CN102370812A - Method for detecting antiphlogistic and antipyretic particles - Google Patents
Method for detecting antiphlogistic and antipyretic particles Download PDFInfo
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- CN102370812A CN102370812A CN2010102639878A CN201010263987A CN102370812A CN 102370812 A CN102370812 A CN 102370812A CN 2010102639878 A CN2010102639878 A CN 2010102639878A CN 201010263987 A CN201010263987 A CN 201010263987A CN 102370812 A CN102370812 A CN 102370812A
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Abstract
The invention relates to a method for detecting a Chinese medicinal preparation, in particular to a method for detecting antiphlogistic and antipyretic particles of Chinese traditional patent medicine. The detecting method comprises the following steps of: (1) identifying whether the antiphlogistic and antipyretic particles contain dandelion by taking caffeic ester as a reference substance with thin-layer chromatography; and (2) measuring the content of glycyrrhizic acid in the antiphlogistic and antipyretic particles with high performance liquid chromatography.
Description
Technical field
The present invention relates to a kind of detection method of Chinese medicine preparation, specifically, the present invention relates to the particulate detection method of Chinese patent medicine anti-inflammatory antipyretic.
Background technology
The anti-inflammatory antipyretic granule is a kind of heat-clearing and toxic substances removing, and removing heat from blood repercussive Chinese patent medicine has gone on the market for many years in China, the clinical cold, fever that is used for, and upper respiratory tract infection, laryngopharynx swelling and pain and various furuncle curative effect such as swell and ache certainly.The anti-inflammatory antipyretic granule is prepared from Chinese crude drug Folium Isatidis, Herba Taraxaci, Herba Violae and the Radix Glycyrrhizae common process by the Chinese patent medicine mixture.The quality standard of this product records in the 5th in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation, and standard is numbered WS
3-B-1008-91.Have no discrimination method in this standard, and have no quantitative detection method, be unfavorable for controlling the particulate product quality of anti-inflammatory antipyretic.
Summary of the invention
The objective of the invention is to have no discrimination method and have no quantitative detection method in order to overcome in the present anti-inflammatory antipyretic granular mass standard; Be unfavorable for controlling the shortcoming of product quality; Provide a kind of specificity strong, and more can accurately control the particulate detection method of anti-inflammatory antipyretic of product quality.
The present invention has increased in the proper mass control method: thin layer chromatography is adopted in (1), is reference substance with the coffee ester, differentiates in the anti-inflammatory antipyretic granule and contains Herba Taraxaci; (2) content of glycyrrhizic acid in the employing high effective liquid chromatography for measuring anti-inflammatory antipyretic granule.
One, thin layer chromatography is differentiated and is contained Herba Taraxaci in the anti-inflammatory antipyretic granule:
Experimental apparatus, reagent and reagent
Experimental apparatus: chromatoplate, chromatography cylinder, point sample capillary tube, ultra-violet lamp etc.
Reagent and reagent: coffee ester reference substance (Nat'l Pharmaceutical & Biological Products Control Institute)
The anti-inflammatory antipyretic granule negative control appearance agents useful for same of anti-inflammatory antipyretic particulate samples, scarce Herba Taraxaci is analytical pure
The need testing solution preparation: get these article 20g, add the methanol solution 30ml of 5% formic acid, supersound process 30 minutes filters; The filtrating evaporate to dryness, residue adds water 10ml makes dissolving, filters; Filtrating is extracted 3 times with the ethyl acetate jolting, each 10ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
Reference substance solution preparation: get coffee ester reference substance, add methanol and process the solution that every 1ml contains 0.5mg, as reference substance solution.
Lack the negative appearance preparation of anti-inflammatory antipyretic granule of Herba Taraxaci: press the preparation of need testing solution method for preparing.
According to thin layer chromatography (Chinese Pharmacopoeia version appendix in 2005 VIB) test, draw each 10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, be developing solvent with the upper solution of butyl acetate-formic acid-water (14: 5: 5), launch, take out, dry.
Develop the color: lamellae is put under the ultra-violet lamp (365nm) inspected.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.Repeatability is good and negative noiseless.
Above result shows that the method can be as the exclusive discriminating of Herba Taraxaci thin layer in the anti-inflammatory antipyretic granule.
Two, the preferable condition of the content of glycyrrhizic acid is in the high effective liquid chromatography for measuring anti-inflammatory antipyretic granule:
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filler: acetonitrile-0.05% phosphoric acid solution (80: 20) is mobile phase; The detection wavelength is 237nm.Number of theoretical plate should be not less than 3000 by the glycyrrhizic acid peak.
The preparation extracting liquorice acid reference substance of reference substance solution is an amount of, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains glycyrrhizic acid 0.1mg, promptly gets.
