CN103245649A - Pingxiao tablet inspection method - Google Patents
Pingxiao tablet inspection method Download PDFInfo
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- CN103245649A CN103245649A CN2013101722087A CN201310172208A CN103245649A CN 103245649 A CN103245649 A CN 103245649A CN 2013101722087 A CN2013101722087 A CN 2013101722087A CN 201310172208 A CN201310172208 A CN 201310172208A CN 103245649 A CN103245649 A CN 103245649A
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Abstract
The invention relates to a pingxiao tablet inspection method which is used for research based on the existing pingxiao tablet inspection method. The inspection method comprises a pingxiao tablet identification method and determination on contents of nux vomica and fructus aurantii stir-fried with bran. The identification method comprises the steps that: taken pingxiao tablets examined; a filtrate serves as a testing solution; a nux vomica control medicinal material filtrate is taken to serve as a contrast medicinal material solution; and a strychnine mixed solution is taken to serve as a contrast substance solution. The inspection method is high in sensitivity, good in reproducibility, simple and convenient in operation, clear in spot, and good in separating effect; and the condition that a negative sample is free from interference can be determined through a negative contrast test.
Description
Technical field
The present invention relates to a kind of method of inspection of medicine, specifically is a kind of flat sheet method of inspection that disappears.
Background technology
The existing flat sheet method of inspection that disappears is though have the inspection technology of comparative maturity, the precision of its check still to remain the leeway of improving to the flat sheet that disappears.
Summary of the invention
The method that the purpose of this invention is to provide the flat sheet that disappears of a kind of more accurate check.
The present invention is the research of carrying out on the basis of the existing flat sheet method of inspection that disappears, and has made a kind of method of inspection new, that improved than existing method.
The present invention includes flat disappear sheet authentication method and vomiting nut, stir-baked FRUCTUS AURANTII in bran assay.
The present invention checks and has increased that excrementum pteropi thin-layer chromatography in the flat sheet that disappears is differentiated and the assay item of Fructus Aurantii, as the quality foundation of the flat sheet that disappears of control.
The excrementum pteropi thin-layer chromatography differentiates that a variable that specificity, the checking of durability methodology are required does not have obvious influence, and method is highly sensitive, favorable reproducibility, and method of operating is easy, clear spot, good separating effect, through the negative control test, negative sample is noiseless.
The assay item of Fructus Aurantii shows that to the factorial experiments that accuracy, precision, specificity, scope, durability, the checking of content limit methodology require method precision is good, highly sensitive, linearity, scope and the recovery all meet the mensuration requirement, and negative control solution is noiseless to measuring.
Embodiment
The flat sheet method of inspection that disappears of the present invention comprises flat disappear sheet authentication method and vomiting nut, stir-baked FRUCTUS AURANTII in bran assay.
One, the flat sheet authentication method that disappears of the present invention is:
(1) the make even sheet that disappears is put microscopically and is observed: unicellular nonglandular hair likeness in form fiber, and how cataclasm, base portion expands like lithocyte, lignify (prepared nux vomica); Use as following each step.
(2) 20 of the sheets of disappearing of making even are removed dressing, and porphyrize is got 4g, adds methenyl choloride-ethanol (volume ratio 10: 1), mixed liquor 10ml and dense ammonia (mass concentration 25%-28%) 0.5ml, and close plug, jolting 5 minutes was placed 2 hours, filtered, and filtrate is as need testing solution;
Other gets vomiting nut control medicinal material 1g, adds methenyl choloride-ethanol (volume ratio 10: 1) mixed liquor 10ml and dense ammonia (mass concentration 25%-28%) test solution 0.5ml, close plug, and jolting 5 minutes was placed 2 hours, filtered, and filtrate is medicinal material solution in contrast;
Get strychnine reference substance, strychnia reference substance again, add methenyl choloride and make the mixed solution that every 1ml contains 1mg, in contrast product solution.
Test according to thin-layered chromatography (Chinese Pharmacopoeia appendix VIB), draw each 5~10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-acetone-ethanol-strong ammonia solution (volume ratio 4: 5: 0.6: 0.4) be developping agent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color.
(3) 10 of the sheets of disappearing of making even are removed dressing, and porphyrize is got 2g, adds methyl alcohol 20ml, is heated to boiling, refluxes 2 hours, filters, and filtrate is as need testing solution.
Other gets Fructus Aurantii control medicinal material 1g, adds methyl alcohol 20ml, is heated to boiling, refluxes 2 hours, filters, and filtrate is medicinal material solution in contrast.
