CN101513467A - Method for controlling quality of dermatosis toxemia preparation - Google Patents
Method for controlling quality of dermatosis toxemia preparation Download PDFInfo
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Abstract
The invention discloses a method for controlling the quality of dermatosis toxemia preparation, wherein the preparation consists of Chinese medicines, namely gamene, peach kernel, schizonepeta spike (char), snake slough (wine fried), red paeonia, angelica, rhizoma imperatae, fructus kochiae, fructus xanthil (fried), radix rehmanniae, forsythia, honeysuckle, corydlis bungeana, glabrous greenbrier rhizome, phellodendron, spina gleditsiae, ballonflower, motherwort, bitter almond (fried without peel), ledebouriella seseloides, poria cocos, radix paeoniae alba, cicada slough, burdock (fried), tree peony bark, dittany bark, prepared radix rehmanniae, rhubarb (wine fried), caulis lonicerae, radix arnebiae seu lithospermi, rhizoma bolbostemmae, hemlock parsley (wine fried), liquorice, angelica dahurica, radix semiaquilegiae, cortex cercis chinensis, spatholobus stem, lemna polyrhiza L and safflower. The method identifies phellodendron, rhubarb, red paeonia, radix paeoniae alba, tree peony bark, forsythia, rhizoma imperatae, ballonflower and burdock by thin-layer chromatography, and carries out content test by using berberine hydrochloride as an index according to high performance liquid chromatography. The method ensures accuracy and advance of quality test on the dermatosis toxemia preparation, and plays a role in controlling the quality of industrial mass production of the preparation, thereby ensuring the clinical efficacy of the preparation.
Description
One, technical field
The present invention relates to the method for quality control field of Chinese medicine preparation, be specifically related to the method for quality control of dermatosis toxemia preparation.
Two, background technology
The dermatosis toxemia preparation crude drug is by the Chinese crude drug Radix Rubiae, Semen Persicae, Herba Schizonepetae (charcoal), Periostracum Serpentis (wine is processed), Radix Paeoniae Rubra, Radix Angelicae Sinensis, Rhizoma Imperatae, the Fructus Kochiae, Fructus Xanthii (stir-fry), Radix Rehmanniae, Fructus Forsythiae, Flos Lonicerae, Herba Corydalis Bungeanae, Rhizoma Smilacis Glabrae, Cortex Phellodendri, Spina Gleditsiae, Radix Platycodonis, Herba Leonuri, Semen Armeniacae Amarum (peeling is fried), Radix Saposhnikoviae, Poria, the Radix Paeoniae Alba, Periostracum Cicadae, Fructus Arctii (stir-fry), Cortex Moutan, Cortex Dictamni, Radix Rehmanniae Preparata, Radix Et Rhizoma Rhei (wine stir-fry), Caulis Lonicerae, Radix Arnebiae (Radix Lithospermi), Rhizoma Bolbostematis, Rhizoma Chuanxiong (wine is processed), Radix Glycyrrhizae, the Radix Angelicae Dahuricae, Radix Semiaquilegiae, Cortex cercis chinensis, Caulis Spatholobi, Herba Spirodelae, compositions such as Flos Carthami, in order to control product quality effectively, we have set up the method for quality control of preparation, this method adopts according to thin layer chromatography Cortex Phellodendri, Radix Et Rhizoma Rhei, Radix Paeoniae Rubra, the Radix Paeoniae Alba, Cortex Moutan, Fructus Forsythiae, Rhizoma Imperatae, Radix Platycodonis, Fructus Arctii is differentiated, and the photograph high performance liquid chromatography is that index is carried out assay with the berberine hydrochloride, this method of quality control has guaranteed the accuracy and the advance of dermatosis toxemia preparation quality inspection standard, can effectively guarantee the quality of dermatosis toxemia preparation, said preparation quality in industrialized great production is effectively controlled.
Three, summary of the invention
The method of quality control that the objective of the invention is to open dermatosis toxemia preparation.
Method of quality control of the present invention comprises following discriminating and/or content assaying method.
Discrimination method of the present invention is one or more of following method:
1.. get dermatosis toxemia preparation 7.2g, porphyrize adds methanol 15~35ml, puts in the water-bath reflux 10~30 minutes, filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-methanol-isopropyl alcohol-water (5~7: 2~4: 1~3: 1~2: 0.15~0.45) be developing solvent, under the ammonia saturated with vapor, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
2.. get dermatosis toxemia preparation 4.8g, porphyrize adds methanol 5~25ml, supersound process 10~30 minutes filters the filtrate evaporate to dryness, residue adds water 5~15ml makes dissolving, adds hydrochloric acid 0.5~1.5ml, puts and heats 20~40 minutes in the water-bath, take out, cooling immediately adds diethyl ether and extracts 1~3 time, each 5~15ml merges ether solution, evaporate to dryness, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, adds methanol and shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (14~16: 4~6: upper strata liquid 0.5~1.5) is developing solvent with petroleum ether (30~60 ℃ of petroleum ether)-Ethyl formate-formic acid, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show five identical same color fluorescence speckles; Put in the ammonia smoked after, speckle becomes redness.
3.. get dermatosis toxemia preparation 21.6g, porphyrize adds methanol 20~40ml, and supersound process 20~40 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rubiae control medicinal material 1g, adds methanol 10~30ml, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60~90 ℃)-acetone (3~5: 0.5~1.5) be developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
4.. get dermatosis toxemia preparation 14.4g, porphyrize adds methanol 20~40ml, puts in the water-bath reflux 20~40 minutes, puts coldly, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-ethyl acetate (7~9: 3~5: 0.5~1.5) be developing solvent, under the ammonia saturated with vapor, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing in 100 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
5.. get dermatosis toxemia preparation 28.8g, porphyrize, the 25~75ml that adds diethyl ether, low temperature reflux is 0.5~1.5 hour in the water-bath, filters, and filtrate volatilizes, and the residue 1ml that adds diethyl ether makes dissolving, as need testing solution; Other gets Rhizoma Imperatae control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with the chloroform, launch, take out, to dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.
