109991359B (en) * | 2018-01-02 | 2021-07-13 | 苏州玉森新药开发有限公司 | Quality control method of Chinese medicinal composition with cough relieving and phlegm eliminating effects |
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