CN106290644A - A kind of quality determining method treating erysipelas medicine - Google Patents

A kind of quality determining method treating erysipelas medicine Download PDF

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Publication number
CN106290644A
CN106290644A CN201610688092.6A CN201610688092A CN106290644A CN 106290644 A CN106290644 A CN 106290644A CN 201610688092 A CN201610688092 A CN 201610688092A CN 106290644 A CN106290644 A CN 106290644A
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solution
reference substance
methanol
need testing
radix angelicae
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徐云
王婷婷
白冰
徐建
任晶
赵俞
李君海
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JILIN XIUZHENG PHARMACEUTICAL NEW MEDICINE DEVELOPMENT Co Ltd
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JILIN XIUZHENG PHARMACEUTICAL NEW MEDICINE DEVELOPMENT Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90Plate chromatography, e.g. thin layer or paper chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027Liquid chromatography

Abstract

A kind of quality determining method treating erysipelas medicine, thin layer including (1) Flos Lonicerae, Radix Angelicae Sinensis, Cortex Moutan, Fructus Gardeniae differentiates, Flos Lonicerae differentiates, need testing solution carry out supersound process, filter, concentrate, constant volume, reference substance solution, takes chlorogenic acid reference substance and adds methanol;Radix Angelicae Sinensis, Cortex Moutan differentiate, need testing solution carries out dissolving, extracts, is evaporated, residue dissolves, and reference substance solution is Radix Angelicae Sinensis reference substance solution, paeonol reference substance solution;Fructus Gardeniae differentiates, reference substance solution takes jasminoidin reference substance, adds methanol and make solution;(2) phillyrin, Determination of Gardenoside assay method, chromatographic condition and system suitability, the preparation of reference substance solution, the preparation of need testing solution, measure;Flos Lonicerae in prescription, Radix Angelicae Sinensis, Cortex Moutan, Fructus Gardeniae carry out qualitative identification, and the method has preferable specificity, repeatability and ruggedness;Phillyrin, jasminoidin are carried out quantitative analysis, and this method has the advantages that separating degree is high, analysis time is short and simple to operate.

Description

A kind of quality determining method treating erysipelas medicine
Technical field
The invention belongs to technical field of Chinese medicines, be specifically related to a kind of quality determining method treating erysipelas medicine.
Background technology
Erysipelas is to accumulate card with wind heat poison to accumulate the card a kind of disease as cardinal symptom with damp and hot poison.It is heat-clearing and toxic substances removing, removing heat from blood The stasis of blood, the most common a kind of disease that the many reasons such as eliminating damp-heat causes, clinical main performance is that wind heat, damp and hot poison accumulate. The clear granule of granted patent erysipelas and preparation method thereof (patent No. ZL200410042526.2) exclusively goes into operation for the applicant at present Product, this medicine is raw materials used and consumption weight fraction ratio is: Fructus Forsythiae 450~550 weight portion, Flos Lonicerae 600~700 weight Amount part, Fructus Gardeniae 300~360 weight portion, Radix Angelicae Sinensis 450~550 weight portion, Semen Coicis (stir-fry) 450~550 weight portion, Cortex Moutan 450 ~550 weight portions, Radix Curcumae 300~360 weight portion, Radix Glycyrrhizae 120~200.It is in the operation initial stage based on said medicine, also there is no structure Organizational system is for the technical scheme of middle quality control, and product quality is difficult to reach persistently to ensure.Set up the method and ensure product quality Stability, controllability.
Summary of the invention
It is an object of the invention to provide a kind of quality determining method treating erysipelas medicine.Quality control for this medicine System, concrete grammar includes that Flos Lonicerae, Radix Angelicae Sinensis, Cortex Moutan, the thin layer of Fructus Gardeniae differentiate and phillyrin, Determination of Gardenoside assay method.
