CN101890095B - Method for detecting cough tablets - Google Patents
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- CN101890095B CN101890095B CN200910039724A CN200910039724A CN101890095B CN 101890095 B CN101890095 B CN 101890095B CN 200910039724 A CN200910039724 A CN 200910039724A CN 200910039724 A CN200910039724 A CN 200910039724A CN 101890095 B CN101890095 B CN 101890095B
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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 detection method of cough-relieving tablets.
[background technology]
Cough-relieving tablets is made up of Chinese medicine Chinese ephedra, pappy shell, Radix Glycyrrhizae, semen armeniacae amarae, balloonflower root, radish seed, gypsum, and wherein preceding four flavors are Ma Xing Shi Gan Tang, originally is the real good recipe of breathing heavily of treatment lung heat; Through the modern science processes; " make mutually with material, smell is in harmony mutually ", change its original intention; Deposit it and become second nature, thereby widened the scope of application; Balloonflower root is opened the sharp key of lung, and the apocenosis of eliminating the phlegm is the special medicine of " disappear and gather sputum "; Pappy shell nature and flavor acid is flat, the solid and gas of astringing the lung, Compendium of Material Medica cloud " all diseases of cough were both of a specified duration, and not receive the lung-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; Pappy shell compatibility Chinese ephedra again, a surname one holds back, and opens the harmony of perverse trend and holds back, the dissipation of convergence lung; Pappy shell and Radix Glycyrrhizae compatibility then have the magical effect of sour-sweet herbs nourishing yin; All medicines share the effect of playing cough-relieving altogether, relieving asthma, eliminating the phlegm; Clinical practice with observe to confirm cough-stopping (Ke Ke) capsule to respiratory system common disease, the caused cough of frequently-occurring disease, cough up phlegm, asthma, uncomfortable in chest, pectoralgia, pharynx are itched etc., and symptom all has tangible curative effect, especially to cough, phlegm, to breathe heavily three primary symptom effects remarkable.
Ephedrine hydrochloride, pseudoephedrine hydrochloride, morphine are the principal ingredient of anesthesia cough-relieving in the cough-relieving tablets; Ephedrine hydrochloride and pseudoephedrine hydrochloride can directly act on α, two kinds of acceptors of 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 adrenaline relatively, to bronchial smooth muscle influence ephedrine to the relexation of bronchial smooth muscle than adrenaline 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 main ingredient Chinese ephedras, Radix Glycyrrhizae, pappy shell is differentiated in having guaranteed preparation; Control the content of above-mentioned 3 kinds of main effective constituents simultaneously with higher standard, thereby guaranteed this preparation higher quality controlling level.
[summary of the invention]
The objective of the invention is to overcome the weak point of prior art; Provide a kind of through effective process the content of 3 kinds of main effective constituents of three flavor main ingredient Chinese ephedras, Radix Glycyrrhizae, pappy shell in the preparation is controlled with higher standard simultaneously, thereby guaranteed that cough-relieving tablets has the detection method of the cough-relieving tablets of better quality.
