CN102520108A - Quality detection method of compound cordate houttuynia mistura by using thin-layer chromatography - Google Patents
Quality detection method of compound cordate houttuynia mistura by using thin-layer chromatography Download PDFInfo
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Abstract
The invention discloses a quality detection method of a traditional Chinese medicine mistura, and particularly relates to a quality detection method of a compound cordate houttuynia mistura by using a thin-layer chromatography. The quality detection method disclosed by the invention comprises the following steps of: taking a mixture of ethyl acetate, butanone, formic acid and water in a ratio of (2-8): (1-5): (0.5-1.5): (0.5-1.5) as a developing agent; taking a mixture of toluene, ethyl acetate, methanol and formic acid in a ratio of (8-12): (1-5): (0.5-1.5): (1-3) as a developing agent; and taking the two different developing agents to carry out two times of developing on a sample, so as to simultaneously identify four spots including baicalin, chlorogenic acid, baicalein and wogonin. The method disclosed by the invention has the advantages of high detection efficiency, low cost and high practical value.
Description
Technical field
The present invention relates to a kind of quality determining method of herb mixture, particularly a kind of quality determining method of thin-layer chromatography of compound houttuynin mixture.
Background technology
The compound houttuynin mixture is by cordate houttuynia, the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, the compound preparation of honeysuckle five kinds of Chinese medicine through being processed into.Have clearing heat and detoxicating effect, what be used for that affection of exogenous wind-heat causes has sore throat; Acpuei pharyngitis, tonsillitis have the wind-heat patient.For the quality of strictness control compound houttuynin mixture, be necessary to study the method for quality control of a cover compound houttuynin mixture.
Summary of the invention
The objective of the invention is to disclose a kind of quality determining method of thin-layer chromatography of compound houttuynin mixture.
The present invention seeks to realize through following technical scheme:
The quality determining method of compound houttuynin mixture of the present invention, this method comprises the steps:
A, need testing solution preparation
Get compound houttuynin mixture 20-30 parts by volume, add water saturated normal butyl alcohol jolting and extract 1-3 time, each 20-30 parts by volume; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 1-3 time, 20-30 parts by volume at every turn; Collect normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1 parts by volume makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance; Add methyl alcohol and process the mixed solution that per 1 parts by volume contains 0.0005-0.0015 weight portion, 0.0005-0.0015 weight portion, 0.0001-0.001 weight portion, 0.0001-0.001 weight portion, as mixing reference substance solution;
C, detection method
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test, draw above-mentioned need testing solution and mix each 0.001-0.01 parts by volume of reference substance solution, put respectively on same silica gel g thin-layer plate; With ethyl acetate-butanone-formic acid-water=2-8: 1-5: 0.5-1.5: 0.5-1.5 is developping agent, launches, and exhibition is apart from 8cm; Taking out, dry, is developping agent with toluene-ethyl acetate-methyl alcohol-formic acid=8-12: 1-5: 0.5-1.5: 1-3 again; Launch, exhibition is taken out apart from 12cm; Dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.
The quality determining method of compound houttuynin mixture of the present invention, this method comprises the steps:
A, need testing solution preparation
Get compound houttuynin mixture 25 parts by volume, add water saturated normal butyl alcohol jolting and extract 2 times, each 25 parts by volume merge normal butyl alcohol liquid; With the saturated water washing of normal butyl alcohol 2 times, each 25 parts by volume are collected normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1 parts by volume makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance; Add methyl alcohol and process the mixed solution that per 1 parts by volume contains 0.001 weight portion, 0.001 weight portion, 0.0005 weight portion, 0.0005 weight portion, as mixing reference substance solution;
C, detection method
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test, draw above-mentioned need testing solution and mix each 0.005 parts by volume of reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water=5: 3: 1: 1 was developping agent; Launch, exhibition is taken out apart from 8cm, dries; Again with toluene-ethyl acetate-methyl alcohol-formic acid=10: 3: 1: 2 is developping agent, launches, and exhibition is apart from 12cm; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.