(1) differentiate
1. Flos Lonicerae differentiates
Taking medicine to be checked appropriate, add methanol 5~15ml, supersound process 10~30 minutes, filter, filtrate is concentrated on a small quantity, adds first Alcohol is settled to 5ml, as need testing solution.Separately take chlorogenic acid reference substance, add methanol make every 1ml containing 0.5~1.5mg molten Liquid, as reference substance solution.Test according to thin layer chromatography general rule 0502, draw above two solution each 2~4 μ l, put respectively in On same silica gel g thin-layer plate, with volume ratio 5~10: 2: 2~the upper solution of 5 butyl acetates-formic acid-water as developing solvent, exhibition Open, take out, dry, put uviol lamp under 365nm and inspect.In test sample chromatograph, on position corresponding with reference substance chromatograph, aobvious phase Fluorescence speckle with color.
2. Radix Angelicae Sinensis, Cortex Moutan differentiate
Take medicine to be checked appropriate, add hot water 20~40ml and dissolve, let cool to room temperature, with ether extraction 2 times, each 30 ml, close And ether solution, it being evaporated to 35 DEG C of water-baths, residue adds ethyl acetate 0.5~1.5ml makes dissolving, as need testing solution.Separately take Radix Angelicae Sinensis control medicinal material 0.5~1.5g, add diethyl ether 30 ml, merceration 1 hour, shakes constantly, filters, and filtrate volatilizes naturally, and residue adds Methanol 0.5~1.5ml makes dissolving, as Radix Angelicae Sinensis control medicinal material solution.Separately take paeonol reference substance, add acetone and make every 1ml containing 2 ~the solution of 4mg, as paeonol reference substance solution.Test according to thin layer chromatography general rule 0502, draw above-mentioned three kinds of solution each 3 ~6 μ l, put respectively on same silica gel g thin-layer plate, with volume ratio 2~4: 0.5~2 thiacyclohexanes-ethyl acetate as developing solvent, Launch, take out, dry.Put uviol lamp under 365nm to inspect, in test sample chromatograph, with the corresponding position of Radix Angelicae Sinensis control medicinal material chromatograph Put, the fluorescence speckle of aobvious same color.Spray with the acid 5% ferric chloride ethanol solution of hydrochloric acid, be heated to speckle at 105 DEG C clear Clear.In test sample chromatograph, with on the corresponding position of paeonol reference substance chromatograph, show the speckle of identical color.
3. Fructus Gardeniae differentiates
Take medicine to be checked appropriate, take jasminoidin reference substance, add methanol and make the solution that every 1ml is containing 3~5mg, molten as reference substance Liquid.Test according to thin layer chromatography general rule 0502, draw need testing solution each 1~3 μ l under reference substance solution and Flos Lonicerae item, respectively Point on same silica gel g thin-layer plate, with volume ratio 4~6: 5: 0.5~2: 0.5~2 ethyl acetates-acetone-formic acid-water be Developing solvent, launches, and takes out, dries, and spray, with 10% ethanol solution of sulfuric acid, is heated to clear spot at 110 DEG C.In test sample chromatograph, On position corresponding with reference substance chromatograph, aobvious identical sepia speckle under daylight;Aobvious same color under ultra-violet lamp 365nm Speckle.
(2) assay
Phillyrin
1. chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica;With volume ratio 15~35: The acetonitrile-water of 65~85 is flowing phase;Detection wavelength is 277nm.Number of theoretical plate is calculated by phillyrin peak should be not less than 3000.
2. the preparation of reference substance solution: it is appropriate that precision weighs phillyrin reference substance, accurately weighed, adds methanol and makes every 1ml Containing the solution of 0.1~0.2mg, to obtain final product.
3. the preparation of need testing solution: take medicine 0.1~2g to be checked, accurately weighed, put in tool plug conical flask, accurate addition 50~70% methanol 50ml, close plug, weighed weight, supersound process 20~40 minutes, let cool, close plug, more weighed weight, with 50~ 70% methanol supplies less loss weight, shakes up, and centrifugal, precision measures supernatant 15~30ml, puts in round-bottomed flask, adds chloroform 15 ~30ml, 75 DEG C of water-bath reflux extraction 3 times, each 30 minutes, combined chloroform layer, water bath method.Residue adds proper amount of methanol and dissolves, Add neutral alumina 0.5~2g to mix thoroughly, be added on neutral alumina column, with 50~70% ethanol 80ml eluting, collect eluent, Be concentrated to dryness, residue with 50~70% methanol dissolve after be transferred in 5ml measuring bottle, and be diluted to scale, shake up, use microporous filter membrane Filter, to obtain final product.