Test according to thin-layered chromatography (Chinese Pharmacopoeia appendix VIB), draw each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, upper solution with ethyl acetate-formic acid-water (volume ratio 10: 2: 3) is developping agent, launch, take out, dry, spray is put under the ultraviolet lamp (365nm) and is inspected with the aluminium choride test solution.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(4) 20 of the sheets of disappearing of making even are removed dressing, and porphyrize adds sherwood oil (30~60 ℃ of mass concentrations) 50ml, ultrasonic processing 20 minutes, filter, filter residue volatilizes, and adds ethanol 50ml, ultrasonic processing 20 minutes, filter, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, gets supernatant as need testing solution.Other gets excrementum pteropi control medicinal material 1g, adds sherwood oil (30~60 ℃) 50ml, and ultrasonic processing 20 minutes filters, filter residue volatilizes, and adds ethanol 50ml, and ultrasonic processing 20 minutes filters, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, gets supernatant medicinal material solution in contrast.According to thin-layered chromatography (Chinese Pharmacopoeia appendix VIB) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with cyclohexane-ethyl acetate (20: 4), open up to 12cm, 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, should show the fluorescence spot of same color.
Two, vomiting nut content is measured according to high performance liquid chromatography (Chinese Pharmacopoeia appendix VID).
Chromatographic condition and system suitability test: be filling agent with the octadecylsilane chemically bonded silica; Be the phase (200-2000ml) that flows with 0.01mol/L sodium heptanesulfonate and 0.02mol/L potassium dihydrogen phosphate mixed in equal amounts solution (with 10% phosphorus acid for adjusting pH value to 2.8) and acetonitrile (79: 21); The detection wavelength is 254nm.Number of theoretical plate calculates by the strychnine peak should be not less than 5000.
The preparation of reference substance solution: get strychnine reference substance 7.5mg, the accurate title, decide, and adds methenyl choloride and make the solution that every 1ml contains the 0.3mg strychnine.Precision is measured 2ml, puts in the 10ml measuring bottle, adds methyl alcohol and is diluted to 10ml, shakes up, and namely gets (every 1ml contains strychnine 60 μ g).
The preparation of need testing solution: 20 of the sheets of disappearing of making even, remove dressing, accurately claim to decide 3g, porphyrize is put in the tool plug Erlenmeyer flask, adds methenyl choloride 20ml, strong ammonia solution 1ml, be heated to boiling, refluxed 2 hours, put cold, claim again to decide weight, supply the weight that subtracts mistake with methenyl choloride, shake up, filter with the filter paper that is covered with a small amount of anhydrous sodium sulfate, precision is measured subsequent filtrate 5ml, puts in the 10ml measuring bottle, be diluted to scale with methyl alcohol, shake up, namely.
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, injects liquid chromatograph, measures, namely.
Every of this product contains prepared nux vomica in strychnine (C21H22N2O2), should be 0.25~0.35mg.
Three, stir-baked FRUCTUS AURANTII in bran content is measured according to high performance liquid chromatography (Chinese Pharmacopoeia appendix VID).
Chromatographic condition and system suitability test: be filling agent with the octadecylsilane chemically bonded silica; Be mobile phase with acetonitrile-water (20: 80) (with phosphorus acid for adjusting pH value to 3); The detection wavelength is 283nm.Number of theoretical plate calculates by the aurantiin peak should be not less than 3000.
The preparation of reference substance solution: get aurantiin, the neohesperidin reference substance of equivalent, add methyl alcohol and make every 1ml and contain aurantiin, the neohesperidin mixed solution of totally 80 μ g, namely.
The preparation of need testing solution: 20 of the sheets of disappearing of making even, remove dressing, porphyrize, get 0.25g, the accurate title, decide, and puts in the tool plug Erlenmeyer flask, the accurate methyl alcohol 25ml that adds claims to decide weight, adds hot reflux 1.5 hours, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely.
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, injects liquid chromatograph, measures, namely.
Every of this product contains stir-baked FRUCTUS AURANTII in bran in aurantiin (C27H32O14), must not be less than 0.80mg; In neohesperidin (C28H34O15), must not be less than 0.60mg.