The objective of the invention is to realize like this:
A kind of detection method of cough-relieving tablets, described by weight cough-relieving tablets is processed by following medicinal material: Chinese crude drug Chinese ephedra 4-8 part, pappy shell 4-8 part; Radix Glycyrrhizae 4-8 part, semen armeniacae amarae 4-8 part, balloonflower root 1-3 part; Radish seed 1-3 part, gypsum 1-3 part 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 filling agent; With the proportioning is 5-10: 100 acetonitrile-0.02mol/l potassium dihydrogen phosphate (transferring pH1-5) is moving 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 process the mixing reference substance solution of the hydrochloric ephedrine .0.05-1.00mg of every 1ml, pseudoephedrine hydrochloride 10-100 μ g, promptly get;
The preparation of c, need testing solution: sample thief, porphyrize, mixing is got about 0.1-5g, and accurate the title, decide; Put in the tool plug conical flask, add strong ammonia solution 0.5-5ml, fully wetting, precision adds methenyl choloride 20-100ml, claims to decide weight; Sonicated 20-50 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methenyl choloride; Shake up, filter, precision is measured subsequent filtrate 10-50ml, evaporate to dryness; Residue adds 0.1% watery hydrochloric acid methanol solution makes dissolving in right amount, is transferred in the measuring bottle and is diluted to scale, shakes up, and promptly gets;
D, assay method: accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, per unit preparation contain Chinese ephedra in ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C10H15NOHCl) total amount, must not be less than 0.5mg;
(2) measure the content of morphine in the cough-relieving tablets with the HPLC method:
A, chromatographic condition: with octyl silane group silica gel is filling agent; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (30-50: 20-40: 20-40) be moving 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 process the solution that every 1ml contains 20-80 μ g, promptly gets;
The preparation of c, need testing solution: sample thief, porphyrize is got powder 0.2-2g, and accurate the title, decide; Put in the tool plug conical flask, the accurate methanol solution 10-100ml that contains acetic acid that adds, close plug claims to decide weight; Sonicated 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 get;
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 liquid chromatograph, measure, promptly get;
E, whenever take unit formulation and contain pappy shell 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 methyl alcohol and process the solution that every 1ml contains 2mg, process 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 cold soaking and spend the night, filter, filtrating is put in the separatory funnel, extracts 1-2 time with the hydrochloric acid solution jolting; Obtain the sour water layer, evaporate to dryness, residue add methyl alcohol 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 methenyl choloride-methyl alcohol-strong ammonia solution (50-150: 10-30: 0.5-5) be developping agent, launch; Take out; Dry, spray is with 0.3% triketohydrindene hydrate butanol solution-acetic acid mixed solution, 105 ℃ of heating colour developings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(4) thin layer of pappy shell is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get pappy shell control medicinal material 1g, it is an amount of to add methyl alcohol, and heating and refluxing extraction filters, the filtrating evaporate to dryness, and residue adds dissolve with methanol, processes 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 methenyl choloride reagent cold soaking and spend the night, filter, filtrating is put in the separating funnel, extracts 1-2 time with the hydrochloric acid solution jolting; Obtain the sour water layer, evaporate to dryness, residue adds dissolve with methanol, processes 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 thin layer plate, with toluene-acetone-ethanol-strong ammonia solution (10-30: 10-30: 1-5: 0.5-5) be developping agent; Launch, take out, dry; Put under the ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot 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 hypo acid reference substance adds ethanol and processes 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 methenyl choloride for extracting reagent, and heating and refluxing extraction is put coldly, filter, and the filtrating evaporate to dryness, residue adds ethanol makes dissolving, processes 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 sherwood oil-toluene-ethyl acetate-glacial acetic acid (5-20: 10-30: 2-15: 0.5-5) be developping agent; Launch, take out, dry; Spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating colour developings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
The method of quality control of aforesaid a kind of cough-relieving tablets, described by weight cough-relieving tablets is processed by following medicinal material: 3.2 parts in Chinese crude drug Chinese ephedra, 3.2 parts of pappy shells, 3.2 parts in Radix Glycyrrhizae, 3.2 parts of semen armeniacae amaraes, 1 part of balloonflower root, 1 part of radish seed, 1 part in gypsum; 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 filling agent; With proportioning is that acetonitrile-0.02mol/l potassium dihydrogen phosphate (transfer pH3.0) of 5: 100 is a moving 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 process the mixing reference substance solution of the hydrochloric ephedrine 0.1mg of every 1ml, pseudoephedrine hydrochloride 40 μ g, promptly get;