The quality determining method of compound houttuynin mixture of the present invention, this method comprises the steps:
A, need testing solution preparation
Get compound houttuynin mixture 22 parts by volume, add water saturated normal butyl alcohol jolting and extract 3 times, each 28 parts by volume merge normal butyl alcohol liquid; With the saturated water washing of normal butyl alcohol 1 time, each 23 parts by volume are collected normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1 parts by volume makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance; Add methyl alcohol and process the mixed solution that per 1 parts by volume contains 0.0012 weight portion, 0.0007 weight portion, 0.0005 weight fraction, 0.0008 weight portion, as mixing reference substance solution;
C, detection method
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test, draw above-mentioned need testing solution and mix each 0.001-0.01 parts by volume of reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water=4: 4: 1.3: 0.8 developping agent; Launch, exhibition is taken out apart from 8cm, dries; Again with toluene-ethyl acetate-methyl alcohol-formic acid=11: 2: 0.8: 3 is developping agent, launches, and exhibition is apart from 12cm; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.
The quality determining method of compound houttuynin mixture of the present invention, this method comprises the steps:
A, need testing solution preparation
Get compound houttuynin mixture 28 parts by volume, add water saturated normal butyl alcohol jolting and extract 2 times, each 24 parts by volume merge normal butyl alcohol liquid; With the saturated water washing of normal butyl alcohol 2 times, each 24 parts by volume are collected normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1 parts by volume makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance; Add methyl alcohol and process the mixed solution that per 1 parts by volume contains 0.0006 weight portion, 0.0012 weight portion, 0.0008 weight portion, 0.0002 weight portion, as mixing reference substance solution;
C, detection method
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test, draw above-mentioned need testing solution and mix each 0.001-0.01 parts by volume of reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water=6: 2: 0.8: 1.1 was developping agent; Launch, exhibition is taken out apart from 8cm, dries; Again with toluene-ethyl acetate-methyl alcohol-formic acid=9: 4: 1.2: 1 is developping agent, launches, and exhibition is apart from 12cm; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.
The raw material and the preparation method of cordate houttuynia mixture are following:
Bulk drug is formed:
Cordate houttuynia 80-120 weight portion root of large-flowered skullcap 15-30 weight portion Radix Isatidis 15-30 weight portion
Capsule of weeping forsythia 7-12 weight portion honeysuckle 7-12 weight portion
Method for making: above five tastes medicinal material, boiling 1-3 time, each 1-2 hour, collecting decoction; Filter, filtrating is concentrated into the clear cream that relative density is 1.18-1.20 (60-80 a ℃), adds ethanol to containing the alcohol amount for 65-80%, stirs; Leave standstill, filter, decompression filtrate recycling ethanol also is concentrated into an amount of; Other gets sucrose 50-70 weight portion, processes simple syrup, adds above-mentioned soup, adds honey, Sodium Benzoate, ethyl hydroxy benzoate, mixing, and the adjustment total amount stirs to ormal weight, filters, can, sterilization promptly gets.
The raw material of cordate houttuynia mixture and preparation method are preferably following:
Bulk drug is formed:
The cordate houttuynia 100 weight portion roots of large-flowered skullcap 25 weight portion Radix Isatidis 25 weight portions
The capsule of weeping forsythia 10 weight portion honeysuckles 10 weight portions
Method for making: above five tastes medicinal material, boiling secondary, each 2 hours, collecting decoction; Filter, filtrating is concentrated into the clear cream that relative density is 1.18-1.20 (60-80 a ℃), and adding ethanol is 70% to containing the alcohol amount, stirs; Left standstill 24 hours, and filtered, decompression filtrate recycling ethanol also is concentrated into an amount of.Other gets sucrose 60 weight portions, processes simple syrup, adds above-mentioned soup, adds honey, Sodium Benzoate, ethyl hydroxy benzoate, mixing, and the adjustment total amount stirs to ormal weight, filters, can, sterilization promptly gets.
The relation of foregoing invention weight portion and parts by volume is the relation of g/ml.