6.. get dermatosis toxemia preparation 21.6g, porphyrize adds methanol 25~75ml, puts in the water-bath reflux 0.5~1.5 hour, filter, filtrate evaporate to dryness, residue add methanol 4~6ml makes dissolving, adds active carbon 0.5~1.5g, jolting 5~15 minutes filters, and filtrate is concentrated into about 2ml as need testing solution; Other gets the phillyrin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-chloroform-toluene-methanol (4~6: 2~4: 4~6: 2~4) be developing solvent, presaturation launched after 20~40 minutes, took out, and dried, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical speckle.
7.. get dermatosis toxemia preparation 7.2g, porphyrize adds hydrochloric acid 2~4ml and chloroform 25~75ml, puts in the water-bath reflux 0.5~1.5 hour, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets Radix Platycodonis control medicinal material 0.2g, makes control medicinal material solution by the need testing solution method for making; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30~60 ℃)-ethyl acetate-glacial acetic acid (15~35: 6~8: 0.25~0.75) be developing solvent, launch, take out, dry, (0.5~1.5: 9~11), it is clear to be heated to the speckle colour developing at 105 ℃ with the mixed solution of 8% vanillin alcoholic solution and sulfuric acid solution (7 → 10) in spray; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
8.. get dermatosis toxemia preparation 28.8g, porphyrize adds ethyl acetate 50~70ml, and supersound process 20~40 minutes filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (30~50: 9~11: lower floor's solution 0.5~1.5) is developing solvent, launches, and takes out, and dries with chloroform-methanol-water; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Content assaying method of the present invention is following method:
According to high effective liquid chromatography for measuring; With the octadecylsilane chemically bonded silica is filler; With acetonitrile-0.05mol/L potassium dihydrogen phosphate (40~45: 55~60, add dodecyl sodium sulfate 1.7g in every 1000ml solution) is mobile phase, and the detection wavelength is 265 ± 2nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 6000; The preparation of reference substance solution: get the berberine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 0.01mg, promptly; The preparation of need testing solution: get dermatosis toxemia preparation, porphyrize is got the about 1.5g of fine powder, the accurate title, decide, and puts in the tool plug conical flask, and precision adds methanol-hydrochloric acid (100: 1) 25~75ml, claim to decide weight, supersound process 20~40 minutes is taken out, cool, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, get supernatant and filter, promptly with microporous filter membrane (0.45 μ m); Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
The thin layer chromatography that the invention provides Cortex Phellodendri, Radix Et Rhizoma Rhei, Radix Paeoniae Rubra, the Radix Paeoniae Alba, Cortex Moutan, Fructus Forsythiae, Rhizoma Imperatae, Radix Platycodonis, Fructus Arctii is differentiated, selected in the Cortex Phellodendri effective ingredient berberine hydrochloride to set up the content assaying method of dermatosis toxemia preparation as the assay index; Through repeated trials repeatedly, confirmation method is easy, repeatability is good, the result accurately and reliably, can be used as the dermatosis toxemia preparation quality control index.
The used preparation of test sample adopts embodiment 1 described dermatosis toxemia sheet in the experimental example of the present invention, and also available have other preparations that same materials is formed with the described dermatosis toxemia sheet of embodiment.
Experimental example:
The assay of berberine hydrochloride
The dermatosis toxemia sheet is a big compound preparation, and square Chinese crude drug consumption is all less, and the content of its composition is also lower.Through experimental study, content of paeoniflorin is higher in the dermatosis toxemia sheet, but because peoniflorin all contains in Radix Paeoniae Rubra, the Radix Paeoniae Alba and Cortex Moutan, specificity is not strong, should not be elected to be the index components of assay; The content of berberine hydrochloride is also higher in the dermatosis toxemia sheet, and the berberine composition is exclusive by Cortex Phellodendri among the we, and specificity is stronger.Its merit of Cortex Phellodendri is in heat clearing and damp drying, and pathogenic fire purging removes steams, and skin ulcer is treated in detoxifcation.Be the principal agent among the we, therefore, can be used as the index components of assay.According to documents and materials, the content difference of berberine composition is bigger in the Cortex Phellodendri, and the content of berberine scope in the Cortex Phellodendri of the different places of production is 0.8~5.0%.In order to control medical material and finished medicines quality better, we adopt high performance liquid chromatography that wherein berberine is carried out assay, and determine with berberine hydrochloride (C
20H
17NO
4That HCl) counts the dermatosis toxemia sheet contains the survey index components.This method has highly sensitive, and sampling amount is few, and measurement result is accurate, favorable reproducibility, response rate advantages of higher.Below sum up for its methodological study.
1. instrument and reagent
Instrument: TSP type high performance liquid chromatograph, P2000 type pump, UV1000 type UV-detector.
Reagent: acetonitrile is a chromatographically pure, and water is double distilled water, and other reagent is analytical pure.
Reference substance: berberine hydrochloride, buy by Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
Test sample: the dermatosis toxemia sheet, specification: every heavy 0.6g is made by embodiment 1.
2. chromatographic condition
Chromatographic column: Kromasil C-18 post,
250 * 4.6mm;
Mobile phase: acetonitrile-0.05mol/L potassium dihydrogen phosphate (42: 58, add dodecyl sodium sulfate 1.7g in every 100ml solution).
Detect wavelength: get berberine hydrochloride reference substance solution (C=0.0105mg/ml), carry out continuous wavelength scanning from 200~400nm with ultraviolet spectrophotometer.The result shows that the berberine hydrochloride reference substance has 3 absworption peaks at 230.0nm, 265.0nm and 350.0nm wavelength place, and our reference literature is reported and thought, 230.0nm though the light absorption of locating is strong, but its wavelength is shorter, in the sample under this wavelength a lot of materials strong absorption, serious interference are all arranged.A little less than the absorption slightly at 350.0nm wavelength place.So select for use λ=265nm as detecting wavelength.
