CN101574439A - Method for controlling quality of Runzao Zhiyang tablet - Google Patents
Method for controlling quality of Runzao Zhiyang tablet Download PDFInfo
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- CN101574439A CN101574439A CNA2009101140709A CN200910114070A CN101574439A CN 101574439 A CN101574439 A CN 101574439A CN A2009101140709 A CNA2009101140709 A CN A2009101140709A CN 200910114070 A CN200910114070 A CN 200910114070A CN 101574439 A CN101574439 A CN 101574439A
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Abstract
The invention discloses a method for controlling the quality of a traditional Chinese medicine preparation-Runzao Zhiyang tablet. The quality control method includes the steps of adopting the thin-layer chromatography to identify kuh-seng and mulberry leaves and adopting the high performance liquid chromatography to determine the content of matrine in the preparation. The quality control method is reliable and feasible, and can guarantee the product quality and the clinical efficacy.
Description
Invention field
The present invention relates to a kind of method of quality control of Chinese medicine preparation, be specifically related to the method for quality control of Runzao Zhiyang tablet.
Background technology
The Runzao Zhiyang tablet recipe derives from " Chinese patent medicine provincial standard rising national standard " (ophthalmology, otorhinolaryngology, skin fascicle) 397 pages of kind Runzao Zhiyang capsules that record, standard code is WS-10029-(ZD-0029)-2002, has nourishing the blood and yin, dispelling wind for relieving itching, effect of relaxing bowel, be used for the skin pruritus due to the blood-deficiency and wind-dry, acne, constipation.The Runzao Zhiyang tablet recipe is: Radix Polygoni Multiflori 291g, Radix Polygoni Multiflori Preparata 265g, Radix Rehmanniae 429g, Folium Mori 291g, Radix Sophorae Flavescentis 291g, Herba Girardinlae Diversifoliae 150g; Method for making is: above Six-element, get Radix Polygoni Multiflori Preparata, and be ground into fine powder, standby; The five tastes such as all the other Radix Sophorae Flavescentiss decoct with water three times, and each 1 hour, collecting decoction, filter, filtrate is concentrated into the thick paste that relative density is 1.38～1.42 (25 ℃), adds above-mentioned Radix Polygoni Multiflori Preparata fine powder, mixing, 75～80 ℃ of dryings are ground into granule, add adjuvants such as an amount of carboxymethylstach sodium, mixing, be pressed into 1000, the bag film-coat, promptly.
The easy moisture absorption of this kind capsule is difficult for preserving, and can not satisfy the clinical application demand, therefore we are tablet with its dosage changing form, extraction process is consistent with tablet, but preparation process is different with adjuvant, needs to formulate truly feasible method of quality control to guarantee product quality and clinical efficacy.And exist in the former capsule standard in matrine thin layer round of visits length and the developing solvent and use the bigger benzene of toxicity, the Folium Mori thin layer chromatography disturbs bigger, assay item emodin content is lower, is difficult to effectively control problems such as this product quality, also needs quality control method is further studied raising.
Summary of the invention
The object of the invention is to provide a kind of method of quality control of Runzao Zhiyang tablet, and then guarantees product quality and clinical efficacy.
The method of quality control of Runzao Zhiyang tablet:
Method of quality control of the present invention has solved the deficiency that exists in the former Runzao Zhiyang capsule standard, the matrine round of visits significantly shortens, developing solvent adopts toluene to substitute the bigger benzene of toxicity, the Folium Mori thin layer chromatography separates good, clear spot, and newly formulated the content of matrine assay method, the quality of the pharmaceutical preparations is controlled better.
The Runzao Zhiyang tablet method of quality control comprises following all or part of content: content of matrine in the Folium Mori in the Radix Sophorae Flavescentis in the thin layer chromatography discriminating preparation, the thin layer chromatography discriminating preparation, the high performance liquid chromatography chromatography determination preparation.