The preparation of c, need testing solution: get 20 of this product, the accurate title, decide, porphyrize, and mixing is got about 0.6g; The accurate title, decide, and puts in the tool plug conical flask, adds strong ammonia solution 2ml, and jolting makes fully wetting, and precision adds chloroform 50ml; Claim decide weight, sonicated 30 minutes is put coldly, and weight decided in title again, supplies the weight that subtracts mistake with chloroform; Shake up, 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, is transferred in the 10ml measuring bottle and is diluted to scale, shakes up, and promptly gets;
D, assay method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, every of these article contain Chinese ephedra in ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C10H15NOHCl) total amount, must not be less than 0.5mg;
(2) measure the content of morphine in the cough-relieving tablets with the HPLC method:
A, chromatographic condition: with octyl silane group silica gel is filling agent; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (40: 30: 30) is moving 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 process the solution that every 1ml contains 40 μ g, promptly gets;
The preparation of c, need testing solution: get 10 of this product, remove dressing, the accurate title, decide, and porphyrize is got 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, and close plug claims to decide weight; Sonicated (power 250W, frequency 40kHz) 30 minutes is put coldly, claims decide weight again, and usefulness contains 20% methanol solution of 5% acetic acid and supplies the weight that subtracts mistake; Shake up, filter, get subsequent filtrate, promptly get;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, whenever take unit formulation and contain pappy shell 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 methyl alcohol and process the solution that every 1ml contains 2mg, process reference substance solution;
The preparation of b, need testing solution: get 6 of these article, remove dressing, porphyrize adds ammonia solution number droplet; Mix thoroughly, add methenyl choloride 20ml, cold soaking spends the night, and filters; Filtrating is put in the separating funnel, and 2 times (10ml 10ml), obtains the sour water layer with hydrochloric acid (3 → 10) solution jolting extraction; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution;
C, thin-layer chromatography are differentiated: draw need testing solution and reference substance solution; Putting respectively on same silica gel g thin-layer plate, is developping agent with methenyl choloride-methyl alcohol-strong ammonia solution (100: 20: 1), launches; Take out; Dry, spray is with 0.3% triketohydrindene hydrate butanol solution-acetic acid (19: 1) mixed solution, 105 ℃ of heating colour developings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(4) thin layer of pappy shell is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get pappy shell control medicinal material 1g, add methyl alcohol 20ml, reflux 30 minutes filters, the filtrating evaporate to dryness, and residue adds methyl alcohol 1ml makes dissolving, as control medicinal material solution;
The preparation of b, need testing solution: get 6 of these article, remove dressing, porphyrize adds ammonia solution number droplet; Mix thoroughly, add methenyl choloride 20ml, cold soaking spends the night, and filters; Filtrating is put in the separating funnel, and 2 times (10ml 10ml), obtains the sour water layer with hydrochloric acid (3 → 10) solution jolting extraction; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution;
C, thin layer differentiate: draw control medicinal material solution and each 10ul of need testing solution, put respectively on the silica gel g thin-layer plate that same usefulness 2% sodium hydroxide solution prepares, with toluene-acetone-ethanol-strong ammonia solution (20: 20: 3: 1) be developping agent; Launch, take out, dry; Put under the ultraviolet lamp (365nm) and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot 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 hypo acid reference substance adds ethanol and processes the solution that every 1ml contains 2mg, as reference substance solution;
The preparation of b, need testing solution: get 4 of these article, remove dressing, porphyrize adds hydrochloric acid 1ml and methenyl choloride 20ml, puts in the water-bath reflux 1 hour, puts coldly, filter, and the filtrating evaporate to dryness, residue adds 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 sherwood oil (30～60 ℃)-toluene-ethyl acetate-glacial acetic acid (10: 20: 7: 0.5) be developping agent; Launch, take out, dry; Spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot 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 pappy shell is differentiated; Five kinds of processing steps of thin layer discriminating of enoxolone are controlled with higher standard the content of 3 kinds of main effective constituents of three flavor main ingredient Chinese ephedras, Radix Glycyrrhizae, pappy shell simultaneously, thereby have guaranteed that cough-relieving tablets has higher quality.