Under above-mentioned analysis condition, the separating degree of berberine hydrochloride peak and adjacent impurity peaks is greater than more than 1.5, and number of theoretical plate is greater than 6000.
3. reference substance purity test
The berberine hydrochloride reference substance of preparation finite concentration (C=0.0105mg/ml) injects chromatograph of liquid, measures in accordance with the law, calculates by area normalization method, and its content is 99.8%.
4. extraction conditions is selected and is extracted completeness and investigate
(1) extract the choice of Solvent berberine hydrochloride and dissolve in hot water, slightly soluble in water or ethanol dissolves in methanol, and soluble,very slightly in chloroform is insoluble in ether.Therefore, we have designed with methanol, acidic methanol and have refluxed, and methods such as methanol, acidic methanol supersound extraction compare test.Take by weighing same batch sample, make sample solution with volume with method, measure by above-mentioned chromatographic condition in accordance with the law, result of the test is asked for an interview table 1
Table 1 extracts choice of Solvent test and result
Result of the test shows that the measurement result of acidic methanol (hydrochloric acid-methanol 1: 100) solvent system supersound process is higher, so select the extraction solvent of acidic methanol solvent system as this method.Select the extracting method of supersound process as this method.
(2) extract the completeness investigation and take by weighing the about 1.5g of same batch sample, precision adds each 50ml of methanol-hydrochloric acid (100: 1), and supersound process is 10,20,30,40 minutes respectively, measures by the text method in accordance with the law, and result of the test is asked for an interview table 2
Table 2 extracts completeness test and result
Result of the test shows that supersound process was extracted after 30 minutes, and its assay result increases not obvious, illustrates substantially and extracts fully, so select the acidic methanol solvent system 30 minutes supersound extraction time as this method of supersound process.
5. methodological study
(1) the accurate absorption of the investigation of linear relationship and scope concentration is reference substance solution 4,8,12,16, the 20 μ l of 0.0105mg/ml, injects chromatograph of liquid respectively, measures in accordance with the law.The result asks for an interview table 3.With the sample size is abscissa, and peak area value is a vertical coordinate, the drawing standard curve, and carry out rectilinear regression, regression equation is Y=3598052.9X+8655.14, r=0.9996.Result of the test shows that this method sample size is good linear relationship in 0.042~0.21 μ g scope.
Table 3 linear relationship is investigated the result
(2) the accurate absorption of precision test concentration is the reference substance solution 10 μ l of C=0.0105mg/ml, repeats sample introduction continuously 5 times, measures the peak area integrated value, and result of the test is asked for an interview table 4
Test of table 4 precision and result
Result of the test shows that the berberine hydrochloride reference substance repeats sample introduction 5 times, records relative standard deviation RSD<2.0% of peak area integrated value, so think that this method has good precision.
(3) the simulation prescription of removing Cortex Phellodendri is got in negative blank test, makes the blank sample that does not contain Cortex Phellodendri, makes blank solution by the need testing solution method for making.Other gets need testing solution and reference substance solution (C=0.0105mg/ml), presses the text method and injects chromatograph of liquid, measures in accordance with the law.Result of the test shows, in the test sample chromatograph, with the corresponding retention time of reference substance chromatograph position on, the single chromatographic peak of a correspondence is arranged, and in the blank liquid chromatography, does not have corresponding peak in this retention time corresponding position and occur.Illustrate that negative blank is noiseless to its mensuration, the specificity of its method is better.
(4) accurate each 10 μ l of berberine hydrochloride reference substance solution that draw need testing solution and same concentration (C=0.0105mg/ml) of stability test, respectively by 0,0.5,1,2,4, hour interval, inject chromatograph of liquid respectively, measure in accordance with the law, result of the test is asked for an interview table 5
Test of table 5 study on the stability and result
Result of the test shows that berberine hydrochloride is measured through this method in reference substance and the sample, and quite stable in 4 hours, its relative standard deviation is respectively RSD=1.23% and RSD=1.78%.
(5) the replica test precision takes by weighing the about 1.5g of sample fine powder, repeats 5 parts, measures respectively by the text content assaying method in accordance with the law, and result of the test is asked for an interview table 6
Test of table 6 sample repeatability and result
Result of the test shows, the average content that repeats to record this batch sample for 5 times is the 0.2291mg/ sheet, and its relative standard deviation is RSD=0.97% by statistics.The repeatability of presentation of results this method is better.
(6) the application of sample recovery test adopts application of sample recovery test method.Precision takes by weighing with a collection of (lot number: 20020901) known content (0.2291mg/ sheet, average sheet heavily is 0.6019g, amount to 0.3806mg/g) the about 0.75g of dermatosis toxemia sheet sample fine powder, the accurate respectively about 0.2~0.3mg of berberine hydrochloride reference substance that adds, measure by the text content assaying method, result of the test is asked for an interview table 7 in accordance with the law
Table 7 application of sample recovery test and result
Result of the test shows that this method has the higher response rate, and its average recovery rate is 98.92%, and relative standard deviation is 1.85%.
6. berberine hydrochloride content in the sample
Get ten batch samples, carry out berberine hydrochloride content by the text method, the result asks for an interview table 8
Table 80 batch sample assay results (n=2)
Following embodiment all can reach the effect of above-mentioned experimental example.