The quality determining method of compound houttuynin mixture of the present invention carries out secondary through two kinds of different developping agents to sample and launches, and can differentiate scutelloside, chlorogenic acid, baicalein, four spots of wogonin simultaneously.The inventive method checking efficiency is high, cost is low, and practical value is high.
Description of drawings:
Fig. 1: the discrimination test figure under the former method chromatographic condition of compound houttuynin mixture
Fig. 2: the discrimination test figure under the radix scutellariae medicinal materials inspection method developping agent condition
Fig. 3: adopt secondary to launch identification experiment figure
Fig. 4: adopt secondary to launch to differentiate figure (specificity)
Fig. 5: repeated experiment figure (6 crowdes)
Fig. 6: repeated experiment figure (6 crowdes)
Experiment and embodiment are used to further specify but are not limited to the present invention below.
Experimental example one: the discrimination test under the former method chromatographic condition of compound houttuynin mixture
Each 25ml of compound houttuynin mixture (3 batches) of embodiment 1 preparation is got in the need testing solution preparation, adds water saturated normal butyl alcohol jolting respectively and extracts 2 times, each 25ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, 25ml at every turn; Collect normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.
Scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance are got in the reference substance solution preparation, add methyl alcohol and process the reference substance solution that every 1ml contains 1mg, 1mg, 0.5mg, 0.5mg respectively, promptly get.
Inspection method is according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (5: 3: 1: 1) be developping agent; Launch; Take out, dry, spray is with 2% ferric trichloride ethanolic solution.
Observe, the result shows: this chromatographic condition can be differentiated chlorogenic acid and scutelloside, but can not separate baicalein with wogonin, so can not differentiate baicalein and wogonin.See Fig. 1, its mid point 1 is chlorogenic acid reference substance 5ul; 2 is scutelloside reference substance 5ul; 3 is baicalein reference substance 5ul; 4 is wogonin reference substance 5ul; 5～7 is each 5ul of need testing solution.
Experimental example two: the discrimination test under the radix scutellariae medicinal materials inspection method developping agent condition
Each 25ml of compound houttuynin mixture (3 batches) of embodiment 1 preparation is got in the need testing solution preparation, adds water saturated normal butyl alcohol jolting respectively and extracts 2 times, each 25ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, 25ml at every turn; Collect normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.
Scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance are got in the reference substance solution preparation, add methyl alcohol and process the reference substance solution that every 1ml contains 1mg, 1mg, 0.5mg, 0.5mg respectively, promptly get.
Inspection method is according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-methyl alcohol-formic acid (10: 3: 1: 2) be developping agent; Launch; Take out, dry, spray is with 2% ferric trichloride ethanolic solution.
Observe, the result shows: this chromatographic condition can be differentiated baicalein and wogonin, but can not separate chlorogenic acid with scutelloside, so can not detect chlorogenic acid and scutelloside.See accompanying drawing 2.Its mid point 1 is chlorogenic acid reference substance 5ul; 2 is scutelloside reference substance 5ul; 3 is baicalein reference substance 5ul; 4 is wogonin reference substance 5ul; 5～7 is each 5ul of need testing solution.
Experimental example three: adopt secondary to launch identification experiment (preliminary experiment)
Each 25ml of compound houttuynin mixture (3 batches) of embodiment 1 preparation is got in the need testing solution preparation, adds water saturated normal butyl alcohol jolting respectively and extracts 2 times, each 25ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, 25ml at every turn; Collect normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.
Scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance are got in the reference substance solution preparation, add methyl alcohol and process the reference substance solution that every 1ml contains 1mg, 1mg, 0.5mg, 0.5mg respectively, promptly get.
Inspection method is drawn each 5 μ l of above-mentioned two kinds of solution according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test, puts respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (5: 3: 1: 1) be developping agent; Launch, exhibition is taken out apart from 8cm, dries; (10: 3: 1: 2) be developping agent, expansion was opened up apart from 12cm with toluene-ethyl acetate-methyl alcohol-formic acid again; Take out, dry, spray is with 2% ferric trichloride ethanolic solution.