Claims (6)
1. put down the sheet authentication method that disappears for one kind, step is:
(1) the make even sheet that disappears is put microscopically and is observed: unicellular nonglandular hair likeness in form fiber, and how cataclasm, base portion expands like lithocyte, the prepared nux vomica lignify; Use as following each step;
(2) sheet that disappears of making even is removed dressing, and porphyrize adds methenyl choloride-ethanol, the close plug of mixed liquor and strong ammonia solution, and jolting is placed the back and is filtered, and filtrate is as need testing solution;
Other gets the vomiting nut control medicinal material, adds methenyl choloride-alcohol mixeding liquid and strong ammonia solution, close plug, and jolting is placed the back and is filtered, and filtrate is medicinal material solution in contrast;
Get strychnine reference substance, strychnia reference substance again, add methenyl choloride and make every mixed solution, in contrast product solution;
Drawing above-mentioned three kinds of solution and put respectively on same silica gel g thin-layer plate, is developping agent with toluene-acetone-ethanol-strong ammonia solution, launches, and takes out, and dries, and spray is with rare bismuth potassium iodide test solution; In the test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color;
(3) sheet that disappears of making even is removed dressing, and porphyrize adds methyl alcohol, is heated to boiling, refluxes, and filters, and filtrate is as need testing solution;
Other gets the Fructus Aurantii control medicinal material, adds methyl alcohol, is heated to boiling, refluxes, and filters, and filtrate is medicinal material solution in contrast;
Drawing above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developping agent with the upper solution of ethyl acetate-formic acid-water, launches, and takes out, and dries, and spray is put under the ultraviolet lamp and inspected with the aluminium choride test solution; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(4) the make even sheet that disappears is removed dressing, and porphyrize adds sherwood oil, and ultrasonic processing filters, and filter residue volatilizes, and adds ethanol, and ultrasonic processing filters, and filtrate evaporate to dryness, residue add ethyl acetate makes dissolving, gets supernatant as need testing solution.Other gets the excrementum pteropi control medicinal material, adds sherwood oil, and ultrasonic processing filters, and filter residue volatilizes, and adds ethanol, and ultrasonic processing filters, and filtrate evaporate to dryness, residue add ethyl acetate makes dissolving, gets supernatant medicinal material solution in contrast; According to the thin-layered chromatography test, draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with cyclohexane-ethyl acetate, 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, should show the fluorescence spot of same color.
2. the flat sheet authentication method that disappears according to claim 1, in step (2): 20 of the sheets of disappearing of making even, remove dressing, porphyrize, get 4g, add methenyl choloride-ethanol (volume ratio 10: 1), mixed liquor 10ml and dense ammonia (mass concentration 25%-28%) test solution 0.5ml, close plug, jolting 5 minutes, placed 2 hours, and filtered, filtrate is as need testing solution;
Other gets vomiting nut control medicinal material 1g, adds methenyl choloride-ethanol (volume ratio 10: 1) mixed liquor 10ml and dense ammonia (mass concentration 25%-28%) test solution 0.5ml, close plug, and jolting 5 minutes was placed 2 hours, filtered, and filtrate is medicinal material solution in contrast;
Get strychnine reference substance, strychnia reference substance again, add methenyl choloride and make the mixed solution that every 1ml contains 1mg, in contrast product solution;
According to the thin-layered chromatography test, draw each 5~10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene acetone-ethanol-strong ammonia solution (volume ratio 4: 5: 0.6: 0.4) be developping agent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color.
3. the flat sheet authentication method that disappears according to claim 1, in step (3): 10 of the sheets of disappearing of making even, remove dressing, porphyrize is got 2g, adds methyl alcohol 20ml, is heated to boiling, refluxed 2 hours, filtration, filtrate is as need testing solution;
Other gets Fructus Aurantii control medicinal material 1g, adds methyl alcohol 20ml, is heated to boiling, refluxes 2 hours, filters, and filtrate is medicinal material solution in contrast;
According to the thin-layered chromatography test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, upper solution with ethyl acetate-formic acid water (volume ratio 10: 2: 3) is developping agent, launches, and takes out, dry, spray is put under the ultraviolet lamp (365nm) and is inspected with the aluminium choride test solution; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
4. the flat sheet authentication method that disappears according to claim 1, in step (4): 20 of the sheets of disappearing of making even, remove dressing, porphyrize adds sherwood oil (30~60 ℃ of mass concentrations) 50ml, ultrasonic processing 20 minutes, filter, filter residue volatilizes, and adds ethanol 50ml, ultrasonic processing 20 minutes, filter, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, gets supernatant as need testing solution.Other gets excrementum pteropi control medicinal material 1g, adds sherwood oil (30~60 ℃) 50ml, and ultrasonic processing 20 minutes filters, filter residue volatilizes, and adds ethanol 50ml, and ultrasonic processing 20 minutes filters, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, gets supernatant medicinal material solution in contrast.According to thin-layered chromatography (Chinese Pharmacopoeia appendix VIB) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with cyclohexane-ethyl acetate (20: 4), open up to 12cm, 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 fluorescence spot of same color.