Four, the specific embodiment
Embodiment 1:
[prescription] Radix Rubiae 16g, Semen Persicae 16g, Herba Schizonepetae (charcoal) 16g, Periostracum Serpentis (wine is processed) 8g, Radix Paeoniae Rubra 16g, Radix Angelicae Sinensis 16g, Rhizoma Imperatae 32g, Fructus Kochiae 16g, Fructus Xanthii (stir-fry) 16g, Radix Rehmanniae 16g, Fructus Forsythiae 16g, Flos Lonicerae 16g, Herba Corydalis Bungeanae 16g, Rhizoma Smilacis Glabrae 16g, Cortex Phellodendri 8g, Spina Gleditsiae 16g, Radix Platycodonis 16g, Herba Leonuri 16g, Semen Armeniacae Amarum (peeling is fried) 16g, Radix Saposhnikoviae 8g, Poria 32g, Radix Paeoniae Alba 16g, Periostracum Cicadae 8g, Fructus Arctii (stir-fry) 16g, Cortex Moutan 16g, Cortex Dictamni 16g, Radix Rehmanniae Preparata 16g, Radix Et Rhizoma Rhei (wine stir-fry) 16g, Caulis Lonicerae 16g, Radix Arnebiae (Radix Lithospermi) 8g, Rhizoma Bolbostematis 16g, Rhizoma Chuanxiong (wine is processed) 8g, Radix Glycyrrhizae 16g, Radix Angelicae Dahuricae 8g, Radix Semiaquilegiae 16g, Cortex cercis chinensis 8g, Caulis Spatholobi 16g, Herba Spirodelae 8g, Flos Carthami 8g
[method for making] above 39 flavors are ground into fine powder, sieve, and mixing is granulated in right amount with simple syrup, and drying adds Pulvis Talci, and mixing is pressed into 1000, coating, and drying, promptly.
12 of this product are got in [discriminating] (1), and porphyrize adds methanol 25ml, put in the water-bath reflux 20 minutes, filter, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution.Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, shines medical material solution in pairs with legal system.Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-methanol-isopropyl alcohol-water (6: 3: 2: 1.5: 0.3) is developing solvent, under the ammonia saturated with vapor, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(2) get 8 of this product, porphyrize adds methanol 15ml, supersound process 20 minutes filters the filtrate evaporate to dryness, residue adds water 10ml makes dissolving, adds hydrochloric acid 1ml, puts in the water-bath and heats 30 minutes, take out, cooling immediately adds diethyl ether and extracts 2 times, each 10ml merges ether solution, evaporate to dryness, residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, adds methanol and shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, upper strata liquid with petroleum ether (30~60 ℃ of petroleum ether)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show five identical fluorescent orange speckles; Put in the ammonia smoked after, speckle becomes redness.
(3) get 36 of this product, porphyrize adds methanol 30ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Rubiae control medicinal material 1g, adds methanol 20ml, shines medical material solution in pairs with legal system.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 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 petroleum ether (60~90 ℃)-acetone (4: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(4) get 24 of this product, porphyrize adds methanol 30ml, puts in the water-bath reflux 30 minutes, puts coldly, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-ethyl acetate (8: 4: 1) is developing solvent, under the ammonia saturated with vapor, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing in 100 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the bluish violet speckle of same color.
(5) get 48 of this product, porphyrize, the 50ml that adds diethyl ether, low temperature reflux is 1 hour in the water-bath, filters, and filtrate volatilizes, and the residue 1ml that adds diethyl ether makes dissolving, as need testing solution.Other gets Rhizoma Imperatae control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with the chloroform is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.
(6) get 36 of this product, porphyrize adds methanol 50ml, puts in the water-bath reflux 1 hour, filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, adds active carbon 1g, and about 10 minutes of jolting filters, and filtrate is concentrated into about 2ml as need testing solution.Other gets the phillyrin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-chloroform-toluene-methanol (5: 3: 5: 3) be developing solvent, presaturation launched after 30 minutes, took out, and dried, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical aubergine speckle.
(7) get 12 of this product, porphyrize adds hydrochloric acid 3ml and chloroform 50ml, puts in the water-bath reflux 1 hour, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Other gets Radix Platycodonis control medicinal material 0.2g, makes control medicinal material solution by the need testing solution method for making.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30~60 ℃)-ethyl acetate-glacial acetic acid (25: 7: 0.5) is developing solvent, launch, take out, dry, spray is with the mixed solution (1: 10) of 8% vanillin alcoholic solution and sulfuric acid solution (7 → 10), and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(8) get 48 of this product, porphyrize adds ethyl acetate 60ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Other gets Fructus Arctii control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, lower floor's solution with chloroform-methanol-water (40: 10: 1) is developing solvent, launch, take out, dry.Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
[inspection] should meet every regulation relevant under the tablet item (an appendix I of Chinese Pharmacopoeia version in 2005 D).
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05mol/L potassium dihydrogen phosphate (43: 57, add dodecyl sodium sulfate 1.7g in every 1000ml solution) is mobile phase, and the detection wavelength is 265nm.Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 6000.
The berberine hydrochloride reference substance is got in the preparation of reference substance solution, adds methanol and makes the solution that every 1ml contains 0.01mg, promptly.
10 of this product are got in the preparation of need testing solution, and porphyrize is got the about 1.5g of fine powder, the accurate title, decide, and puts in the tool plug conical flask, and precision adds methanol-hydrochloric acid (100: 1) 50ml, claim to decide weight, supersound process 30 minutes is taken out, cool, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, get supernatant and filter, promptly with microporous filter membrane (0.45 μ m).
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Cortex Phellodendri with berberine hydrochloride (C
20H
17NO
4HCl) meter must not be less than 0.2mg.