Observe, the result shows: in the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.See Fig. 3.Its mid point 1 is chlorogenic acid reference substance 5ul; 2 is scutelloside reference substance 5ul; 3 is baicalein reference substance 5ul; 4 is wogonin reference substance 5ul; 5～7 is each 5ul of need testing solution.
Experimental example four: adopt secondary to launch identification experiment (specificity)
Each 25ml of compound houttuynin mixture (3 batches) of embodiment 1 preparation is got in the need testing solution preparation, adds water saturated normal butyl alcohol jolting respectively and extracts 2 times, each 25ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, 25ml at every turn; Collect normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.
The negative sample 25ml that lacks the root of large-flowered skullcap is got in the preparation that lacks root of large-flowered skullcap need testing solution, adds water saturated normal butyl alcohol jolting and extracts 2 times, each 25ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, 25ml at every turn; Collect normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as scarce root of large-flowered skullcap need testing solution.
Mix the reference substance solution preparation and get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance, add methyl alcohol and process the mixed solution that every 1ml contains 1mg, 1mg, 0.5mg, 0.5mg, as mixing reference substance solution.
Inspection method is drawn each 5 μ l of above-mentioned three kinds of solution according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test, puts respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (5: 3: 1: 1) be developping agent; Launch, exhibition is taken out apart from 8cm, dries; (10: 3: 1: 2) be developping agent, expansion was opened up apart from 12cm with toluene-ethyl acetate-methyl alcohol-formic acid again; Take out, dry, spray is with 2% ferric trichloride ethanolic solution.
Observe; The result shows: in the test sample chromatogram; With mix the spot that contrast chromatogram corresponding position detects scutelloside, baicalein, wogonin; In lacking the negative sample chromatogram of the root of large-flowered skullcap, do not detect the spot of scutelloside, baicalein, wogonin, it is strong to explain that this method detects the specificity of scutelloside, baicalein, wogonin.The chlorogenic acid spot is total spot.See Fig. 4.Wherein 1 is that mixing reference substance 5ul, 2～4 is that each 5ul of need testing solution, 5 is for lacking root of large-flowered skullcap need testing solution 5ul.
Experimental example five: repeated experiment
1, sample determination (6 batches)
Lot number is respectively: 110714102,110708103,110719103,110720103,110709102,110717102;
Each 25ml of compound houttuynin mixture (6 batches) of embodiment 1 preparation is got in the need testing solution preparation, adds water saturated normal butyl alcohol jolting respectively and extracts 2 times, each 25ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, 25ml at every turn; Collect normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.
Mix the reference substance solution preparation and get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance, add methyl alcohol and process the mixed solution that every 1ml contains 1mg, 1mg, 0.5mg, 0.5mg, as mixing reference substance solution.
Inspection method is drawn each 5 μ l of above-mentioned two kinds of solution according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test, puts respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (5: 3: 1: 1) be developping agent; Launch, exhibition is taken out apart from 8cm, dries; (10: 3: 1: 2) be developping agent, expansion was opened up apart from 12cm with toluene-ethyl acetate-methyl alcohol-formic acid again; Take out, dry, spray is with 2% ferric trichloride ethanolic solution.
Observe, the result shows: in the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.See Fig. 5.Wherein 1 for mixing reference substance 5ul; 2 is each 5ul lot number of need testing solution: 110711102; 3 is each 5ul lot number of need testing solution: 110708103; 4 is each 5ul lot number of need testing solution: 110719103; 5 is each 5ul lot number of need testing solution: 110720103; 6 is each 5ul lot number of need testing solution: 110709102; 7 is each 5ul lot number of need testing solution: 110717102
2, sample determination (6 batches again)
The need testing solution preparation: method is with 1.Lot number: 110715103,110721103,110716103,110718103,11011601,11011602.
Mix the reference substance solution preparation: method is with 1.
Inspection method: method is with 1.
Observe, the result shows: in the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.See Fig. 6.Wherein 1 for mixing reference substance 5ul; 2 is each 5ul lot number of need testing solution: 110715103; 3 is each 5ul lot number of need testing solution: 110721103; 4 is each 5ul lot number of need testing solution: 110716103; 5 is each 5ul lot number of need testing solution: 110718103; 6 is each 5ul lot number of need testing solution: 11011601; 7 is each 5ul lot number of need testing solution: 11011602.Following embodiment is used to further specify but is not limited to the present invention.