5. put down vomiting nut content assaying method in the sheet that disappears for one kind, the steps include:
Chromatographic condition and system suitability test: be filling agent with the octadecylsilane chemically bonded silica; Be the phase (200-2000ml) that flows with 0.01mol/L sodium heptanesulfonate and 0.02mol/L potassium dihydrogen phosphate mixed in equal amounts solution (with 10% phosphorus acid for adjusting pH value to 2.8) and acetonitrile (79: 21); The detection wavelength is 254nm; Number of theoretical plate calculates by the strychnine peak should be not less than 5000;
The preparation of reference substance solution: get strychnine reference substance 7.5mg, the accurate title, decide, and adds methenyl choloride and make the solution that every 1ml contains the 0.3mg strychnine.Precision is measured 2ml, puts in the 10ml measuring bottle, adds methyl alcohol and is diluted to 10ml, shakes up, and namely gets (every 1ml contains strychnine 60 μ g);
The preparation of need testing solution: 20 of the sheets of disappearing of making even, remove dressing, accurately claim to decide 3g, porphyrize is put in the tool plug Erlenmeyer flask, adds methenyl choloride 20ml, strong ammonia solution 1ml, be heated to boiling, refluxed 2 hours, put cold, claim again to decide weight, supply the weight that subtracts mistake with methenyl choloride, shake up, filter with the filter paper that is covered with a small amount of anhydrous sodium sulfate, precision is measured subsequent filtrate 5ml, puts in the 10ml measuring bottle, be diluted to scale with methyl alcohol, shake up, namely;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, injects liquid chromatograph, measures, namely;
Every of this product contains prepared nux vomica in strychnine (C21H22N202), should be 0.25~0.35mg.
6. put down stir-baked FRUCTUS AURANTII in bran content assaying method in the sheet that disappears for one kind, the steps include:
Chromatographic condition and system suitability test: be filling agent with the octadecylsilane chemically bonded silica; Be mobile phase with acetonitrile-water (20: 80) (with phosphorus acid for adjusting pH value to 3); The detection wavelength is 283nm.Number of theoretical plate calculates by the aurantiin peak should be not less than 3000;
The preparation of reference substance solution: get aurantiin, the neohesperidin reference substance of equivalent, add methyl alcohol and make every 1ml and contain aurantiin, the neohesperidin mixed solution of totally 80 μ g, namely;
The preparation of need testing solution: 20 of the sheets of disappearing of making even, remove dressing, porphyrize, get 0.25g, the accurate title, decide, and puts in the tool plug Erlenmeyer flask, the accurate methyl alcohol 25ml that adds claims to decide weight, adds hot reflux 1.5 hours, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, injects liquid chromatograph, measures, namely;
Every of this product contains stir-baked FRUCTUS AURANTII in bran in aurantiin (C27H32O14), must not be less than 0.80mg; In neohesperidin (C28H34O15), must not be less than 0.60mg.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105334286A (en) * | 2015-11-25 | 2016-02-17 | 吉林修正药业新药开发有限公司 | Quality control method for medicine for treating common cold due to wind-cold |
CN105738555A (en) * | 2016-03-02 | 2016-07-06 | 广州白云山奇星药业有限公司 | Limit test method for strychnine in Huatuo Zaizao pills |
Citations (2)
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CN1772237A (en) * | 2005-11-15 | 2006-05-17 | 江西汇仁药业有限公司 | Quality control method for pile eliminating tablet |
CN1799591A (en) * | 2005-09-20 | 2006-07-12 | 天津宏仁堂药业有限公司 | Preparation method of 'Xue Fu Zhu Yu' capsule and quality standard thereof |
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2013
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Patent Citations (2)
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CN1799591A (en) * | 2005-09-20 | 2006-07-12 | 天津宏仁堂药业有限公司 | Preparation method of 'Xue Fu Zhu Yu' capsule and quality standard thereof |
CN1772237A (en) * | 2005-11-15 | 2006-05-17 | 江西汇仁药业有限公司 | Quality control method for pile eliminating tablet |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105334286A (en) * | 2015-11-25 | 2016-02-17 | 吉林修正药业新药开发有限公司 | Quality control method for medicine for treating common cold due to wind-cold |
CN105738555A (en) * | 2016-03-02 | 2016-07-06 | 广州白云山奇星药业有限公司 | Limit test method for strychnine in Huatuo Zaizao pills |
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Application publication date: 20130814 |