Embodiment 2:
[prescription] Radix Rubiae 16g, Semen Persicae 16g, Herba Schizonepetae (charcoal) 16g, Periostracum Serpentis (wine is processed) 8g, Radix Paeoniae Rubra 16g, Radix Angelicae Sinensis 16g, Rhizoma Imperatae 32g, Fructus Kochiae 16g, Fructus Xanthii (stir-fry) 16g, Radix Rehmanniae 16g, Fructus Forsythiae 16g, Flos Lonicerae 16g, Herba Corydalis Bungeanae 16g, Rhizoma Smilacis Glabrae 16g, Cortex Phellodendri 8g, Spina Gleditsiae 16g, Radix Platycodonis 16g, Herba Leonuri 16g, Semen Armeniacae Amarum (peeling is fried) 16g, Radix Saposhnikoviae 8g, Poria 32g, Radix Paeoniae Alba 16g, Periostracum Cicadae 8g, Fructus Arctii (stir-fry) 16g, Cortex Moutan 16g, Cortex Dictamni 16g, Radix Rehmanniae Preparata 16g, Radix Et Rhizoma Rhei (wine stir-fry) 16g, Caulis Lonicerae 16g, Radix Arnebiae (Radix Lithospermi) 8g, Rhizoma Bolbostematis 16g, Rhizoma Chuanxiong (wine is processed) 8g, Radix Glycyrrhizae 16g, Radix Angelicae Dahuricae 8g, Radix Semiaquilegiae 16g, Cortex cercis chinensis 8g, Caulis Spatholobi 16g, Herba Spirodelae 8g, Flos Carthami 8g
[method for making] above 39 flavors are ground into fine powder, sieve, and mixing is granulated in right amount with simple syrup, and drying adds Pulvis Talci, and mixing is encapsulated, promptly.
The method of quality control of this medicine is with embodiment 1.
Claims (6)
1, the method of quality control of dermatosis toxemia preparation, wherein said preparation is by the Chinese crude drug Radix Rubiae, Semen Persicae, Herba Schizonepetae (charcoal), Periostracum Serpentis (wine is processed), Radix Paeoniae Rubra, Radix Angelicae Sinensis, Rhizoma Imperatae, the Fructus Kochiae, Fructus Xanthii (stir-fry), Radix Rehmanniae, Fructus Forsythiae, Flos Lonicerae, Herba Corydalis Bungeanae, Rhizoma Smilacis Glabrae, Cortex Phellodendri, Spina Gleditsiae, Radix Platycodonis, Herba Leonuri, Semen Armeniacae Amarum (peeling is fried), Radix Saposhnikoviae, Poria, the Radix Paeoniae Alba, Periostracum Cicadae, Fructus Arctii (stir-fry), Cortex Moutan, Cortex Dictamni, Radix Rehmanniae Preparata, Radix Et Rhizoma Rhei (wine stir-fry), Caulis Lonicerae, Radix Arnebiae (Radix Lithospermi), Rhizoma Bolbostematis, Rhizoma Chuanxiong (wine is processed), Radix Glycyrrhizae, the Radix Angelicae Dahuricae, Radix Semiaquilegiae, Cortex cercis chinensis, Caulis Spatholobi, the Herba Spirodelae and Flos Carthami is formed, and it is characterized in that discrimination method in this method is one or more of following method:
1.. get dermatosis toxemia preparation 7.2g, porphyrize adds methanol 15~35ml, puts in the water-bath reflux 10~30 minutes, filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-methanol-isopropyl alcohol-water (5~7: 2~4: 1~3: 1~2: 0.15~0.45) be developing solvent, under the ammonia saturated with vapor, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
2.. get dermatosis toxemia preparation 4.8g, porphyrize adds methanol 5~25ml, supersound process 10~30 minutes filters the filtrate evaporate to dryness, residue adds water 5~15ml makes dissolving, adds hydrochloric acid 0.5~1.5ml, puts and heats 20~40 minutes in the water-bath, take out, cooling immediately adds diethyl ether and extracts 1~3 time, each 5~15ml merges ether solution, evaporate to dryness, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, adds methanol and shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (14~16: 4~6: upper strata liquid 0.5~1.5) is developing solvent with petroleum ether (30~60 ℃ of petroleum ether)-Ethyl formate-formic acid, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show five identical same color fluorescence speckles; Put in the ammonia smoked after, speckle becomes redness;
3.. get dermatosis toxemia preparation 21.6g, porphyrize adds methanol 20~40ml, and supersound process 20~40 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rubiae control medicinal material 1g, adds methanol 10~30ml, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60~90 ℃)-acetone (3~5: 0.5~1.5) be developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
4.. get dermatosis toxemia preparation 14.4g, porphyrize adds methanol 20~40ml, puts in the water-bath reflux 20~40 minutes, puts coldly, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-ethyl acetate (7~9: 3~5: 0.5~1.5) be developing solvent, under the ammonia saturated with vapor, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing in 100 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
5.. get dermatosis toxemia preparation 28.8g, porphyrize, the 25~75ml that adds diethyl ether, low temperature reflux is 0.5~1.5 hour in the water-bath, filters, and filtrate volatilizes, and the residue 1ml that adds diethyl ether makes dissolving, as need testing solution; Other gets Rhizoma Imperatae control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with the chloroform, launch, take out, to dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
6.. get dermatosis toxemia preparation 21.6g, porphyrize adds methanol 25~75ml, puts in the water-bath reflux 0.5~1.5 hour, filter, filtrate evaporate to dryness, residue add methanol 4~6ml makes dissolving, adds active carbon 0.5~1.5g, jolting 5~15 minutes filters, and filtrate is concentrated into about 2ml as need testing solution; Other gets the phillyrin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-chloroform-toluene-methanol (4~6: 2~4: 4~6: 2~4) be developing solvent, presaturation launched after 20~40 minutes, took out, and dried, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical speckle;
7.. get dermatosis toxemia preparation 7.2g, porphyrize adds hydrochloric acid 2~4ml and chloroform 25~75ml, puts in the water-bath reflux 0.5~1.5 hour, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets Radix Platycodonis control medicinal material 0.2g, makes control medicinal material solution by the need testing solution method for making; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30~60 ℃)-ethyl acetate-glacial acetic acid (15~35: 6~8: 0.25~0.75) be developing solvent, launch, take out, dry, (0.5~1.5: 9~11), it is clear to be heated to the speckle colour developing at 105 ℃ with the mixed solution of 8% vanillin alcoholic solution and sulfuric acid solution (7 → 10) in spray; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
8.. get dermatosis toxemia preparation 28.8g, porphyrize adds ethyl acetate 50~70ml, and supersound process 20~40 minutes filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (30~50: 9~11: lower floor's solution 0.5~1.5) is developing solvent, launches, and takes out, and dries with chloroform-methanol-water; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