During the Runzao Zhiyang tablet method of quality control may further comprise the steps one or more:
(1) thin layer chromatography is differentiated Radix Sophorae Flavescentis: it is an amount of to get this product, removes film-coat, and porphyrize adds chloroform 25ml, strong ammonia solution 0.5ml, and supersound process 15-60 minute, filter, filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets Radix Sophorae Flavescentis control medicinal material 1g, shines medical material solution in pairs with legal system.Get the matrine reference substance again, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (the corresponding appendix of Chinese Pharmacopoeia), draw above-mentioned need testing solution and each 5ul of control medicinal material solution, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-acetone-ethyl acetate-strong ammonia solution (2: 3: 4: 0.2) be developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) thin layer chromatography is differentiated Folium Mori: it is an amount of to get this product, removes film-coat, porphyrize, add methanol 10～100ml, supersound process 10～60 minutes filters, the filtrate evaporate to dryness, residue adds water 10～100ml makes dissolving, uses ethyl acetate extraction 1～3 time, each 10～100ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Mori control medicinal material 2g, adds petroleum ether (60～90 ℃) heating and refluxing extraction, discards petroleum ether liquid, and medicinal residues volatilize, add the ethanol supersound process, filter, filtrate evaporate to dryness, residue add the hot water stirring makes dissolving, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (the corresponding appendix of Chinese Pharmacopoeia), draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ethyl acetate-formic acid (5: 2: 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.
(3) content of matrine in high effective liquid chromatography for measuring this product
Measure according to high performance liquid chromatography (the corresponding appendix of Chinese Pharmacopoeia).
Chromatographic condition and system suitability test are filler with amino bonded silica gel; With acetonitrile-methanol-3% phosphoric acid solution is mobile phase; UV-detector.
It is an amount of that the preparation precision of reference substance solution takes by weighing the matrine reference substance, adds appropriate solvent and make the solution that every 1ml contains 50 μ g, promptly.
The preparation of need testing solution is got this product and is removed coating, porphyrize.Get in right amount, the accurate title, decide, and puts in the measuring bottle, adds strong ammonia solution and soak into, add the methanol supersound process again, put coldly, be diluted to scale, shake up with methanol, filter, precision is measured the subsequent filtrate of certain volume, crosses the neutral alumina post, successively with chloroform, chloroform-methanol (5～10: 1～5) an amount of eluting, collect eluent, reclaim solvent to doing, residue adds appropriate solvent makes dissolving, be transferred in the measuring bottle, and be diluted to scale, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
Above-mentioned described mobile phase can be that (85～95: 2～8: 2～8), the best is acetonitrile-methanol-3% phosphoric acid solution (90: 5: 5) to acetonitrile-methanol-3% phosphoric acid solution
The used mensuration wavelength of above-mentioned described UV-detector can be 200nm～220nm, and optimal wavelength is the best 210nm of being of 208nm～212nm.
Above-mentioned described appropriate solvent can be methanol or acetonitrile or both any ratios, and (20～95: be good 80～5), the best is acetonitrile-methanol (80: 20) with acetonitrile-methanol.
Above-mentioned method of quality control favorable reproducibility also can be used for the quality control of other Runzao Zhiyang preparations, the sampling amount amount of regularlying sample of various preparations and deciding.
Above-mentioned Runzao Zhiyang preparation is meant in Runzao Zhiyang capsule prescription ratio, with the preparation that prior preparation method is made, comprise clinical or pharmaceutically acceptable common formulations such as tablet, capsule, granule, drop pill, oral liquid, syrup, soft extract, buccal tablet, pill, powder, suppository, patch, injection.
The specific embodiment
Preparation method of the present invention and method of quality control are the preferred plan that obtains through a large amount of screenings, and following experimental example is used to further specify technical scheme of the present invention and technique effect.
Experimental example 1: for the thin layer chromatography feature of Radix Sophorae Flavescentis is differentiated.