Embodiment one:
Cordate houttuynia 100g root of large-flowered skullcap 25g Radix Isatidis 25g
Capsule of weeping forsythia 10g honeysuckle 10g
Method for making: above five tastes medicinal material, boiling secondary, each 2 hours, collecting decoction; Filter, filtrating is concentrated into the clear cream that relative density is 1.18-1.20 (60-80 a ℃), and adding ethanol is 70% to containing the alcohol amount, stirs; Left standstill 24 hours, and filtered, decompression filtrate recycling ethanol also is concentrated into an amount of.Other gets sucrose 60 weight portions, processes simple syrup, adds above-mentioned soup, adds honey, Sodium Benzoate, ethyl hydroxy benzoate, mixing, and the adjustment total amount stirs to ormal weight, filters, can, sterilization promptly gets.
A, need testing solution preparation
Get compound houttuynin mixture 25ml, add water saturated normal butyl alcohol jolting and extract 2 times, each 25ml merges normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, and each 25ml, collection normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance, add methyl alcohol and process the mixed solution that every 1ml contains 0.001g, 0.001g, 0.0005g, 0.0005g, as mixing reference substance solution;
C, detection method
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test, draw each 0.005ml of above-mentioned need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water=5: 3: 1: 1 was developping agent; Launch, exhibition is taken out apart from 8cm, dries; Again with toluene-ethyl acetate-methyl alcohol-formic acid=10: 3: 1: 2 is developping agent, launches, and exhibition is apart from 12cm; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.
Embodiment two:
Cordate houttuynia 100g root of large-flowered skullcap 25g Radix Isatidis 25g
Capsule of weeping forsythia 10g honeysuckle 10g
Method for making: above five tastes medicinal material, boiling secondary, each 2 hours, collecting decoction; Filter, filtrating is concentrated into the clear cream that relative density is 1.18-1.20 (60-80 a ℃), and adding ethanol is 70% to containing the alcohol amount, stirs; Left standstill 24 hours, and filtered, decompression filtrate recycling ethanol also is concentrated into an amount of.Other gets sucrose 60 weight portions, processes simple syrup, adds above-mentioned soup, adds honey, Sodium Benzoate, ethyl hydroxy benzoate, mixing, and the adjustment total amount stirs to ormal weight, filters, can, sterilization promptly gets.
A, need testing solution preparation
Get compound houttuynin mixture 22ml, add water saturated normal butyl alcohol jolting and extract 3 times, each 28ml merges normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 1 time, and each 23ml, collection normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance, add methyl alcohol and process the mixed solution that every 1ml contains 0.0012g, 0.0007g, 0.0005g, 0.0008g, as mixing reference substance solution;
C, detection method
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test, draw each 0.001-0.01ml of above-mentioned need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water=4: 4: 1.3: 0.8 developping agent; Launch, exhibition is taken out apart from 8cm, dries; Again with toluene-ethyl acetate-methyl alcohol-formic acid=11: 2: 0.8: 3 is developping agent, launches, and exhibition is apart from 12cm; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.
Embodiment three:
Cordate houttuynia 100g root of large-flowered skullcap 25g Radix Isatidis 25g
Capsule of weeping forsythia 10g honeysuckle 10g
Method for making: above five tastes medicinal material, boiling secondary, each 2 hours, collecting decoction; Filter, filtrating is concentrated into the clear cream that relative density is 1.18-1.20 (60-80 a ℃), and adding ethanol is 70% to containing the alcohol amount, stirs; Left standstill 24 hours, and filtered, decompression filtrate recycling ethanol also is concentrated into an amount of.Other gets sucrose 60 weight portions, processes simple syrup, adds above-mentioned soup, adds honey, Sodium Benzoate, ethyl hydroxy benzoate, mixing, and the adjustment total amount stirs to ormal weight, filters, can, sterilization promptly gets.