These article are got in the preparation of need testing solution, and porphyrize is got 2g, and accurate the title decides, and puts in the tool plug conical flask; The accurate 70% ethanol 20ml that adds, close plug is claimed to decide weight, and supersound process 30 minutes is put cold; Claim to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, precision is measured subsequent filtrate 1ml; Put in the 5ml measuring bottle, add 70% ethanol dilution, shake up, promptly get to scale.
The methodological study of content assaying method:
1, linear relationship: it is an amount of that precision takes by weighing the glycyrrhizic acid reference substance, puts in the 10ml measuring bottle, adds 70% ethanol and process the solution that every 1ml contains glycyrrhizic acid 1mg, shakes up; Precision absorption 0.25,0.5,1.0,2.0ml put respectively in the 10ml measuring bottle, add Diluted Alcohol and are diluted to scale, shake up.Sample introduction 20 μ l inject chromatograph of liquid respectively, measure the peoniflorin peak area.With the peak height is vertical coordinate, is abscissa with glycyrrhizic acid concentration, and the drawing standard curve calculates regression equation: Y=64.5X+0.961, r=0.9989.The result shows that the glycyrrhizic acid reference substance solution has good linear relationship in 0.2～0.025mg scope.
2, precision experiment: accurate absorption concentration is the reference substance solution of 0.1mg/ml, presses liquid phase chromatogram condition, repeats sample introduction 5 times, measures the result and sees table 1.
Table 1 Precision test result
Above result shows that this method precision is good.
3, replica test: accurate 5 parts of the random sample article of claiming, every part of about 2g measures according to liquid phase chromatogram condition.The result sees table 2.
Table 2
Above result shows that this method repeatability is good.
4, response rate experiment: 5 parts in the accurate sample of claiming decide known content, every part of about 2g accurately respectively adds glycyrrhizic acid according to article, and employing application of sample recovery test is pressed chromatographic condition mensuration, calculate recovery rate, the result sees table 3.
Table 3
Above result shows that this method response rate is good.
This assay method is through the methodology checking, and negative sample is noiseless to measuring.Measure ten batches of anti-inflammatory antipyretic particulate samples with this method, the content results of glycyrrhizic acid is (mg) as follows:
According to above result and primary standard, stipulate that every bag of these article (10g) contain Radix Glycyrrhizae in glycyrrhizic acid, must not be less than 0.2mg.
The particulate method of quality control of anti-inflammatory antipyretic of the present invention; Not only increased the qualitative identification method but also increased the Content Measurement of Effective Ingredient in Happiness method; Improve the specificity and the quality stability of anti-inflammatory antipyretic granular mass control method, guaranteed the safety and the effectiveness of people's medications.The particulate method of quality control of anti-inflammatory antipyretic of the present invention both can be used for controlling the particulate quality of anti-inflammatory antipyretic, can be used for controlling the quality of other dosage form such as the granule etc. of identical prescription again.
The specific embodiment
Below in conjunction with embodiment the present invention is described further, but not as restriction.
Embodiment 1, to get lot number that the applicant produces be 090101 anti-inflammatory antipyretic granule.
These article 20g is got in [discriminating] (1), adds the methanol solution 30ml of 5% formic acid, and supersound process 30 minutes filters; The filtrating evaporate to dryness, residue adds water 10ml makes dissolving, filters; Filtrating is extracted 3 times with the ethyl acetate jolting, each 10ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets coffee ester reference substance, adds methanol and processes the solution that every 1ml contains 0.5mg, as reference substance solution.According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with the upper solution of butyl acetate-formic acid-water (14: 5: 5), launch, take out, dry, put under the ultraviolet light (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
[inspection] should meet each item regulation (appendix IJ of Chinese Pharmacopoeia version in 2005) relevant under the mixture item.
[assay] takes high picture liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D) mensuration.
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filler: acetonitrile-0.05% phosphoric acid solution (80: 20) is mobile phase; The detection wavelength is 237nm.Number of theoretical plate should be not less than 3000 by the glycyrrhizic acid peak.
The preparation extracting liquorice acid reference substance of reference substance solution is an amount of, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains glycyrrhizic acid 0.1mg, promptly gets.
These article are got in the preparation of need testing solution, and porphyrize is got 2g, and accurate the title decides, and puts in the tool plug conical flask; The accurate 70% ethanol 20ml that adds, close plug is claimed to decide weight, and supersound process 30 minutes is put cold; Claim to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, precision is measured subsequent filtrate 1ml; Put in the 5ml measuring bottle, add 70% ethanol dilution, shake up, promptly get to scale.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, and promptly get.
These article every bag (10g) contain Radix Glycyrrhizae in glycyrrhizic acid, are 0.22mg.
Claims (4)
1. particulate detection method of anti-inflammatory antipyretic is characterized in that said detection method comprises: thin layer chromatography is adopted in (1), is reference substance with the coffee ester, differentiates in the anti-inflammatory antipyretic granule and contains Herba Taraxaci; (2) content of glycyrrhizic acid in the employing high effective liquid chromatography for measuring anti-inflammatory antipyretic granule.