4. algoscopy: precision draws reference substance solution and need testing solution each 10~20 μ l respectively, injects chromatograph of liquid, Measure, to obtain final product.
Jasminoidin
1. chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica;With volume ratio 10~20: The acetonitrile-water of 80~90 is flowing phase;Detection wavelength is 238nm.Number of theoretical plate is calculated by phillyrin peak should be not less than 3000.
2. the preparation of reference substance solution: it is appropriate that precision weighs jasminoidin reference substance, accurately weighed, adds methanol and makes every 1ml Containing the solution of 0.02~0.05mg, to obtain final product.
3. the preparation of need testing solution: take medicine 0.1~2g to be checked, accurately weighed, put in tool plug conical flask, accurate addition Methanol 50ml, close plug, weighed weight, supersound process 20~40 minutes, let cool, close plug, more weighed weight, supply with methanol and subtract Weight loss, shakes up, and filters, to obtain final product.
4. algoscopy: precision draws reference substance solution and need testing solution each 10~20 μ l respectively, injects chromatograph of liquid, Measure, to obtain final product.
There is advantages that
The method of quality control of this treatment erysipelas medicine, carries out qualitative to the Flos Lonicerae in prescription, Radix Angelicae Sinensis, Cortex Moutan, Fructus Gardeniae Differentiating, the method has preferable specificity, repeatability and ruggedness;Phillyrin, jasminoidin are carried out quantitative analysis, and this method has There is the feature that separating degree is high, analysis time is short and simple to operate, can effectively improve production efficiency, save the energy.Use simultaneously Diode array detector, investigates the specificity of method;Different instrument and different chromatographic column is used to investigate the ruggedness of method.This Method specificity is strong, and favorable reproducibility, result is accurate.The qualitative and quantitative analysis of this treatment erysipelas Control of drug quality method, for This treatment heat-clearing and toxic substances removing, cooling blood and removing stasis, the medicine of eliminating damp-heat provides safely and effectively quality control method, for the production of medicine Effective guarantee is provided with clinical practice.
Accompanying drawing explanation
Fig. 1 is Flos Lonicerae thin layer identification color spectrogram of the present invention;
Fig. 2 is Radix Angelicae Sinensis of the present invention, Cortex Moutan thin layer identification color spectrogram-Radix Angelicae Sinensis;
Fig. 3 is Radix Angelicae Sinensis of the present invention, Cortex Moutan thin layer identification color spectrogram-Cortex Moutan;
Fig. 4 is Fructus Gardeniae thin layer identification color spectrogram-daylight of the present invention;
Fig. 5 is Fructus Gardeniae thin layer identification color spectrogram-fluorescence of the present invention;
Fig. 6 is phillyrin reference substance solution high-efficient liquid phase chromatogram of the present invention;
Fig. 7 is phillyrin need testing solution high-efficient liquid phase chromatogram of the present invention;
Fig. 8 is jasminoidin reference substance solution high-efficient liquid phase chromatogram of the present invention;
Fig. 9 is jasminoidin need testing solution high-efficient liquid phase chromatogram of the present invention.
Detailed description of the invention:
Embodiment 1
Medicine to be checked: by the preparation side of granule in clear granule of erysipelas and preparation method thereof (ZL200410042526.2) embodiment Method makes granule.
(1) differentiate
1. Flos Lonicerae differentiates
Taking medicine to be checked appropriate, add methanol 15ml, supersound process 20 minutes, filter, filtrate is concentrated on a small quantity, adds methanol constant volume extremely 5ml, as need testing solution.Separately take chlorogenic acid reference substance, add methanol and make every 1ml solution containing 0.5mg, molten as reference substance Liquid.Test according to thin layer chromatography general rule 0502, draw each 2 μ l of above two solution, put respectively on same silica gel g thin-layer plate, With the upper solution of volume ratio 7: 2: 2.5 butyl acetates-formic acid-water as developing solvent, launch, take out, dry, put under 365nm Uviol lamp is inspected.In test sample chromatograph, on position corresponding with reference substance chromatograph, the fluorescence speckle of aobvious same color.