[embodiment]
Embodiment 1: described by weight cough-relieving tablets is processed by following medicinal material: Chinese crude drug Chinese ephedra 4-8 part, pappy shell 4-8 part, Radix Glycyrrhizae 4-8 part, semen armeniacae amarae 4-8 part, balloonflower root 1-3 part, radish seed 1-3 part, gypsum 1-3 part; Above-mentioned raw materials seven flavors, Chinese ephedra and pappy shell are ground into fine powder, sieve; Stay fine powder subsequent use, the residue meal decocts secondary, each 2 hours with acidic aqueous solution (with about 10% hydrochloric acid solution adjust pH to 5); Filter, filtrating is with 10% sodium hydroxide solution adjust pH to 7, and soup is subsequent use; Five tastes boiling secondaries such as all the other Radix Glycyrrhizaes, each 1 hour, filter, filtrating merges with above-mentioned solution, is concentrated into the thick paste shape, adds Chinese ephedra and pappy shell fine powder, and mixing 60～70 ℃ of dryings, is ground into fine powder, adds auxiliary material, 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 filling agent; With acetonitrile-0.02mol/l potassium dihydrogen phosphate (transferring pH to 2.7) (5: 100) is moving 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 process the mixing reference substance solution of the hydrochloric ephedrine 0.05mg of every 1ml, pseudoephedrine hydrochloride 10 μ g, promptly get;
The preparation of c, need testing solution: get 20 of this product, the accurate title, decide, porphyrize, and mixing is got about 0.1g, and accurate title is fixed; Put in the tool plug conical flask, add strong ammonia solution 0.5, fully wetting, precision adds chloroform 20ml, claims to decide weight, sonicated 20 minutes; Put coldly, claim again decide weight, supply the weight that subtracts mistake, shake up with chloroform, filtration, precision is measured subsequent filtrate 10ml; Evaporate to dryness, residue add 0.1% watery hydrochloric acid methanol solution makes dissolving in right amount, is transferred in the measuring bottle and is diluted to scale, shakes up, and promptly gets;
D, assay method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, per unit preparation contain Chinese ephedra with ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C
10H15NOHCl) total amount meter must not be less than 0.5mg;
(2) measure the content of morphine in the cough-relieving tablets with the HPLC method:
A, chromatographic condition: with octyl silane group silica gel is filling agent; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (30: 20: 20) is moving 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 process the solution that every 1ml contains 20 μ g, promptly gets;
The preparation of c, need testing solution: get 10 of this product, remove dressing, the accurate title, decide, and porphyrize is got powder 0.2g; The accurate title, decide, and puts in the tool plug conical flask, the accurate methanol solution 10ml that contains acetic acid that adds, and close plug claims to decide weight; Sonicated 20 minutes is put coldly, claims decide weight again, and usefulness contains acetate methanol solution and supplies the weight that subtracts mistake; Shake up, filter, get subsequent filtrate, promptly get;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, whenever take unit formulation and contain pappy shell 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 methyl alcohol and process the solution that every 1ml contains 2mg, process reference substance solution;
The preparation of b, need testing solution: get 6 of this product, remove dressing, porphyrize adds ammonia solution number droplet, mixes thoroughly; Add the chloroform cold soaking and spend the night, filter, filtrating is put in the separatory funnel, extracts 1 time with the hydrochloric acid solution jolting; Obtain the sour water layer, evaporate to dryness, residue add methyl alcohol makes dissolving, makes test sample solution;
C, thin-layer chromatography are differentiated: draw need testing solution and reference substance solution; Putting respectively on same silica gel g thin-layer plate, is developping agent with methenyl choloride-methyl alcohol-strong ammonia solution (50: 10: 0.5), launches; Take out; Dry, spray is with 0.3% triketohydrindene hydrate butanol solution-acetic acid mixed solution, 105 ℃ of heating colour developings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(4) thin layer of pappy shell is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get pappy shell control medicinal material 1g, it is an amount of to add methyl alcohol, and heating and refluxing extraction filters, the filtrating evaporate to dryness, and residue adds dissolve with methanol, processes control medicinal material solution;