2. detection method according to claim 1 is characterized in that, said discrimination method comprises:
These article of getting 20g adds the methanol solution 30ml of 5% formic acid, and supersound process 30 minutes filters, the filtrating evaporate to dryness; Residue adds water 10ml makes dissolving, filters, and filtrating is extracted 3 times with the ethyl acetate jolting, each 10ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets coffee ester reference substance, adds methanol and processes the solution that every 1ml contains 0.5mg, as reference substance solution.According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with the upper solution of butyl acetate-formic acid-water (14: 5: 5), launch, take out, dry, put under the ultraviolet light (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
3. detection method according to claim 1 is characterized in that, said content assaying method comprises:
Take the high picture liquid chromatography for measuring of Chinese Pharmacopoeia version in 2005 appendix VI D
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filler: acetonitrile-0.05% phosphoric acid solution (80: 20) is mobile phase; The detection wavelength is 237nm.Number of theoretical plate should be not less than 3000 by the glycyrrhizic acid peak,
The preparation extracting liquorice acid reference substance of reference substance solution is an amount of, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains glycyrrhizic acid 0.1mg, promptly get,
These article are got in the preparation of need testing solution, and porphyrize is got 2g, and accurate the title decides, and puts in the tool plug conical flask; The accurate 70% ethanol 20ml that adds, close plug is claimed to decide weight, and supersound process 30 minutes is put cold; Claim to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, precision is measured subsequent filtrate 1ml; Put in the 5ml measuring bottle, add 70% ethanol dilution, shake up, promptly get to scale
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly get,
These article every bag (10g) contain Radix Glycyrrhizae in glycyrrhizic acid, are 0.22mg.
4. particulate detection method of anti-inflammatory antipyretic is characterized in that said detection method comprises:
These article 20g is got in [discriminating] (1), adds the methanol solution 30ml of 5% formic acid, and supersound process 30 minutes filters; The filtrating evaporate to dryness, residue adds water 10ml makes dissolving, filters; Filtrating is extracted 3 times with the ethyl acetate jolting, each 10ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets coffee ester reference substance, adds methanol and processes the solution that every 1ml contains 0.5mg, as reference substance solution.According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with the upper solution of butyl acetate-formic acid-water (14: 5: 5), launch, take out, dry, put under the ultraviolet light (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
[inspection] should meet each item regulation (appendix IJ of Chinese Pharmacopoeia version in 2005) relevant under the mixture item.
[assay] takes high picture liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005) mensuration.
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filler: acetonitrile-0.05% phosphoric acid solution (80: 20) is mobile phase; The detection wavelength is 237nm.Number of theoretical plate should be not less than 3000 by the glycyrrhizic acid peak.
The preparation extracting liquorice acid reference substance of reference substance solution is an amount of, and accurate the title decides, and adds 70% ethanol and processes the solution that every 1ml contains glycyrrhizic acid 0.1mg, promptly gets.
These article are got in the preparation of need testing solution, and porphyrize is got 2g, and accurate the title decides, and puts in the tool plug conical flask; The accurate 70% ethanol 20ml that adds, close plug is claimed to decide weight, and supersound process 30 minutes is put cold; Claim to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, precision is measured subsequent filtrate 1ml; Put in the 5ml measuring bottle, add 70% ethanol dilution, shake up, promptly get to scale.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, and promptly get.
These article every bag (10g) contain Radix Glycyrrhizae in glycyrrhizic acid, are 0.22mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2010102639878A CN102370812A (en) | 2010-08-26 | 2010-08-26 | Method for detecting antiphlogistic and antipyretic particles |
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| CN2010102639878A CN102370812A (en) | 2010-08-26 | 2010-08-26 | Method for detecting antiphlogistic and antipyretic particles |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048397A (en) * | 2012-11-29 | 2013-04-17 | 四川科伦药业股份有限公司 | Method for detecting anti-inflammation and fever-abatement medicament |
| CN114099592A (en) * | 2020-08-31 | 2022-03-01 | 南京海昌中药集团有限公司 | Anti-inflammation and antipyretic granules and quality detection method thereof |
-
2010
- 2010-08-26 CN CN2010102639878A patent/CN102370812A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048397A (en) * | 2012-11-29 | 2013-04-17 | 四川科伦药业股份有限公司 | Method for detecting anti-inflammation and fever-abatement medicament |
| CN114099592A (en) * | 2020-08-31 | 2022-03-01 | 南京海昌中药集团有限公司 | Anti-inflammation and antipyretic granules and quality detection method thereof |
| CN114099592B (en) * | 2020-08-31 | 2022-12-27 | 南京海昌中药集团有限公司 | Anti-inflammation and antipyretic granules and quality detection method thereof |
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Application publication date: 20120314 |