2. Radix Angelicae Sinensis, Cortex Moutan differentiate
Take medicine to be checked appropriate, add hot water 30ml and dissolve, let cool to room temperature, with ether extraction 2 times, each 30 ml, merge second Ether liquid, is evaporated to 35 DEG C of water-baths, and residue adds ethyl acetate 1.5ml makes dissolving, as need testing solution.Separately take Radix Angelicae Sinensis comparison medicine Material 0.5g, add diethyl ether 30 ml, merceration 1 hour, shakes constantly, filters, and filtrate volatilizes naturally, and residue adds methanol 0.5ml to be made molten Solve, as Radix Angelicae Sinensis control medicinal material solution.Separately take paeonol reference substance, add acetone and make every 1ml solution containing 2mg, as Cortex Moutan Phenol reference substance solution.Test according to thin layer chromatography general rule 0502, draw each 3 μ l of above-mentioned three kinds of solution, put respectively in same silica gel G On lamellae, with volume ratio 2: 1 thiacyclohexanes-ethyl acetate as developing solvent, launch, take out, dry.Put ultraviolet lamp inspection under 365nm Depending on, in test sample chromatograph, with on the corresponding position of Radix Angelicae Sinensis control medicinal material chromatograph, show the fluorescence speckle of same color.Spray is with salt The acid 5% ferric chloride ethanol solution of acid, is heated to clear spot at 105 DEG C.In test sample chromatograph, with paeonol reference substance On the corresponding position of chromatograph, the speckle of aobvious identical color.
3. Fructus Gardeniae differentiates
Take medicine to be checked appropriate, take jasminoidin reference substance, add methanol and make every 1ml solution containing 3mg, as reference substance solution. Test according to thin layer chromatography general rule 0502, draw each 3 μ l of need testing solution under reference substance solution and Flos Lonicerae item, put respectively in same On one silica gel g thin-layer plate, with volume ratio 5: 5: 1: 2 ethyl acetates-acetone-formic acid-water as developing solvent, launch, take out, dry in the air Dry, spray, with 10% ethanol solution of sulfuric acid, is heated to clear spot at 110 DEG C.In test sample chromatograph, corresponding to reference substance chromatograph Position on, aobvious identical sepia speckle under daylight;The speckle of aobvious same color under ultra-violet lamp 365nm.
(2) assay
1. chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica;With volume ratio 40:60 Acetonitrile-water is flowing phase;Detection wavelength is 277nm.Number of theoretical plate is calculated by phillyrin peak should be not less than 3000.
2. the preparation of reference substance solution: it is appropriate that precision weighs phillyrin reference substance, accurately weighed, adds methanol and makes every 1ml Containing the solution of 0.1, to obtain final product.
3. the preparation of need testing solution: take medicine 1g to be checked, accurately weighed, to put in tool plug conical flask, precision adds 70% methanol 50ml, close plug, weighed weight, supersound process 40 minutes, let cool, close plug, more weighed weight, supply less loss weight with 70% methanol, Shaking up, centrifugal, precision measures supernatant 20ml, puts in round-bottomed flask, adds chloroform 30ml, 75 DEG C of water-bath reflux extraction 3 times, often Secondary 30 minutes, combined chloroform layer, water bath method.Residue adds proper amount of methanol and dissolves, and adds neutral alumina 2g and mixes thoroughly, is added on neutral oxygen Changing on aluminum post, with 70% ethanol 80ml eluting, collect eluent, be concentrated to dryness, residue is transferred to 5ml amount with 70% methanol after dissolving In Ping, and it is diluted to scale, shakes up, filter with microporous filter membrane, to obtain final product.
4. algoscopy: precision draws reference substance solution and each 10 μ l of need testing solution respectively, injects chromatograph of liquid, surveys Fixed, to obtain final product.