2, the method for quality control of dermatosis toxemia sheet as claimed in claim 1 is characterized in that discrimination method in this method is one or more of following method:
1.. get 12 of dermatosis toxemia sheets, porphyrize adds methanol 25ml, puts in the water-bath reflux 20 minutes, filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-methanol-isopropyl alcohol-water (6: 3: 2: 1.5: 0.3) is developing solvent, under the ammonia saturated with vapor, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
2.. get 8 of dermatosis toxemia sheets, porphyrize adds methanol 15ml, supersound process 20 minutes filters the filtrate evaporate to dryness, residue adds water 10ml makes dissolving, adds hydrochloric acid 1ml, puts in the water-bath and heats 30 minutes, take out, cooling immediately adds diethyl ether and extracts 2 times, each 10ml merges ether solution, evaporate to dryness, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, adds methanol and shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, upper strata liquid with petroleum ether (30~60 ℃ of petroleum ether)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show five identical same color fluorescence speckles; Put in the ammonia smoked after, speckle becomes redness;
3.. get 36 of dermatosis toxemia sheets, porphyrize adds methanol 30ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rubiae control medicinal material 1g, adds methanol 20ml, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with petroleum ether (60~90 ℃)-acetone (4: 1), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
4.. get 24 of dermatosis toxemia sheets, porphyrize adds methanol 30ml, puts in the water-bath reflux 30 minutes, puts coldly, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-ethyl acetate (8: 4: 1) is developing solvent, under the ammonia saturated with vapor, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing in 100 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
5.. get 48 of dermatosis toxemia sheets, porphyrize, the 50ml that adds diethyl ether, low temperature reflux is 1 hour in the water-bath, filters, and filtrate volatilizes, and the residue 1ml that adds diethyl ether makes dissolving, as need testing solution; Other gets Rhizoma Imperatae control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with the chloroform, launch, take out, to dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
6.. get 36 of dermatosis toxemia sheets, porphyrize adds methanol 50ml, puts in the water-bath reflux 1 hour, filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, adds active carbon 1g, and jolting 10 minutes filters, and filtrate is concentrated into about 2ml as need testing solution; Other gets the phillyrin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-chloroform-toluene-methanol (5: 3: 5: 3) be developing solvent, presaturation launched after 30 minutes, took out, and dried, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical aubergine speckle;
7.. get 12 of dermatosis toxemia sheets, porphyrize adds hydrochloric acid 3ml and chloroform 50ml, puts in the water-bath reflux 1 hour, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets Radix Platycodonis control medicinal material 0.2g, makes control medicinal material solution by the need testing solution method for making; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30~60 ℃)-ethyl acetate-glacial acetic acid (25: 7: 0.5) is developing solvent, launch, take out, dry, spray is with the mixed solution (1: 10) of 8% vanillin alcoholic solution and sulfuric acid solution (7 → 10), and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
8.. get 48 of dermatosis toxemia sheets, porphyrize adds ethyl acetate 60ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with lower floor's solution of chloroform-methanol-water (40: 10: 1), launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
3, the method of quality control of dermatosis toxemia preparation, wherein said preparation is by the Chinese crude drug Radix Rubiae, Semen Persicae, Herba Schizonepetae (charcoal), Periostracum Serpentis (wine is processed), Radix Paeoniae Rubra, Radix Angelicae Sinensis, Rhizoma Imperatae, the Fructus Kochiae, Fructus Xanthii (stir-fry), Radix Rehmanniae, Fructus Forsythiae, Flos Lonicerae, Herba Corydalis Bungeanae, Rhizoma Smilacis Glabrae, Cortex Phellodendri, Spina Gleditsiae, Radix Platycodonis, Herba Leonuri, Semen Armeniacae Amarum (peeling is fried), Radix Saposhnikoviae, Poria, the Radix Paeoniae Alba, Periostracum Cicadae, Fructus Arctii (stir-fry), Cortex Moutan, Cortex Dictamni, Radix Rehmanniae Preparata, Radix Et Rhizoma Rhei (wine stir-fry), Caulis Lonicerae, Radix Arnebiae (Radix Lithospermi), Rhizoma Bolbostematis, Rhizoma Chuanxiong (wine is processed), Radix Glycyrrhizae, the Radix Angelicae Dahuricae, Radix Semiaquilegiae, Cortex cercis chinensis, Caulis Spatholobi, the Herba Spirodelae and Flos Carthami is formed, and it is characterized in that the content assaying method in this method is following method:
According to high effective liquid chromatography for measuring; With the octadecylsilane chemically bonded silica is filler; With acetonitrile-0.05mol/L potassium dihydrogen phosphate (40~45: 55~60, add dodecyl sodium sulfate 1.7g in every 1000ml solution) is mobile phase, and the detection wavelength is 265 ± 2nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 6000; The preparation of reference substance solution: get the berberine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 0.01mg, promptly; The preparation of need testing solution: get dermatosis toxemia preparation, porphyrize is got the about 1.5g of fine powder, the accurate title, decide, and puts in the tool plug conical flask, and precision adds methanol-hydrochloric acid (100: 1) 25~75ml, claim to decide weight, supersound process 20~40 minutes is taken out, cool, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, get supernatant and filter, promptly with microporous filter membrane (0.45 μ m); Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
4, the method for quality control of dermatosis toxemia sheet as claimed in claim 3 is characterized in that the content assaying method in this method is following method:
According to high effective liquid chromatography for measuring; With the octadecylsilane chemically bonded silica is filler; With acetonitrile-0.05mol/L potassium dihydrogen phosphate (43: 57, add dodecyl sodium sulfate 1.7g in every 1000ml solution) is mobile phase, and the detection wavelength is 265nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 6000; The preparation of reference substance solution: get the berberine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 0.01mg, promptly; The preparation of need testing solution: get 10 of dermatosis toxemia sheets, porphyrize is got the about 1.5g of fine powder, the accurate title, decide, and puts in the tool plug conical flask, and precision adds methanol-hydrochloric acid (100: 1) 50ml, claim to decide weight, supersound process 30 minutes is taken out, cool, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, get supernatant and filter, promptly with microporous filter membrane (0.45 μ m); Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
5, the method of quality control of dermatosis toxemia preparation, wherein said preparation is by the Chinese crude drug Radix Rubiae, Semen Persicae, Herba Schizonepetae (charcoal), Periostracum Serpentis (wine is processed), Radix Paeoniae Rubra, Radix Angelicae Sinensis, Rhizoma Imperatae, the Fructus Kochiae, Fructus Xanthii (stir-fry), Radix Rehmanniae, Fructus Forsythiae, Flos Lonicerae, Herba Corydalis Bungeanae, Rhizoma Smilacis Glabrae, Cortex Phellodendri, Spina Gleditsiae, Radix Platycodonis, Herba Leonuri, Semen Armeniacae Amarum (peeling is fried), Radix Saposhnikoviae, Poria, the Radix Paeoniae Alba, Periostracum Cicadae, Fructus Arctii (stir-fry), Cortex Moutan, Cortex Dictamni, Radix Rehmanniae Preparata, Radix Et Rhizoma Rhei (wine stir-fry), Caulis Lonicerae, Radix Arnebiae (Radix Lithospermi), Rhizoma Bolbostematis, Rhizoma Chuanxiong (wine is processed), Radix Glycyrrhizae, the Radix Angelicae Dahuricae, Radix Semiaquilegiae, Cortex cercis chinensis, Caulis Spatholobi, the Herba Spirodelae and Flos Carthami is formed, and it is characterized in that this method comprises following method:
Differentiate: 1.. get dermatosis toxemia preparation 7.2g, porphyrize adds methanol 15~35ml, puts in the water-bath reflux 10~30 minutes, filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-methanol-isopropyl alcohol-water (5~7: 2~4: 1~3: 1~2: 0.15~0.45) be developing solvent, under the ammonia saturated with vapor, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
2.. get dermatosis toxemia preparation 4.8g, porphyrize adds methanol 5~25ml, supersound process 10~30 minutes filters the filtrate evaporate to dryness, residue adds water 5~15ml makes dissolving, adds hydrochloric acid 0.5~1.5ml, puts and heats 20~40 minutes in the water-bath, take out, cooling immediately adds diethyl ether and extracts 1~3 time, each 5~15ml merges ether solution, evaporate to dryness, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, adds methanol and shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (14~16: 4~6: upper strata liquid 0.5~1.5) is developing solvent with petroleum ether (30~60 ℃ of petroleum ether)-Ethyl formate-formic acid, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show five identical same color fluorescence speckles; Put in the ammonia smoked after, speckle becomes redness;
3.. get dermatosis toxemia preparation 21.6g, porphyrize adds methanol 20~40ml, and supersound process 20~40 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rubiae control medicinal material 1g, adds methanol 10~30ml, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60~90 ℃)-acetone (3~5: 0.5~1.5) be developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
4.. get dermatosis toxemia preparation 14.4g, porphyrize adds methanol 20~40ml, puts in the water-bath reflux 20~40 minutes, puts coldly, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-ethyl acetate (7~9: 3~5: 0.5~1.5) be developing solvent, under the ammonia saturated with vapor, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing in 100 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
5.. get dermatosis toxemia preparation 28.8g, porphyrize, the 25~75ml that adds diethyl ether, low temperature reflux is 0.5~1.5 hour in the water-bath, filters, and filtrate volatilizes, and the residue 1ml that adds diethyl ether makes dissolving, as need testing solution; Other gets Rhizoma Imperatae control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with the chloroform, launch, take out, to dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
6.. get dermatosis toxemia preparation 21.6g, porphyrize adds methanol 25~75ml, puts in the water-bath reflux 0.5~1.5 hour, filter, filtrate evaporate to dryness, residue add methanol 4~6ml makes dissolving, adds active carbon 0.5~1.5g, jolting 5~15 minutes filters, and filtrate is concentrated into about 2ml as need testing solution; Other gets the phillyrin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-chloroform-toluene-methanol (4~6: 2~4: 4~6: 2~4) be developing solvent, presaturation launched after 20~40 minutes, took out, and dried, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical speckle;
7.. get dermatosis toxemia preparation 7.2g, porphyrize adds hydrochloric acid 2~4ml and chloroform 25~75ml, puts in the water-bath reflux 0.5~1.5 hour, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets Radix Platycodonis control medicinal material 0.2g, makes control medicinal material solution by the need testing solution method for making; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30~60 ℃)-ethyl acetate-glacial acetic acid (15~35: 6~8: 0.25~0.75) be developing solvent, launch, take out, dry, (0.5~1.5: 9~11), it is clear to be heated to the speckle colour developing at 105 ℃ with the mixed solution of 8% vanillin alcoholic solution and sulfuric acid solution (7 → 10) in spray; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
8.. get dermatosis toxemia preparation 28.8g, porphyrize adds ethyl acetate 50~70ml, and supersound process 20~40 minutes filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (30~50: 9~11: lower floor's solution 0.5~1.5) is developing solvent, launches, and takes out, and dries with chloroform-methanol-water; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Assay: according to high effective liquid chromatography for measuring; With the octadecylsilane chemically bonded silica is filler; With acetonitrile-0.05mol/L potassium dihydrogen phosphate (40~45: 55~60, add dodecyl sodium sulfate 1.7g in every 1000ml solution) is mobile phase, and the detection wavelength is 265 ± 2nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 6000; The preparation of reference substance solution: get the berberine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 0.01mg, promptly; The preparation of need testing solution: get dermatosis toxemia preparation, porphyrize is got the about 1.5g of fine powder, the accurate title, decide, and puts in the tool plug conical flask, and precision adds methanol-hydrochloric acid (100: 1) 25: 75ml, claim to decide weight, supersound process 20: 40 minutes is taken out, cool, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, get supernatant and filter, promptly with microporous filter membrane (0.45 μ m); Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