The preparation of b, need testing solution: get 6 of this product, remove dressing, porphyrize adds ammonia solution number droplet, mixes thoroughly; Add chloroform reagent cold soaking and spend the night, filter, filtrating is put in the separatory funnel, extracts 1 time with the hydrochloric acid solution jolting; Obtain the sour water layer, evaporate to dryness, residue add the methyl alcohol dissolving, make test sample solution;
C, thin layer differentiate: draw control medicinal material solution and need testing solution, put respectively on same alkaline silica gel G thin layer plate, with toluene-acetone-ethanol-strong ammonia solution (10: 10: 1: 0.5) be developping agent; Launch, take out, dry; Put under the ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot 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 hypo acid reference substance adds ethanol and processes control medicinal material solution in right amount;
The preparation of b, need testing solution: get 4 of these article, remove dressing, porphyrize adds mineral acid and methenyl choloride for extracting reagent, and heating and refluxing extraction is put coldly, filter, and the filtrating evaporate to dryness, residue adds ethanol makes dissolving, processes 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 sherwood oil-toluene-ethyl acetate-glacial acetic acid (5: 10: 2: 0.5) be developping agent; Launch, take out, dry; Spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating colour developings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
Embodiment 2: cough-relieving tablets is processed by following medicinal material by weight: 3.2 parts in Chinese crude drug Chinese ephedra, 3.2 parts of pappy shells, 3.2 parts in Radix Glycyrrhizae, 3.2 parts of semen armeniacae amaraes, 1 part of balloonflower root, 1 part of radish seed, 1 part in gypsum.Above-mentioned raw materials seven flavors, Chinese ephedra and pappy shell are ground into fine powder, sieve; Stay fine powder subsequent use, the residue meal decocts secondary, each 2 hours with acidic aqueous solution (with about 10% hydrochloric acid solution adjust pH to 5); Filter, filtrating is with 10% sodium hydroxide solution adjust pH to 7, and soup is subsequent use; Five tastes boiling secondaries such as all the other Radix Glycyrrhizaes, each 1 hour, filter, filtrating merges with above-mentioned solution, is concentrated into the thick paste shape, adds Chinese ephedra and pappy shell fine powder, and mixing 60～70 ℃ of dryings, is ground into fine powder, adds auxiliary material, 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 filling agent; With proportioning is that acetonitrile-0.02mol/l potassium dihydrogen phosphate (transfer pH to 5) of 10: 100 is a moving 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 process the mixing reference substance solution of the hydrochloric ephedrine 1.00mg of every 1ml, pseudoephedrine hydrochloride 100 μ g, promptly get;
The preparation of c, need testing solution: get 20 of this product, the accurate title, decide, porphyrize, and mixing,, get about 5g; The accurate title, decide, and puts in the tool plug conical flask, adds strong ammonia solution 5ml, and fully wetting, precision adds chloroform 100ml, claims to decide weight; Sonicated 50 minutes is put coldly, claims decide weight again, supplies the weight that subtracts mistake with chloroform, shakes up filtration; Precision is measured subsequent filtrate 50ml, and evaporate to dryness, residue add 0.1% watery hydrochloric acid methanol solution makes dissolving in right amount, is transferred in the measuring bottle and is diluted to scale, shakes up, and promptly gets;
D, assay method: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, per unit preparation contain Chinese ephedra in ephedrine hydrochloride (C10H15NOHCl) and pseudoephedrine hydrochloride (C10H15NOHCl) total amount, must not be less than 0.5mg;
(2) measure the content of morphine in the cough-relieving tablets with the HPLC method:
A, chromatographic condition: with octyl silane group silica gel is filling agent; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (50: 40: 40) is moving 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 process the solution that every 1ml contains 80 μ g, promptly gets;
The preparation of c, need testing solution: get 10 of this product, remove dressing, the accurate title, decide, and porphyrize is got powder 2g; The accurate title, decide, and puts in the tool plug conical flask, the accurate methanol solution 100ml that contains acetic acid that adds, and close plug claims to decide weight; Sonicated 50 minutes is put coldly, claims decide weight again, and usefulness contains acetate methanol solution and supplies the weight that subtracts mistake; Shake up, filter, get subsequent filtrate, promptly get;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, whenever take unit formulation and contain pappy shell 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 methyl alcohol and process the solution that every 1ml contains 2mg, process reference substance solution;
