CN101601821B - Active component content measurement and authentication method for shenfukang tablets - Google Patents
Active component content measurement and authentication method for shenfukang tablets Download PDFInfo
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- CN101601821B CN101601821B CN2009100672544A CN200910067254A CN101601821B CN 101601821 B CN101601821 B CN 101601821B CN 2009100672544 A CN2009100672544 A CN 2009100672544A CN 200910067254 A CN200910067254 A CN 200910067254A CN 101601821 B CN101601821 B CN 101601821B
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Abstract
The invention relates to an active principle determination and identification method for shenfukang tablets, which belongs to the technical field of Chinese medicaments, and particularly refers to a method for content determination and identification of components in a Chinese medicinal preparation. The method comprises the steps of: determining the content of rutin C27H30O16 in a medicament by using a high performance liquid chromatography; and identifying a rutin component, namely a main component of flower of Chinese scholartree in the medicament by using a thin-layer chromatography. The invention has the advantages that the invention establishes the advanced quality control method for the medicament, establishes an identification item and a content determination item of the medicament and a detection method thereof, performs the identification by the thin-layer chromatography on the medicinal odor of the flower of the Chinese scholartree, namely a main medicament in the medicament, adopts the high performance liquid chromatography to determine the content of the rutin in the medicament, ensures the accuracy and advancement of the quality control method for the medicament, and can effectively control the product quality of the medicament.
Description
Technical field
The invention belongs to technical field of Chinese medicines, refer in particular to component content mensuration and discrimination method in the Chinese medicine preparation.
Background technology
The compound Chinese medicinal preparation that shenfukang tablets is made up of Rhizoma Smilacis Glabrae 366g, Flos Sophorae 93g, Rhizoma Imperatae 366g, Herba Leonuri 93g, Herba Pogostemonis 28g, Rhizoma Smilacis Glabrae 183g, Herba Pogostemonis are ground into fine powder; All the other Rhizoma Smilacis Glabrae 183g, Flos Sophorae, Rhizoma Imperatae, Herba Leonuri decocte with water secondary, decocte with water for the first time 3 hours, decocte with water for the second time 2 hours filters merging filtrate; Being concentrated into relative density is the thick paste of 1.32-1.35 (50 ℃), adds Rhizoma Smilacis Glabrae, Herba Pogostemonis fine powder, mixing, and drying under reduced pressure is ground into fine powder; Add Icing Sugar, mixing is granulated, and drying adds carboxymethylstach sodium, magnesium stearate; Mixing is pressed into 1000, and the bag film-coat promptly gets.
This medicine is a Film coated tablets, removes to show yellowish-brown behind the coating; Feeble QI, it is little sweet to distinguish the flavor of.The function of this medicine cure mainly into: clearing away heat and promoting diuresis, kidney tonifyingization is turbid, is used for the puckery pain of pyretic stranguria, acute nephritis edema, chronic nephritis acute attack.The usage and dosage of this medicine: oral, one time 4～6,3 times on the one.Every of this medicine medical material 0.946g that is equivalent to write out a prescription.
Flos Sophorae is the dry flower and alabastrum of leguminous plant Chinese scholartree Sophora japonica L., has cooling blood for hemostasis, the effect of clearing away heat and cooling blood; Be used to have blood in stool; Hematuria, stranguria with blood etc. go out blood disorder, and main component rutin, Quercetin have antiinflammatory, microcirculation improvement, spasmolytic, antiulcer effect.
Rhizoma Smilacis Glabrae is the dry rhizome of liliaceous plant smilacis glabra Smilax glabra Roxb., has dehumidifying, detoxifcation, and the effect of easing joint movement is used for damp and hot stranguria with turbid discharge, leukorrhagia, carbuncle, scrofula, scabies.
Herba Leonuri is the fresh or dry aerial parts of labiate Herba Leonuri Leonurus japonicus Houtt., has promoting blood flow to regulate menstruation, and the effect of inducing diuresis to remove edema can be used for the edema oliguria, acute nephritis edema.