6, the method for quality control of dermatosis toxemia sheet as claimed in claim 5 is characterized in that comprising in this method following method:
Differentiate: 1.. get 12 of dermatosis toxemia sheets, porphyrize adds methanol 25ml, puts in the water-bath reflux 20 minutes, filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-methanol-isopropyl alcohol-water (6: 3: 2: 1.5: 0.3) is developing solvent, under the ammonia saturated with vapor, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
2.. get 8 of dermatosis toxemia sheets, porphyrize adds methanol 15ml, supersound process 20 minutes filters the filtrate evaporate to dryness, residue adds water 10ml makes dissolving, adds hydrochloric acid 1ml, puts in the water-bath and heats 30 minutes, take out, cooling immediately adds diethyl ether and extracts 2 times, each 10ml merges ether solution, evaporate to dryness, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, adds methanol and shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, upper strata liquid with petroleum ether (30~60 ℃ of petroleum ether)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show five identical same color fluorescence speckles; Put in the ammonia smoked after, speckle becomes redness;
3.. get 36 of dermatosis toxemia sheets, porphyrize adds methanol 30ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rubiae control medicinal material 1g, adds methanol 20ml, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with petroleum ether (60~90 ℃)-acetone (4: 1), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
4.. get 24 of dermatosis toxemia sheets, porphyrize adds methanol 30ml, puts in the water-bath reflux 30 minutes, puts coldly, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-ethyl acetate (8: 4: 1) is developing solvent, under the ammonia saturated with vapor, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing in 100 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
5.. get 48 of dermatosis toxemia sheets, porphyrize, the 50ml that adds diethyl ether, low temperature reflux is 1 hour in the water-bath, filters, and filtrate volatilizes, and the residue 1ml that adds diethyl ether makes dissolving, as need testing solution; Other gets Rhizoma Imperatae control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with the chloroform, launch, take out, to dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
6.. get 36 of dermatosis toxemia sheets, porphyrize adds methanol 50ml, puts in the water-bath reflux 1 hour, filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, adds active carbon 1g, and about 10 minutes of jolting filters, and filtrate is concentrated into about 2ml as need testing solution; Other gets the phillyrin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-chloroform-toluene-methanol (5: 3: 5: 3) be developing solvent, presaturation launched after 30 minutes, took out, and dried, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical aubergine speckle;
7.. get 12 of dermatosis toxemia sheets, porphyrize adds hydrochloric acid 3ml and chloroform 50ml, puts in the water-bath reflux 1 hour, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets Radix Platycodonis control medicinal material 0.2g, makes control medicinal material solution by the need testing solution method for making; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30~60 ℃)-ethyl acetate-glacial acetic acid (25: 7: 0.5) is developing solvent, launch, take out, dry, spray is with the mixed solution (1: 10) of 8% vanillin alcoholic solution and sulfuric acid solution (7 → 10), and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
8.. get 48 of dermatosis toxemia sheets, porphyrize adds ethyl acetate 60ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Other gets Fructus Arctii control medicinal material 1g, makes control medicinal material solution by the need testing solution method for making; According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with lower floor's solution of chloroform-methanol-water (40: 10: 1), launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Assay: according to high effective liquid chromatography for measuring; With the octadecylsilane chemically bonded silica is filler; With acetonitrile-0.05mol/L potassium dihydrogen phosphate (43: 57, add dodecyl sodium sulfate 1.7g in every 1000ml solution) is mobile phase, and the detection wavelength is 265nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 6000; The preparation of reference substance solution: get the berberine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 0.01mg, promptly; The preparation of need testing solution: get 10 of dermatosis toxemia sheets, porphyrize is got the about 1.5g of fine powder, the accurate title, decide, and puts in the tool plug conical flask, and precision adds methanol-hydrochloric acid (100: 1) 50ml, claim to decide weight, supersound process 30 minutes is taken out, cool, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, get supernatant and filter, promptly with microporous filter membrane (0.45 μ m); Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
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CN101564514B (en) * | 2009-06-12 | 2013-06-05 | 杨文龙 | Method for analyzing children Fengreqing particle |
CN104678045A (en) * | 2014-12-18 | 2015-06-03 | 南方医科大学 | Method for detecting radix sophorae flavescentis-eucalyptus robusta rash-eliminating gel medicine |
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CN101564514B (en) * | 2009-06-12 | 2013-06-05 | 杨文龙 | Method for analyzing children Fengreqing particle |
CN104678045A (en) * | 2014-12-18 | 2015-06-03 | 南方医科大学 | Method for detecting radix sophorae flavescentis-eucalyptus robusta rash-eliminating gel medicine |
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CN105004800A (en) * | 2015-06-10 | 2015-10-28 | 贵州省科晖制药厂 | Quality detection method of cool and refreshing sunstroke prevention agent |
CN105467059A (en) * | 2015-12-30 | 2016-04-06 | 云南理想药业有限公司 | Quality detecting method for traditional Chinese medicine composition for treating hematuresis |
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CN113834883A (en) * | 2021-06-22 | 2021-12-24 | 海南葫芦娃药业集团股份有限公司 | Method for determining content of fructus forsythiae in infantile lung heat cough and asthma granules |
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