Jasminoidin
1. chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica;With volume ratio 10:90 Acetonitrile-water is flowing phase;Detection wavelength is 238nm.Number of theoretical plate is calculated by phillyrin peak should be not less than 3000.
2. the preparation of reference substance solution: it is appropriate that precision weighs jasminoidin reference substance, accurately weighed, adds methanol and makes every 1ml Containing the solution of 0.03, to obtain final product.
3. the preparation of need testing solution: take medicine 0.5g to be checked, accurately weighed, to put in tool plug conical flask, precision adds methanol 50ml, close plug, weighed weight, supersound process 30 minutes, let cool, close plug, more weighed weight, supply less loss weight with methanol, shake Even, filter, to obtain final product.
4. algoscopy: precision draws reference substance solution and each 10 μ l of need testing solution respectively, injects chromatograph of liquid, surveys Fixed, to obtain final product.

Claims (1)

1. treat a quality determining method for erysipelas medicine, including Flos Lonicerae, Radix Angelicae Sinensis, Cortex Moutan, Fructus Gardeniae thin layer differentiate and Phillyrin, Determination of Gardenoside assay method, is characterized in that:
(1) differentiate
1. Flos Lonicerae differentiates
Taking medicine to be checked appropriate, add methanol 5~15ml, supersound process 10~30 minutes, filter, filtrate is concentrated on a small quantity, adds first Alcohol is settled to 5ml, as need testing solution;
Separately take chlorogenic acid reference substance, add methanol and make the solution that every 1ml is containing 0.5~1.5mg, as reference substance solution;
Test according to thin layer chromatography general rule 0502, draw above two solution each 2~4 μ l, put respectively in same silica gel g thin-layer plate On, with volume ratio 5~10: 2: 2~the upper solution of 5 butyl acetates-formic acid-water as developing solvent, launch, take out, dry, put Under 365nm, uviol lamp is inspected;
In test sample chromatograph, on position corresponding with reference substance chromatograph, the fluorescence speckle of aobvious same color;
2. Radix Angelicae Sinensis, Cortex Moutan differentiate
Take medicine to be checked appropriate, add hot water 20~40ml and dissolve, let cool to room temperature, with ether extraction 2 times, each 30 ml, close And ether solution, it being evaporated to 35 DEG C of water-baths, residue adds ethyl acetate 0.5~1.5ml makes dissolving, as need testing solution;
Separately taking Radix Angelicae Sinensis control medicinal material 0.5~1.5g, add diethyl ether 30 ml, and merceration 1 hour shakes constantly, filters, and filtrate is waved naturally Dry, residue adds methanol 0.5~1.5ml makes dissolving, as Radix Angelicae Sinensis control medicinal material solution;
Separately take paeonol reference substance, add acetone and make the solution that every 1ml is containing 2~4mg, as paeonol reference substance solution;
Test according to thin layer chromatography general rule 0502, draw above-mentioned three kinds of solution each 3~6 μ l, put respectively in same silica gel g thin-layer plate On, with volume ratio 2~4: 0.5~2 thiacyclohexanes-ethyl acetate as developing solvent, launch, take out, dry;
Put uviol lamp under 365nm to inspect, in test sample chromatograph, with on the corresponding position of Radix Angelicae Sinensis control medicinal material chromatograph, show identical The fluorescence speckle of color;
Spray with the acid 5% ferric chloride ethanol solution of hydrochloric acid, be heated to clear spot at 105 DEG C;
In test sample chromatograph, with on the corresponding position of paeonol reference substance chromatograph, show the speckle of identical color;
3. Fructus Gardeniae differentiates
Take medicine to be checked appropriate, take jasminoidin reference substance, add methanol and make the solution that every 1ml is containing 3~5mg, molten as reference substance Liquid;
Test according to thin layer chromatography general rule 0502, draw reference substance solution and differentiate need testing solution each 1~3 μ l under [1] item, point Other point is on same silica gel g thin-layer plate, with volume ratio 4~6: 5: 0.5~2: 0.5~2 ethyl acetates-acetone-formic acid-water For developing solvent, launching, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to clear spot at 110 DEG C;