Rhizoma Imperatae is the dry rhizome of grass Herba Imperatae Imperata cylindrica Beauv.var.major (Nees) C.E.Hubb., has cooling blood for hemostasis, and the effect of clearing away heat and promoting diuresis can be used for heat in blood and spits blood; Epistaxis, hematuria, calentura excessive thirst; Jaundice, edema, the puckery pain of pyretic stranguria; Acute nephritis edema.
Herba Pogostemonis is the dry aerial parts of labiate Herba Pogostemonis Pogostemon cablin (Blanco) Benth. or the dry aerial parts of labiate Herba Pogostemonis Agastache rugosus (Fisch.et.Mey.) O.Ktze., has eliminating turbid pathogen with aromatics, the appetizing preventing or arresting vomiting; Deliver the effect of expelling summer-heat, can be used for turbid damp obstructing in middle-JIAO, the vomiting of gastral cavity painful abdominal mass; The heat-damp in summer asthenia, uncomfortable in chest easypro, cold-damp is closed summer-heat; Stomachache is vomited and diarrhoea, nasosinusitis headache.
The present method of quality control of this medicine is comparatively single; At the 13 104 pages of quality standards of issuing SHENFUKANG JIAONANG of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation); In the quality standard of SHENFUKANG JIAONANG, there are not discrimination method and content assaying method, the method for quality control limitation is big; Specificity is not strong, the product quality of restive medicine.
Summary of the invention
The present invention provides a kind of assay and discrimination method of shenfukang tablets, and method of quality control is comparatively single, specificity is not strong, the problem of the product quality of restive medicine to solve.The technical scheme that the present invention takes is: comprise the content with a kind of composition of the said medicine of high effective liquid chromatography for measuring; Differentiate a kind of composition wherein with thin layer chromatography;
With rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16Content:
Chromatographic condition:
With the octadecylsilane chemically bonded silica is filler; With methanol: water: glacial acetic acid=10-40: 57-89: 1-3 or methanol: water: phosphoric acid=10-40: 57-89: 0.2-2.5 is a mobile phase; The detection wavelength is 276nm ± 2nm;
The preparation of reference substance solution:
It is an amount of that precision takes by weighing control substance of Rutin, adds methanol or ethanol and process the solution that every 1ml contains rutin 25 μ g-75 μ g;
The preparation of need testing solution:
10 of these article of getting, remove coating after, the accurate title, decided drug weight, porphyrize is got 0.5g; The accurate title, decide, and puts in the tool plug conical flask, and accurate 25ml-75ml methanol or the ethanol of adding is claimed to decide weight, supersound process 20-40 minute; Ultrasonic power 50-200W, frequency 25-75KHz is placed to 18～25 ℃, claims to decide weight again; Supply the weight that subtracts mistake with methanol or ethanol, filter, get filtrating, promptly get;
Content assaying method:
Accurate respectively reference substance solution and each 1 μ l-10 μ l of need testing solution of drawing injects chromatograph of liquid, measures rutin content;
Differentiate the main component rutin of Flos Sophorae with thin layer chromatography:
The preparation of need testing solution:
20 of these article of getting are removed coating, add methanol or the ethanol of 10ml-20ml, and supersound process 10-20 minute, filter, filtrating is concentrated into 2.5ml-7.5ml, as need testing solution;
The preparation of reference substance solution:
Take by weighing control substance of Rutin, add methanol or ethanol and process the solution that every 1ml contains rutin 1mg-3mg, as reference substance solution;
The thin layer chromatography test:
Draw each 5 μ l-15 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, launch with developing solvent, take out, dry, spray, is put under the 365nm ultra-violet lamp and is inspected after waiting to volatilize with the aluminum chloride test solution.