The preparation of b, need testing solution: get 6 of this product, remove dressing, porphyrize adds ammonia solution number droplet, mixes thoroughly; Add the chloroform cold soaking and spend the night, filter, filtrating is put in the separatory funnel, extracts 2 times with the hydrochloric acid solution jolting; Obtain the sour water layer, evaporate to dryness, residue add methyl alcohol makes dissolving, makes test sample solution;
C, thin-layer chromatography are differentiated: draw need testing solution and reference substance solution; Putting respectively on same silica gel g thin-layer plate, is developping agent with methenyl choloride-methyl alcohol-strong ammonia solution (150: 30: 5), launches; Take out; Dry, spray is with 0.3% triketohydrindene hydrate butanol solution-acetic acid mixed solution, 105 ℃ of heating colour developings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(4) thin layer of pappy shell is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get pappy shell control medicinal material 1g, it is an amount of to add methyl alcohol, and heating and refluxing extraction filters, the filtrating evaporate to dryness, and residue adds dissolve with methanol, processes control medicinal material solution;
The preparation of b, need testing solution: get 6 of this product, remove dressing, porphyrize adds ammonia solution number droplet, mixes thoroughly; Add chloroform reagent cold soaking and spend the night, filter, filtrating is put in the separatory funnel, extracts 2 times with the hydrochloric acid solution jolting; Obtain the sour water layer, evaporate to dryness, residue add the methyl alcohol dissolving, make test sample solution;
C, thin layer differentiate: draw control medicinal material solution and need testing solution, put respectively on same alkaline silica gel G thin layer plate, with toluene-acetone-ethanol-strong ammonia solution (30: 30: 5: 5) be developping agent; Launch, take out, dry; Put under the ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot 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 hypo acid reference substance adds ethanol and processes control medicinal material solution in right amount;
The preparation of b, need testing solution: get 4 of these article, remove dressing, porphyrize adds mineral acid and methenyl choloride for extracting reagent, and heating and refluxing extraction is put coldly, filter, and the filtrating evaporate to dryness, residue adds ethanol makes dissolving, processes 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 sherwood oil-toluene-ethyl acetate-glacial acetic acid (20: 30: 15: 5) be developping agent; Launch, take out, dry; Spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating colour developings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
Embodiment 3: cough-relieving tablets is processed by following medicinal material by weight: 4.8 parts in Chinese crude drug Chinese ephedra, 4.8 parts of pappy shells, 4.8 parts in Radix Glycyrrhizae, 4.8 parts of semen armeniacae amaraes, 1.5 parts of balloonflower roots, 1.5 parts of radish seeds, 1.5 parts in gypsum.Above-mentioned raw materials seven flavors, Chinese ephedra and pappy shell are ground into fine powder, sieve; Stay fine powder subsequent use, the residue meal decocts secondary, each 2 hours with acidic aqueous solution (with about 10% hydrochloric acid solution adjust pH to 5); Filter, filtrating is with 10% sodium hydroxide solution adjust pH to 7, and soup is subsequent use; Five tastes boiling secondaries such as all the other Radix Glycyrrhizaes, each 1 hour, filter, filtrating merges with above-mentioned solution, is concentrated into the thick paste shape, adds Chinese ephedra and pappy shell fine powder, and mixing 60～70 ℃ of dryings, is ground into fine powder, adds auxiliary material, 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 filling agent; With the proportioning is 5-10: 100 acetonitrile-0.02mol/l potassium dihydrogen phosphate (transferring pH to 3) is moving 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 process the mixing reference substance solution of the hydrochloric ephedrine 0.75mg of every 1ml, pseudoephedrine hydrochloride 50 μ g, promptly get;
The preparation of c, need testing solution: get 20 of this product, the accurate title, decide, porphyrize, and mixing is got about 2.5g, and accurate title is fixed; Put in the tool plug conical flask, add strong ammonia solution 2.7ml, fully wetting, precision adds chloroform 60ml, claims to decide weight, sonicated 35 minutes; Put coldly, claim again decide weight, supply the weight that subtracts mistake, shake up with chloroform, filtration, precision is measured subsequent filtrate 30ml; Evaporate to dryness, residue add 0.1% watery hydrochloric acid methanol solution makes dissolving in right amount, is transferred in the measuring bottle and is diluted to scale, shakes up, and promptly gets;