In test sample chromatograph, on position corresponding with reference substance chromatograph, aobvious identical sepia speckle under daylight;Ultra-violet lamp The speckle of aobvious same color under 365nm;
(2) assay
Phillyrin
1. chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica;With volume ratio acetonitrile-water 15~35:65~85 is flowing phase;Detection wavelength is 277nm;
Number of theoretical plate is calculated by phillyrin peak should be not less than 3000;
2. the preparation of reference substance solution: it is appropriate that precision weighs phillyrin reference substance, accurately weighed, adds methanol and makes every 1ml containing 0.1 ~the solution of 0.2mg, to obtain final product;
3. the preparation of need testing solution: take medicine 0.1~2g to be checked, accurately weighed, put in tool plug conical flask, accurate add 50~ 70% methanol 50ml, close plug, weighed weight, supersound process 20~40 minutes, let cool, close plug, more weighed weight, with 50~70% first Less loss weight supplied by alcohol, shakes up, centrifugal, and precision measures supernatant 15~30ml, puts in round-bottomed flask, add chloroform 15~ 30ml, 75 DEG C of water-bath reflux extraction 3 times, each 30 minutes, combined chloroform layer, water bath method;
Residue adds proper amount of methanol and dissolves, and adds neutral alumina 0.5~2g and mixes thoroughly, is added on neutral alumina column, with 50~70% second Alcohol 80ml eluting, collects eluent, is concentrated to dryness, and residue is transferred in 5ml measuring bottle after methanol dissolving with 50~70%, and dilutes To scale, shake up, filter with microporous filter membrane, to obtain final product;
4. algoscopy: precision draws reference substance solution and need testing solution each 10~20 μ l respectively, injects chromatograph of liquid, surveys Fixed, to obtain final product;
Jasminoidin
1. chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica;With volume ratio 10~20: The acetonitrile-water of 80~90 is flowing phase;Detection wavelength is 238nm;
Number of theoretical plate is calculated by phillyrin peak should be not less than 3000;
2. the preparation of reference substance solution: it is appropriate that precision weighs jasminoidin reference substance, accurately weighed, adds methanol and makes every 1ml and contain The solution of 0.02~0.05mg, to obtain final product;
3. the preparation of need testing solution: take medicine 0.1~2g to be checked, accurately weighed, put in tool plug conical flask, accurate addition methanol 50ml, close plug, weighed weight, supersound process 20~40 minutes, let cool, close plug, more weighed weight, supply less loss weight with methanol Amount, shakes up, and filters, to obtain final product;
4. algoscopy: precision draws reference substance solution and need testing solution each 10~20 μ l respectively, injects chromatograph of liquid, surveys Fixed, to obtain final product.
CN201610688092.6A 2016-08-19 2016-08-19 A kind of quality determining method treating erysipelas medicine Pending CN106290644A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110967441A (en) * 2019-12-23 2020-04-07 河北中医学院 Rapid thin-layer identification method for Jinshi Liyan granules
CN113504158A (en) * 2021-07-14 2021-10-15 山东诺明康药物研究院有限公司 In-vitro transdermal test method for medicament containing boron dermatitis
CN114166965A (en) * 2021-11-26 2022-03-11 兰州佛慈制药股份有限公司 Detection method of traditional Chinese medicine composition for treating vertigo

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110967441A (en) * 2019-12-23 2020-04-07 河北中医学院 Rapid thin-layer identification method for Jinshi Liyan granules
CN110967441B (en) * 2019-12-23 2021-07-02 河北中医学院 Rapid thin-layer identification method for Jinshi Liyan granules
CN113504158A (en) * 2021-07-14 2021-10-15 山东诺明康药物研究院有限公司 In-vitro transdermal test method for medicament containing boron dermatitis
CN114166965A (en) * 2021-11-26 2022-03-11 兰州佛慈制药股份有限公司 Detection method of traditional Chinese medicine composition for treating vertigo
CN114166965B (en) * 2021-11-26 2024-04-26 兰州佛慈制药股份有限公司 Detection method of traditional Chinese medicine composition for treating dizziness

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Application publication date: 20170104