One embodiment of the present invention is: with 1% sodium nitrite solution, it is clear to be heated to speckle colour developing, under daylight, inspects with 10% ethanol solution of sulfuric acid or spray in spray in the chromogenic reaction;
One embodiment of the present invention is: developing solvent is a dichloromethane: methanol: formic acid=15-25: 2.5-7.5: 0.5-1.5 or ethyl acetate: formic acid: water=6-10: 0.5-1.5: 0.5-1.5 upper solution or ethyl acetate: butanone: formic acid: water=8-12: 4-8: 0.5-1.5: the 1-3 upper solution; And other developing solvent and proportioning commonly used.
Advantage of the present invention is: the deficiency that has overcome prior art; Improve the quality control standard of medicine, set up the advanced method of quality control of this medicine, set up discriminating project and the assay project and the detection method thereof of medicine; Principal agent Flos Sophorae flavour of a drug in the medicine have been carried out the thin layer chromatography discriminating; Adopt the content of the rutin in this medicine of high effective liquid chromatography for measuring, guaranteed the accuracy and the advance of drug quality control method, can control the product quality of this medicine effectively.
The specific embodiment
Embodiment 1
Comprise content with a kind of composition of the said medicine of high effective liquid chromatography for measuring; Differentiate a kind of composition wherein with thin layer chromatography;
With rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16Content:
Chromatographic condition:
With the octadecylsilane chemically bonded silica is filler; With methanol: water: glacial acetic acid=10: 89: 1 is a mobile phase; The detection wavelength is 276nm ± 2nm, and number of theoretical plate calculates by the rutin peak should be not less than 3000;
The preparation of reference substance solution:
It is an amount of that precision takes by weighing control substance of Rutin, adds methanol and process the solution that every 1ml contains rutin 25 μ g;
The preparation of need testing solution:
10 of these article of getting, remove coating after, the accurate title, decided drug weight, porphyrize is got 0.5g; The accurate title, decide, and puts in the tool plug conical flask, and the accurate 25ml methanol that adds claims to decide weight, supersound process 20 minutes; Ultrasonic power 200W, frequency 75KHz is placed to 18 ℃, claims to decide weight again; Supply the weight that subtracts mistake with methanol, filter, get filtrating, promptly get;
Content assaying method:
Accurate respectively reference substance solution and each 1 μ l of need testing solution of drawing injects chromatograph of liquid, measures rutin content;
Every of this medicine contains Flos Sophorae with rutin C
27H
30O
16Meter must not be less than 0.95mg;
Differentiate the main component rutin of Flos Sophorae with thin layer chromatography:
The preparation of need testing solution:
20 of these article of getting are removed coating, add the methanol of 10ml, and supersound process 20 minutes filters, and filtrating is concentrated into 2.5ml, as need testing solution;
The preparation of reference substance solution:
Take by weighing control substance of Rutin, add methanol and process the solution that every 1ml contains rutin 3mg, as reference substance solution;
The thin layer chromatography test:
Draw each 5 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with the developing solvent ethyl acetate: formic acid: water=upper solution expansion in 6: 0.5: 0.5; Take out, dry, spray is with the aluminum chloride test solution; After waiting to volatilize, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
In the present embodiment: with rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16The chromatographic condition of content, can also be: with methanol: water: phosphoric acid=10: 89: 0.2 be mobile phase;
In the present embodiment: differentiate with thin layer chromatography in the main component rutin of Flos Sophorae; Spray is perhaps sprayed with 1% sodium nitrite solution with 10% ethanol solution of sulfuric acid in the chromogenic reaction; It is clear to be heated to the speckle colour developing, under daylight, inspects, in the test sample chromatograph; With the corresponding position of reference substance chromatograph on, show the speckle of same color;
In the present embodiment: differentiate that with thin layer chromatography developing solvent can also be a dichloromethane: methanol: formic acid=15: 2.5: 0.5 or ethyl acetate: butanone: formic acid: water=8: 4: 0.5: 1 upper solution in the main component rutin of Flos Sophorae.