D, assay method: accurate respectively reference substance solution and each 12 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, per unit preparation contain Chinese ephedra 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 filling agent; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution (40: 30: 30) is moving 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 process the solution that every 1ml contains 50 μ g, promptly gets;
The preparation of c, need testing solution: get 10 of this product, remove dressing, the accurate title, decide, and porphyrize is got powder 1.1g; The accurate title, decide, and puts in the tool plug conical flask, the accurate methanol solution 50ml that contains acetic acid that adds, and close plug claims to decide weight; Sonicated 35 minutes is put coldly, claims decide weight again, and usefulness contains acetate methanol solution and supplies the weight that subtracts mistake; Shake up, filter, get subsequent filtrate, promptly get;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 12 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, whenever take unit formulation and contain pappy shell 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 methyl alcohol and process the solution that every 1ml contains 2mg, process reference substance solution;
The preparation of b, need testing solution: get 6 of this product, remove dressing, porphyrize adds ammonia solution number droplet, mixes thoroughly; Add the chloroform cold soaking and spend the night, filter, filtrating is put in the separatory funnel, extracts 1.5 times with the hydrochloric acid solution jolting; Obtain the sour water layer, evaporate to dryness, residue add methyl alcohol makes dissolving, makes test sample solution;
C, thin-layer chromatography are differentiated: draw need testing solution and reference substance solution; Putting respectively on same silica gel g thin-layer plate, is developping agent with methenyl choloride-methyl alcohol-strong ammonia solution (100: 20: 3), launches; Take out; Dry, spray is with 0.3% triketohydrindene hydrate butanol solution-acetic acid mixed solution, 105 ℃ of heating colour developings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(4) thin layer of pappy shell is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get pappy shell control medicinal material 1g, it is an amount of to add methyl alcohol, and heating and refluxing extraction filters, the filtrating evaporate to dryness, and residue adds dissolve with methanol, processes control medicinal material solution;
The preparation of b, need testing solution: get 6 of this product, remove dressing, porphyrize adds ammonia solution number droplet, mixes thoroughly; Add chloroform reagent cold soaking and spend the night, filter, filtrating is put in the separatory funnel, extracts 1.5 times with the hydrochloric acid solution jolting; Obtain the sour water layer, evaporate to dryness, residue add the methyl alcohol dissolving, make test sample solution;
C, thin layer differentiate: draw control medicinal material solution and need testing solution, put respectively on same alkaline silica gel G thin layer plate, with toluene-acetone-ethanol-strong ammonia solution (20: 20: 3: 3) be developping agent; Launch, take out, dry; Put under the ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot 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 hypo acid reference substance adds ethanol and processes control medicinal material solution in right amount;
The preparation of b, need testing solution: get 4 of these article, remove dressing, porphyrize adds mineral acid and methenyl choloride for extracting reagent, and heating and refluxing extraction is put coldly, filter, and the filtrating evaporate to dryness, residue adds ethanol makes dissolving, processes 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 sherwood oil-toluene-ethyl acetate-glacial acetic acid (12: 20: 8: 3) be developping agent; Launch, take out, dry; Spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating colour developings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
Claims (1)
1. the detection method of a cough-relieving tablets, described by weight cough-relieving tablets is processed by following medicinal material: 3.2 parts in Chinese crude drug Chinese ephedra, 3.2 parts of pappy shells, 3.2 parts in Radix Glycyrrhizae, 3.2 parts of semen armeniacae amaraes, 1 part of balloonflower root, 1 part of radish seed, 1 part in gypsum; It is characterized in that this method step is following:
(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 filling agent; With proportioning is that to transfer pH be 3.0 to be moving phase for 5: 100 acetonitrile-0.02mol/l potassium dihydrogen phosphate; 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 process the mixing reference substance solution of the hydrochloric ephedrine 0.1mg of every 1ml, pseudoephedrine hydrochloride 40 μ g, promptly get;