During the thin layer chromatography of capsule quality standard Radix Sophorae Flavescentis was differentiated, the test sample preparation time was long, is unfavorable for experiment progress, and in addition, its development system agents useful for same---benzene toxicity is big, is unfavorable for environmental protection.And the extracting method simple possible that invention is recorded, development system substitutes with the less toluene of toxicity, also can make the fine separation of speckle.
Following extracting method is tested: get 4 of this product, remove film-coat, porphyrize, the 25ml that adds methylene chloride, strong ammonia solution 0.5ml, supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.Speckle is not obvious in the test sample chromatograph as a result, so do not adopt.
Test by embodiment 1 Radix Sophorae Flavescentis thin layer discrimination method, as a result in the test sample chromatograph, with Radix Sophorae Flavescentis control medicinal material and the corresponding position of matrine reference substance chromatograph on, show identical punctation.The thin layer chromatography good separating effect, the speckle rounding, Rf value is moderate, and repeatability and specificity are good, and negative control is noiseless.
Experimental example 2: for the thin layer chromatography feature of Folium Mori is differentiated.
The thin layer chromatography discrimination method of capsule quality standard Folium Mori, it is big disturbed by impurity, be difficult for observing, and the present invention records method thin layer chromatography good separating effect, the speckle rounding, repeatability and specificity are good, and negative control is noiseless.
Following method for extraction and purification has been carried out contrast test: 1. get 4 of this product, remove film-coat, porphyrize adds ethanol 20ml, and supersound process 1 hour filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.2. get 4 of this product, remove film-coat, porphyrize adds ethanol 20ml, reflux 1 hour, put coldly, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, with ethyl acetate extraction 2 times, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.3. get 4 of this product, remove film-coat, porphyrize adds 70% ethanol 30ml supersound process 30 minutes, filters, and filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution.As a result method 1. (capsule quality standard method), 3. in the test sample chromatograph, the feature speckle is clear inadequately, impurity disturbs big; 2. in the test sample chromatograph, the feature speckle is not obvious, so do not adopt for method.
Test by embodiment 1 Folium Mori thin layer discrimination method, as a result in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show 2 identical blue-fluorescence speckles.
Experimental example 3: determination of matrine research
Because emodin content is lower in the preparation, content is lower than ten thousand/, the quality controllability deficiency is so the present invention has newly set up content of matrine assay method in the preparation.Result of the test shows, good separation under selected condition, and methodological studies such as linearity, stability, repeatability, the response rate all meet the requirement of assay, can be used for controlling the index of this quality of the pharmaceutical preparations.Result of the test is as follows:
1. the preparation of solution
The preparation of reference substance solution: precision takes by weighing matrine reference substance 10.22mg, puts in the 10ml measuring bottle, adds dissolve with methanol and is diluted to scale, shake up, precision is measured 0.5ml and is put in the 10ml measuring bottle, adds acetonitrile-methanol (80: 20) and is diluted to scale, shake up, promptly get (every 1ml contains matrine 51.1 μ g).
The need testing solution preparation: get 10 of this product, remove coating, the accurate title, decided porphyrize.Get 0.4g, the accurate title, decide, and puts in the 25ml measuring bottle, add strong ammonia solution 1ml, soak into, add methanol 20ml again, supersound process (power 260W frequency 50HKz) 30 minutes is put coldly, is diluted to scale with methanol, shake up, filter, precision is measured subsequent filtrate 10ml, cross neutral alumina post (100～200 orders, 5g, internal diameter 1cm), successively with chloroform, each 40ml eluting of chloroform-methanol (7: 3), collect eluent, reclaim solvent to doing, residue adds acetonitrile-methanol (80: 20) makes dissolving, and be transferred in the 10ml measuring bottle, add acetonitrile-methanol (80: 20) and be diluted to scale, shake up, filter, get subsequent filtrate, promptly.
The present invention investigated the supersound extraction time (15 minutes, 30 minutes, 60 minutes), and the result all can extract matrine preferably, and best extraction time is 30 minutes.