Embodiment 2
Comprise content with a kind of composition of the said medicine of high effective liquid chromatography for measuring; Differentiate a kind of composition wherein with thin layer chromatography;
Rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16Content
Chromatographic condition:
With the octadecylsilane chemically bonded silica is filler; With methanol: water: glacial acetic acid=25: 73: 2 is a mobile phase; The detection wavelength is 276nm ± 2nm, and number of theoretical plate calculates by the rutin peak should be not less than 3000;
The preparation of reference substance solution:
It is an amount of that precision takes by weighing control substance of Rutin, adds methanol and process the solution that every 1ml contains rutin 50 μ g;
The preparation of need testing solution:
10 of these article of getting, remove coating after, the accurate title, decided drug weight, porphyrize is got 0.5g; The accurate title, decide, and puts in the tool plug conical flask, and the accurate 50ml methanol that adds claims to decide weight, supersound process 30 minutes; Ultrasonic power 120W, frequency 50KHz is placed to 21 ℃, claims to decide weight again; Supply the weight that subtracts mistake with methanol, filter, get filtrating, promptly get;
Content assaying method:
Accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing inject chromatograph of liquid, measure rutin content;
Every of this medicine contains Flos Sophorae with rutin C
27H
30O
16Meter must not be less than 0.95mg;
Differentiate the main component rutin of Flos Sophorae with thin layer chromatography:
The preparation of need testing solution:
20 of these article of getting are removed coating, add the methanol of 15ml, and supersound process 15 minutes filters, and filtrating is concentrated into 5ml, as need testing solution;
The preparation of reference substance solution:
Take by weighing control substance of Rutin, add methanol and process the solution that every 1ml contains rutin 2mg, as reference substance solution;
The thin layer chromatography test:
Draw respectively 10 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: formic acid: the upper solution of water=8: 1: 1 is developing solvent; Launch, take out, dry; Spray, is put under the 365nm ultra-violet lamp and is inspected after waiting to volatilize with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
In the present embodiment: with rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16The chromatographic condition of content, can also be with methanol: water: phosphoric acid=25: 73: 2 be mobile phase;
In the present embodiment: differentiate with thin layer chromatography in the main component rutin of Flos Sophorae; Spray is perhaps sprayed with 1% sodium nitrite solution with 10% ethanol solution of sulfuric acid in the chromogenic reaction; It is clear to be heated to the speckle colour developing, under daylight, inspects, in the test sample chromatograph; With the corresponding position of reference substance chromatograph on, show the speckle of same color;
In the present embodiment: differentiate that with thin layer chromatography developing solvent can also be a dichloromethane: methanol: formic acid=20: 5: 1 or ethyl acetate: butanone: formic acid: water=10: 6: 1: 2 upper solution in the main component rutin of Flos Sophorae.