A, need testing solution preparation
Get compound houttuynin mixture 28ml, add water saturated normal butyl alcohol jolting and extract 2 times, each 24ml merges normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, and each 24ml, collection normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance, add methyl alcohol and process the mixed solution that every 1ml contains 0.0006g, 0.0012g, 0.0008g, 0.0002g, as mixing reference substance solution;
C, detection method
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B) test, draw each 0.001-0.01ml of above-mentioned need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water=6: 2: 0.8: 1.1 was developping agent; Launch, exhibition is taken out apart from 8cm, dries; Again with toluene-ethyl acetate-methyl alcohol-formic acid=9: 4: 1.2: 1 is developping agent, launches, and exhibition is apart from 12cm; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.
Claims (7)
1. the quality determining method of a compound houttuynin mixture is characterized in that this method comprises the steps:
A, need testing solution preparation
Get compound houttuynin mixture 20-30 parts by volume, add water saturated normal butyl alcohol jolting and extract 1-3 time, each 20-30 parts by volume; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 1-3 time, 20-30 parts by volume at every turn; Collect normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1 parts by volume makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance; Add methyl alcohol and process the mixed solution that per 1 parts by volume contains 0.0005-0.0015 weight portion, 0.0005-0.0015 weight portion, 0.0001-0.001 weight portion, 0.0001-0.001 weight portion, as mixing reference substance solution;
C, detection method
According to the thin-layered chromatography test, draw each 0.001-0.01 parts by volume of above-mentioned need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, be developping agent with ethyl acetate-butanone-formic acid-water=2-8: 1-5: 0.5-1.5: 0.5-1.5; Launch, exhibition is taken out apart from 8cm, dries; Be developping agent with toluene-ethyl acetate-methyl alcohol-formic acid=8-12: 1-5: 0.5-1.5: 1-3 again, launch that exhibition is apart from 12cm; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color;
The compound houttuynin mixture is processed by following method:
Cordate houttuynia 80-120 weight portion root of large-flowered skullcap 15-30 weight portion Radix Isatidis 15-30 weight portion
Capsule of weeping forsythia 7-12 weight portion honeysuckle 7-12 weight portion
Method for making: above five tastes medicinal material, boiling 1-3 time, each 1-2 hour, collecting decoction; Filter, filtrating is concentrated into the clear cream that relative density is 1.18-1.20 under 60-80 ℃, adds ethanol to containing the alcohol amount for 65-80%, stirs; Leave standstill, filter, decompression filtrate recycling ethanol also is concentrated into an amount of; Other gets sucrose 50-70 weight portion, processes simple syrup, adds above-mentioned soup, adds honey, Sodium Benzoate, ethyl hydroxy benzoate, mixing, and the adjustment total amount stirs to ormal weight, filters, can, sterilization promptly gets.
2. the quality determining method of compound houttuynin mixture as claimed in claim 1 is characterized in that this method comprises the steps:
A, need testing solution preparation
Get compound houttuynin mixture 25 parts by volume, add water saturated normal butyl alcohol jolting and extract 2 times, each 25 parts by volume merge normal butyl alcohol liquid; With the saturated water washing of normal butyl alcohol 2 times, each 25 parts by volume are collected normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1 parts by volume makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance; Add methyl alcohol and process the mixed solution that per 1 parts by volume contains 0.001 weight portion, 0.001 weight portion, 0.0005 weight portion, 0.0005 weight portion, as mixing reference substance solution;
C, detection method
According to thin-layered chromatography test, draw above-mentioned need testing solution and mix each 0.005 parts by volume of reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water=5: 3: 1: 1 was developping agent; Launch, exhibition is taken out apart from 8cm, dries; Again with toluene-ethyl acetate methanol-formic acid=10: 3: 1: 2 is developping agent, launches, and exhibition is apart from 12cm; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.