The present invention investigates ultrasonic strong ammonia solution addition (0.5ml, 1ml, 2ml), and it is little that the result records result difference, and best addition is 1ml.The strong ammonia solution addition is soaked into for good just with test sample.
Methanol-acetonitrile mixed solvent with methanol, acetonitrile and different proportion is investigated the residue dissolubility, the equal solubilized of result, and (20-95: being good 80-5), is the best with acetonitrile-methanol (80: 20) with acetonitrile-methanol.
The preparation of negative sample solution: negative sample is to make the negative preparation that lacks Radix Sophorae Flavescentis by method for making, gets this negative preparation does not contain Radix Sophorae Flavescentis by the preparation of above-mentioned " need testing solution preparation " method negative sample solution again.
2. chromatographic condition and system suitability test
Chromatographic column: amino bonded silica gel chromatographic column (NH
2Post, 250mm * 4.6mm); Mobile phase: acetonitrile-methanol-3% phosphoric acid solution (90: 5: 5); Flow velocity: 1.0ml/min, column temperature: room temperature; Detector: UV-detector, detect wavelength 210nm.
Draw matrine reference substance solution, need testing solution respectively and do not contain each 10 μ l of negative sample solution of Radix Sophorae Flavescentis, inject chromatograph of liquid, matrine and other component reach baseline separation under this condition, separating degree R＞1.5, number of theoretical plate is pressed the matrine peak and is calculated greater than 4000, and the matrine retention time is about 11 minutes.Negative sample solution chromatograph does not have absworption peak in the relevant position, and is visible negative noiseless.
3. measure the selection of wavelength
Getting concentration is the matrine reference substance solution of 10.22 μ g/ml, and in the interscan of 190～400nm scope, matrine has bigger absorption at 200-220nm as a result, all can be used as the mensuration wavelength with ultraviolet spectrophotometer.The optimum detection wavelength is 210nm.
4. reference substance purity test
Get the matrine reference substance solution of 1.03mg/ml, sample introduction 20 μ l calculate with the peak area normalization method, and content is 99.70%, calculates by 100% during calculating.
5. methodology checking
Linear relationship is investigated: with peak area integration A matrine sample size C (μ g) is carried out regression analysis, get regression equation: A=1618420C-19649, r=0.9999.Show that the matrine sample size is good in 0.1022～2.044 μ g scope internal linear relation, and the straight-line pass initial point, available single-point external standard method is measured and is calculated.The instrument precision test: matrine peak area meansigma methods is 842912 as a result, and RSD is 0.37%, shows that precision is better.The test liquid stability test: peak area in a few days meansigma methods is 970015, and RSD is 1.34%; Peak area 3 daily means are 979070, and RSD is 1.36%, show that need testing solution is stable in 72 hours.Replica test: the content meansigma methods is the 1.922mg/ sheet, and RSD is 1.94%, shows method repeatability better.The average recovery test: average recovery rate is 99.36%, and RSD is 1.92%, shows that the method response rate is better.
Specific embodiment is as follows:
Embodiment 1 Runzao Zhiyang tablet method of quality control
(1) get 4 of this product, remove film-coat, porphyrize adds chloroform 25ml, strong ammonia solution 0.5ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets Radix Sophorae Flavescentis control medicinal material 1g, shines medical material solution in pairs with legal system.Get the matrine reference substance again, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw above-mentioned need testing solution and each 5ul of control medicinal material solution, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-acetone-ethyl acetate-strong ammonia solution (2: 3: 4: 0.2) be developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get 4 of this product, remove film-coat, porphyrize adds methanol 20ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, uses ethyl acetate extraction 2 times, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Mori control medicinal material 2g, adds petroleum ether (60～90 ℃) 30ml, reflux 30 minutes, discard petroleum ether liquid, medicinal residues volatilize, and add ethanol 30ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add hot water 10ml stirring makes dissolving, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ethyl acetate-formic acid (5: 2: 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.