The preparation of c, need testing solution: get 20 of these article, the accurate title, decide, porphyrize, and mixing is got 0.6g; The accurate title, decide, and puts in the tool plug conical flask, adds strong ammonia solution 2ml, and jolting makes fully wetting, and precision adds methenyl choloride 50ml; Claim decide weight, sonicated 30 minutes is put coldly, and weight decided in title again, supplies the weight that subtracts mistake with methenyl choloride; Shake up, 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, is transferred in the 10ml measuring bottle and is diluted to scale, shakes up, and promptly gets;
D, assay method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, every of these article contain Chinese ephedra in ephedrine hydrochloride and pseudoephedrine hydrochloride total amount, must not be less than 0.5mg;
(2) measure the content of morphine in the cough-relieving tablets with the HPLC method:
A, chromatographic condition: with octyl silane group silica gel is filling agent; With acetonitrile-0.01mol/L dipotassium hydrogen phosphate solution-0.005mol/L heptanesulfonic acid sodium water solution is moving phase at 40: 30: 30; 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 process the solution that every 1ml contains 40 μ g, promptly gets;
The preparation of c, need testing solution: get 10 of this product, remove dressing, the accurate title, decide, and porphyrize is got powder 0.75g, and accurate title is fixed; Put 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, sonicated; Power 250W, frequency 40kHz, 30 minutes, put coldly, claim to decide weight again; 20% methanol solution with containing 5% acetic acid is supplied the weight that subtracts mistake, shakes up, and filters, and gets subsequent filtrate, promptly gets;
The content assaying method of d, morphine: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
E, whenever take unit formulation and contain pappy shell with morphine C17H19O
3The N 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 methyl alcohol and process the solution that every 1ml contains 2mg, process reference substance solution;
The preparation of b, need testing solution: get 6 of these article, remove dressing, porphyrize adds ammonia solution number droplet; Mix thoroughly, add methenyl choloride 20ml, cold soaking spends the night, and filters; Filtrating is put in the separating funnel, extracts 2 times with hydrochloric acid 3 → 10 solution joltings, and each 10ml obtains the sour water layer; Evaporate to dryness, residue add methyl alcohol 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, be developping agent with methenyl choloride-methyl alcohol-strong ammonia solution at 100: 20: 1, launches; Take out; Dry, spray is with 19: 1 mixed solutions of 0.3% triketohydrindene hydrate butanol solution-acetic acid, 105 ℃ of heating colour developings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(4) thin layer of pappy shell is differentiated in the cough-relieving tablets:
The preparation of a, control medicinal material solution: get pappy shell control medicinal material 1g, add methyl alcohol 20ml, reflux 30 minutes filters, the filtrating evaporate to dryness, and residue adds methyl alcohol 1ml makes dissolving, as control medicinal material solution;
The preparation of b, need testing solution: get 6 of these article, remove dressing, porphyrize adds ammonia solution number droplet; Mix thoroughly, add methenyl choloride 20ml, cold soaking spends the night, and filters; Filtrating is put in the separating funnel, extracts 2 times with hydrochloric acid 3 → 10 solution joltings, and each 10ml obtains the sour water layer; Obtain the sour water layer, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution;
C, thin layer differentiate: draw control medicinal material solution and each 10ul of need testing solution, put respectively on the silica gel g thin-layer plate that same usefulness 2% sodium hydroxide solution prepares, with toluene-acetone-ethanol-strong ammonia solution 20: 20: 3: 1 was developping agent; Launch, take out, dry; Put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot 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 hypo acid reference substance adds ethanol and processes the solution that every 1ml contains 2mg, as reference substance solution;
The preparation of b, need testing solution: get 4 of these article, remove dressing, porphyrize adds hydrochloric acid 1ml and methenyl choloride 20ml, puts in the water-bath reflux 1 hour, puts coldly, filter, and the filtrating evaporate to dryness, residue adds 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 30～60 ℃-toluene-ethyl acetate of sherwood oil-glacial acetic acid 10: 20: 7: 0.5 was developping agent; Launch, take out, dry; Spray is with 10% phosphomolybdic acid ethanol solution, 105 ℃ of heating; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
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