Embodiment 3
Comprise content with a kind of composition of the said medicine of high effective liquid chromatography for measuring; Differentiate a kind of composition wherein with thin layer chromatography;
Rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16Content:
Chromatographic condition:
With the octadecylsilane chemically bonded silica is filler; With methanol: water: glacial acetic acid=40: 57: 3 is a mobile phase; The detection wavelength is 276nm ± 2nm, and number of theoretical plate calculates by the rutin peak should be not less than 3000;
The preparation of reference substance solution:
It is an amount of that precision takes by weighing control substance of Rutin, adds methanol and process the solution that every 1ml contains rutin 75 μ g;
The preparation of need testing solution:
10 of these article of getting, remove coating after, the accurate title, decided drug weight, porphyrize is got 0.5g; The accurate title, decide, and puts in the tool plug conical flask, and the accurate 75ml methanol that adds claims to decide weight, supersound process 40 minutes; Ultrasonic power 50W, frequency 25KHz is placed to 25 ℃, claims to decide weight again; Supply the weight that subtracts mistake with methanol, filter, get filtrating, promptly get;
Content assaying method:
Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure rutin content;
Every of this medicine contains Flos Sophorae with rutin C
27H
30O
16Meter must not be less than 0.95mg;
Differentiate the main component rutin of Flos Sophorae with thin layer chromatography:
The preparation of need testing solution:
20 of these article of getting are removed coating, add the methanol of 20ml, and supersound process 10 minutes filters, and filtrating is concentrated into 7.5ml, as need testing solution;
The preparation of reference substance solution:
Take by weighing control substance of Rutin, add methanol and process the solution that every 1ml contains rutin 1mg, as reference substance solution;
The thin layer chromatography test:
Draw each 15 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with the developing solvent ethyl acetate: formic acid: water=upper solution expansion in 10: 1.5: 1.5; Take out, dry, spray is with the aluminum chloride test solution; After waiting to volatilize, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
In the present embodiment: with rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16The chromatographic condition of content, can also be with methanol: water: phosphoric acid=40: 57.5: 2.5 be mobile phase;
In the present embodiment: differentiate with thin layer chromatography in the main component rutin of Flos Sophorae; Spray is perhaps sprayed with 1% sodium nitrite solution with 10% ethanol solution of sulfuric acid in the chromogenic reaction; It is clear to be heated to the speckle colour developing, under daylight, inspects, in the test sample chromatograph; With the corresponding position of reference substance chromatograph on, show the speckle of same color;
In the present embodiment: differentiate that with thin layer chromatography developing solvent can also be a dichloromethane: methanol: formic acid=25: 7.5: 1.5 or ethyl acetate: butanone: formic acid: water=12: 8: 1.5: 3 upper solution in the main component rutin of Flos Sophorae.
Embodiment 4
Comprise content with a kind of composition of the said medicine of high effective liquid chromatography for measuring; Differentiate a kind of composition wherein with thin layer chromatography;
With rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16Content:
Chromatographic condition:
With the octadecylsilane chemically bonded silica is filler; With methanol: water: glacial acetic acid=10: 89: 1 is a mobile phase; The detection wavelength is 276nm ± 2nm, and number of theoretical plate calculates by the rutin peak should be not less than 3000;
The preparation of reference substance solution:
It is an amount of that precision takes by weighing control substance of Rutin, adds ethanol and process the solution that every 1ml contains rutin 25 μ g;
The preparation of need testing solution:
10 of these article of getting, remove coating after, the accurate title, decided drug weight, porphyrize is got 0.5g; The accurate title, decide, and puts in the tool plug conical flask, and the accurate 25ml ethanol that adds claims to decide weight, supersound process 20 minutes; Ultrasonic power 200W, frequency 75KHz is placed to 18 ℃, claims to decide weight again; Supply the weight that subtracts mistake with ethanol, filter, get filtrating, promptly get;
Content assaying method:
Accurate respectively reference substance solution and each 1 μ l of need testing solution of drawing injects chromatograph of liquid, measures rutin content;
Every of this medicine contains Flos Sophorae with rutin C
27H
30O
16Meter must not be less than 0.95mg;