(3) content of matrine is measured: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test are filler with amino bonded silica gel; With acetonitrile-methanol-3% phosphoric acid solution (90: 5: 5) is mobile phase; The detection wavelength is 210nm.
It is an amount of that the preparation precision of reference substance solution takes by weighing the matrine reference substance, adds acetonitrile-methanol (80: 20) and make the solution that every 1ml contains 50 μ g, promptly.
10 of this product are got in the preparation of need testing solution, remove film-coat, and accurate the title decided porphyrize.Get 0.4g, the accurate title, decide, and puts in the 25ml measuring bottle, add strong ammonia solution 1ml, soak into, add methanol 20ml again, supersound process (power 260W frequency 50HKz) 30 minutes is put coldly, is diluted to scale with methanol, shake up, filter, precision is measured subsequent filtrate 10ml, cross neutral alumina post (100～200 orders, 5g, internal diameter 1cm), successively with chloroform, each 40ml eluting of chloroform-methanol (7: 3), collect eluent, reclaim solvent to doing, residue adds acetonitrile-methanol (80: 20) makes dissolving, and be transferred in the 10ml measuring bottle, add acetonitrile-methanol (80: 20) and be diluted to scale, shake up, filter, get subsequent filtrate, promptly.
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 Radix Sophorae Flavescentis with matrine (C
15H
24O
2) meter, must not be less than 1.2mg.
Embodiment 2 Runzao Zhiyang tablet method of quality control
(1) get 4 of this product, remove film-coat, porphyrize adds chloroform 25ml, strong ammonia solution 0.5ml, and supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets Radix Sophorae Flavescentis control medicinal material 1g, shines medical material solution in pairs with legal system.Get the matrine reference substance again, add ethanol and make 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 above-mentioned need testing solution and each 5ul of control medicinal material solution, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-acetone-ethyl acetate-strong ammonia solution (2: 3: 4: 0.2) be developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get 8 of this product, remove film-coat, porphyrize adds methanol 100ml, supersound process 60 minutes, filter, filtrate evaporate to dryness, residue add water 100ml makes dissolving, extracts with ethyl acetate 100ml, get acetic acid ethyl fluid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Mori control medicinal material 2g, adds petroleum ether (60～90 ℃) 30ml, reflux 30 minutes, discard petroleum ether liquid, medicinal residues volatilize, and add ethanol 30ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add hot water 10ml stirring makes dissolving, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ethyl acetate-formic acid (5: 2: 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.
(3) content of matrine is measured: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test are filler with amino bonded silica gel; With acetonitrile-methanol-3% phosphoric acid solution (85: 8: 7) is mobile phase; The detection wavelength is 200nm.
It is an amount of that the preparation precision of reference substance solution takes by weighing the matrine reference substance, adds acetonitrile-methanol (20: 80) and make the solution that every 1ml contains 50 μ g, promptly.
The preparation of need testing solution is got this product and is removed film-coat, and accurate the title decided porphyrize.Get 0.2g, the accurate title, decide, and puts in the 25ml measuring bottle, add strong ammonia solution 0.5ml, soak into, add methanol 20ml again, supersound process 15 minutes is put coldly, is diluted to scale with methanol, shake up, filter, precision is measured subsequent filtrate 10ml, cross neutral alumina post (100～200 orders, 3g, internal diameter 1cm), successively with chloroform, each 20ml eluting of chloroform-methanol (10: 1), collect eluent, reclaim solvent to doing, residue adds acetonitrile-methanol (20: 80) makes dissolving, and be transferred in the 10ml measuring bottle, add acetonitrile-methanol (20: 80) and be diluted to scale, shake up, filter, get subsequent filtrate, promptly.
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.