3. the quality determining method of compound houttuynin mixture as claimed in claim 1 is characterized in that this method comprises the steps:
A, need testing solution preparation
Get compound houttuynin mixture 22 parts by volume, add water saturated normal butyl alcohol jolting and extract 3 times, each 28 parts by volume merge normal butyl alcohol liquid; With the saturated water washing of normal butyl alcohol 1 time, each 23 parts by volume are collected normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1 parts by volume makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance; Add methyl alcohol and process the mixed solution that per 1 parts by volume contains 0.0012 weight portion, 0.0007 weight portion, 0.0005 weight portion, 0.0008 weight portion, as mixing reference substance solution;
C, detection method
According to thin-layered chromatography test, draw above-mentioned need testing solution and mix each 0.001-0.01 parts by volume of reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water=4: 4: 1.3: 0.8 developping agent; Launch, exhibition is taken out apart from 8cm, dries; Again with toluene-ethyl acetate-methyl alcohol-formic acid=11: 2: 0.8: 3 is developping agent, launches, and exhibition is apart from 12cm; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.
4. the quality determining method of compound houttuynin mixture as claimed in claim 1 is characterized in that this method comprises the steps:
A, need testing solution preparation
Get compound houttuynin mixture 28 parts by volume, add water saturated normal butyl alcohol jolting and extract 2 times, each 24 parts by volume merge normal butyl alcohol liquid; With the saturated water washing of normal butyl alcohol 2 times, each 24 parts by volume are collected normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1 parts by volume makes dissolving, as need testing solution;
B, the preparation of mixing reference substance solution
Get scutelloside reference substance, chlorogenic acid reference substance, baicalein reference substance, wogonin reference substance; Add methyl alcohol and process the mixed solution that per 1 parts by volume contains 0.0006 weight portion, 0.0012 weight portion, 0.0008 weight portion, 0.0002 weight portion, as mixing reference substance solution;
C, detection method
According to thin-layered chromatography test, draw above-mentioned need testing solution and mix each 0.001-0.01 parts by volume of reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone formic acid-water=6: 2: 0.8: 1.1 was developping agent; Launch, exhibition is taken out apart from 8cm, dries; Again with toluene-ethyl acetate-methyl alcohol-formic acid=9: 4: 1.2: 1 is developping agent, launches, and exhibition is apart from 12cm; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, respectively with the corresponding position of reference substance chromatogram on, show the spot of same color.
5. like the quality determining method of the arbitrary described compound houttuynin mixture of claim 1-4, it is characterized in that the raw material of the cordate houttuynia mixture in this method consists of:
The cordate houttuynia 100 weight portion roots of large-flowered skullcap 25 weight portion Radix Isatidis 25 weight portions
The capsule of weeping forsythia 10 weight portion honeysuckles 10 weight portions.
6. like the quality determining method of the arbitrary described compound houttuynin mixture of claim 1-4, it is characterized in that the cordate houttuynia mixture in this method is processed by following method:
Above five tastes medicinal material, boiling secondary, each 2 hours, collecting decoction; Filter, filtrating is concentrated into the clear cream that relative density is 1.18-1.20 under 60-80 ℃, and adding ethanol is 70% to containing the alcohol amount, stirs; Left standstill 24 hours, and filtered, decompression filtrate recycling ethanol also is concentrated into an amount of.Other gets sucrose 60 weight portions, processes simple syrup, adds above-mentioned soup, adds honey, Sodium Benzoate, ethyl hydroxy benzoate, mixing, and the adjustment total amount stirs to ormal weight, filters, can, sterilization promptly gets.
7. the quality determining method of compound houttuynin mixture as claimed in claim 5 is characterized in that the cordate houttuynia mixture in this method is processed by following method:
Above five tastes medicinal material, boiling secondary, each 2 hours, collecting decoction; Filter, filtrating is concentrated into the clear cream that relative density is 1.18-1.20 under 60-80 ℃, and adding ethanol is 70% to containing the alcohol amount, stirs; Left standstill 24 hours, and filtered, decompression filtrate recycling ethanol also is concentrated into an amount of.Other gets sucrose 60 weight portions, processes simple syrup, adds above-mentioned soup, adds honey, Sodium Benzoate, ethyl hydroxy benzoate, mixing, and the adjustment total amount stirs to ormal weight, filters, can, sterilization promptly gets.
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