Differentiate the main component rutin of Flos Sophorae with thin layer chromatography:
The preparation of need testing solution:
20 of these article of getting are removed coating, add the ethanol of 10ml, and supersound process 20 minutes filters, and filtrating is concentrated into 2.5ml, as need testing solution;
The preparation of reference substance solution:
Take by weighing control substance of Rutin, add ethanol and process the solution that every 1ml contains rutin 3mg, as reference substance solution;
The thin layer chromatography test:
Draw each 5 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with the developing solvent ethyl acetate: formic acid: water=upper solution expansion in 6: 0.5: 0.5; Take out, dry, spray is with the aluminum chloride test solution; After waiting to volatilize, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
Embodiment 5
Comprise content with a kind of composition of the said medicine of high effective liquid chromatography for measuring; Differentiate a kind of composition wherein with thin layer chromatography;
Rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16Content
Chromatographic condition:
With the octadecylsilane chemically bonded silica is filler; With methanol: water: glacial acetic acid=25: 73: 2 is a mobile phase; The detection wavelength is 276nm ± 2nm, and number of theoretical plate calculates by the rutin peak should be not less than 3000;
The preparation of reference substance solution:
It is an amount of that precision takes by weighing control substance of Rutin, adds ethanol and process the solution that every 1ml contains rutin 50 μ g;
The preparation of need testing solution:
10 of these article of getting, remove coating after, the accurate title, decided drug weight, porphyrize is got 0.5g; The accurate title, decide, and puts in the tool plug conical flask, and the accurate 50ml ethanol that adds claims to decide weight, supersound process 30 minutes; Ultrasonic power 120W, frequency 50KHz is placed to 21 ℃, claims to decide weight again; Supply the weight that subtracts mistake with ethanol, filter, get filtrating, promptly get;
Content assaying method:
Accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing inject chromatograph of liquid, measure rutin content;
Every of this medicine contains Flos Sophorae with rutin C
27H
30O
16Meter must not be less than 0.95mg;
Differentiate the main component rutin of Flos Sophorae with thin layer chromatography:
The preparation of need testing solution:
20 of these article of getting are removed coating, add the ethanol of 15ml, and supersound process 15 minutes filters, and filtrating is concentrated into 5ml, as need testing solution;
The preparation of reference substance solution:
Take by weighing control substance of Rutin, add ethanol and process the solution that every 1ml contains rutin 2mg, as reference substance solution;
The thin layer chromatography test:
Draw respectively 10 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: formic acid: the upper solution of water=8: 1: 1 is developing solvent; Launch, take out, dry; Spray, is put under the 365nm ultra-violet lamp and is inspected after waiting to volatilize with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Embodiment 6
Comprise content with a kind of composition of the said medicine of high effective liquid chromatography for measuring; Differentiate a kind of composition wherein with thin layer chromatography;
Rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16Content:
Chromatographic condition:
With the octadecylsilane chemically bonded silica is filler; With methanol: water: glacial acetic acid=40: 57: 3 is a mobile phase; The detection wavelength is 276nm ± 2nm, and number of theoretical plate calculates by the rutin peak should be not less than 3000;
The preparation of reference substance solution:
It is an amount of that precision takes by weighing control substance of Rutin, adds ethanol and process the solution that every 1ml contains rutin 75 μ g;
The preparation of need testing solution:
10 of these article of getting, remove coating after, the accurate title, decided drug weight, porphyrize is got 0.5g; The accurate title, decide, and puts in the tool plug conical flask, and the accurate 75ml ethanol that adds claims to decide weight, supersound process 40 minutes; Ultrasonic power 50W, frequency 25KHz is placed to 25 ℃, claims to decide weight again; Supply the weight that subtracts mistake with ethanol, filter, get filtrating, promptly get;
Content assaying method:
Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure rutin content;
Every of this medicine contains Flos Sophorae with rutin C
27H
30O
16Meter must not be less than 0.95mg;
Differentiate the main component rutin of Flos Sophorae with thin layer chromatography:
The preparation of need testing solution:
20 of these article of getting are removed coating, add the ethanol of 20ml, and supersound process 10 minutes filters, and filtrating is concentrated into 7.5ml, as need testing solution;
The preparation of reference substance solution:
Take by weighing control substance of Rutin, add ethanol and process the solution that every 1ml contains rutin 1mg, as reference substance solution;
The thin layer chromatography test:
Draw each 15 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with the developing solvent ethyl acetate: formic acid: water=upper solution expansion in 10: 1.5: 1.5; Take out, dry, spray is with the aluminum chloride test solution; After waiting to volatilize, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
Claims (1)
1. the active constituent content measuring of a shenfukang tablets and discrimination method is characterized in that: adopt the content of a kind of composition of the said medicine of high effective liquid chromatography for measuring, and differentiate a kind of composition wherein with thin layer chromatography; Said shenfukang tablets is the tablet of being processed by Rhizoma Smilacis Glabrae 366g, Flos Sophorae 93g, Rhizoma Imperatae 366g, Herba Leonuri 93g, Herba Pogostemonis 28g;
Rutin C in this medicine of high effective liquid chromatography for measuring
27H
30O
16Content:
Chromatographic condition:
With the octadecylsilane chemically bonded silica is filler; With methanol: water: glacial acetic acid=10-40: 57-89: 1-3 or methanol: water: phosphoric acid=10-40: 57-89: 0.2-2.5 is a mobile phase; The detection wavelength is 276nm ± 2nm;
The preparation of reference substance solution:
It is an amount of that precision takes by weighing control substance of Rutin, adds methanol or ethanol and process the solution that every 1ml contains rutin 25 μ g-75 μ g;
The preparation of need testing solution:
10 of these article of getting, remove coating after, the accurate title, decided drug weight, porphyrize is got 0.5g; The accurate title, decide, and puts in the tool plug conical flask, and accurate 25ml-75ml methanol or the ethanol of adding is claimed to decide weight, supersound process 20-40 minute; Ultrasonic power 50-200W, frequency 25-75KHz is placed to 18～25 ℃, claims to decide weight again; Supply the weight that subtracts mistake with methanol or ethanol, filter, get filtrating, promptly get;
Content assaying method:
Accurate respectively reference substance solution and each 1 μ l-10 μ l of need testing solution of drawing injects chromatograph of liquid, measures rutin content;
Differentiate the main component rutin of Flos Sophorae with thin layer chromatography:
The preparation of need testing solution:
20 of these article of getting are removed coating, add methanol or the ethanol of 10ml-20ml, and supersound process 10-20 minute, filter, filtrating is concentrated into 2.5ml-7.5ml, as need testing solution;
The preparation of reference substance solution:
Take by weighing control substance of Rutin, add methanol or ethanol and process the solution that every 1ml contains rutin 1mg-3mg, as reference substance solution;
The thin layer chromatography test:
Draw each 5 μ l-15 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, launch with developing solvent, take out, dry, spray, is put under the 365nm ultra-violet lamp and is inspected after waiting to volatilize with the aluminum chloride test solution; Perhaps spray with 10% ethanol solution of sulfuric acid or 1% sodium nitrite solution, it is clear to be heated to speckle colour developing, under daylight, inspects;
Said developing solvent is a dichloromethane: methanol: formic acid=15-25: 2.5-7.5: 0.5-1.5 or ethyl acetate: formic acid: water=6-10: 0.5-1.5: 0.5-1.5 upper solution or ethyl acetate: butanone: formic acid: water=8-12: 4-8: 0.5-1.5: the 1-3 upper solution.
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| CN101601821B true CN101601821B (en) | 2012-03-21 |
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| CN106053707A (en) * | 2016-06-24 | 2016-10-26 | 广西灵峰药业有限公司 | Production quality control method of medicated tortoise jelly |
| CN110715900A (en) * | 2018-07-11 | 2020-01-21 | 四川省中医药科学院 | Method for detecting content of main chemical components of turmeric according to color of turmeric powder |
| CN110090274A (en) * | 2019-05-28 | 2019-08-06 | 青岛蔚蓝生物股份有限公司 | A kind of Chinese medicine composition and preparation method and application for treating the swollen humidifier fever of chicken kidney |
| CN110772484A (en) * | 2019-11-12 | 2020-02-11 | 安徽协和成制药有限公司 | Fried sophora flower formula particle and preparation method and quality standard detection method thereof |
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| CN1095279A (en) * | 1993-05-17 | 1994-11-23 | 吉林省敦化市制药厂 | A kind of medicine for the treatment of nephropathy |
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