Embodiment 3 Runzao Zhiyang tablet method of quality control
(1) get 4 of this product, remove film-coat, porphyrize adds chloroform 25ml, strong ammonia solution 0.5ml, and supersound process 60 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets Radix Sophorae Flavescentis control medicinal material 1g, shines medical material solution in pairs with legal system.Get the matrine reference substance again, add ethanol and make 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 above-mentioned need testing solution and each 5ul of control medicinal material solution, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-acetone-ethyl acetate-strong ammonia solution (2: 3: 4: 0.2) be developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get 2 of this product, remove film-coat, porphyrize adds methanol 10ml, supersound process 10 minutes, filter, filtrate evaporate to dryness, residue add water 10ml makes dissolving, uses ethyl acetate extraction 3 times, each 10ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Mori control medicinal material 2g, adds petroleum ether (60～90 ℃) 30ml, reflux 30 minutes, discard petroleum ether liquid, medicinal residues volatilize, and add ethanol 30ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add hot water 10ml stirring makes dissolving, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ethyl acetate-formic acid (5: 2: 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.
(3) content of matrine is measured: measure 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 amino bonded silica gel; With acetonitrile-methanol-3% phosphoric acid solution (90: 5: 5) is mobile phase; The detection wavelength is 220nm.
It is an amount of that the preparation precision of reference substance solution takes by weighing the matrine reference substance, adds acetonitrile-methanol (95: 5) and make the solution that every 1ml contains 50 μ g, promptly.
This product is got in the preparation of need testing solution, removes film-coat, and accurate the title decided porphyrize.Get 0.8g, the accurate title, decide, and puts in the 50ml measuring bottle, add strong ammonia solution 2ml, soak into, add methanol 45ml again, supersound process (power 260W frequency 50HKz) 30 minutes is put coldly, is diluted to scale with methanol, shake up, filter, precision is measured subsequent filtrate 20ml, cross neutral alumina post (100～200 orders, 8g, internal diameter 1cm), successively with chloroform, each 40ml eluting of chloroform-methanol (1: 1), collect eluent, reclaim solvent to doing, residue adds acetonitrile-methanol (95: 5) makes dissolving, and be transferred in the 10ml measuring bottle, add acetonitrile-methanol (95: 5) and be diluted to scale, shake up, filter, get subsequent filtrate, promptly.
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.
Embodiment 4 Runzao Zhiyang capsule quality control methods
(1) get the content of 3 of this product, porphyrize adds chloroform 25ml, strong ammonia solution 0.5ml, and supersound process 60 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets Radix Sophorae Flavescentis control medicinal material 1g, shines medical material solution in pairs with legal system.Get the matrine reference substance again, add ethanol and make 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 above-mentioned need testing solution and each 5ul of control medicinal material solution, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-acetone-ethyl acetate-strong ammonia solution (2: 3: 4: 0.2) be developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get the content of 3 of this product, porphyrize adds methanol 50ml, and supersound process 40 minutes filters, filtrate evaporate to dryness, residue add water 30ml makes dissolving, uses ethyl acetate extraction 2 times, each 30ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Mori control medicinal material 2g, adds petroleum ether (60～90 ℃) 50ml, reflux 60 minutes, discard petroleum ether liquid, medicinal residues volatilize, and add ethanol 50ml, supersound process 60 minutes, filter, filtrate evaporate to dryness, residue add hot water 20ml stirring makes dissolving, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ethyl acetate-formic acid (5: 2: 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.
(3) content of matrine is measured: measure 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 amino bonded silica gel; With acetonitrile-methanol-3% phosphoric acid solution (85: 8: 7) is mobile phase; The detection wavelength is 215nm.
It is an amount of that the preparation precision of reference substance solution takes by weighing the matrine reference substance, adds acetonitrile-methanol (20: 80) and make the solution that every 1ml contains 50 μ g, promptly.
This product content, porphyrize are got in the preparation of need testing solution.Get 0.3g, the accurate title, decide, and puts in the 50ml measuring bottle, add strong ammonia solution 0.5ml, soak into, add methanol 40ml again, supersound process (power 150W frequency 30HKz) 60 minutes is put coldly, is diluted to scale with methanol, shake up, filter, precision is measured subsequent filtrate 10ml, cross neutral alumina post (100～200 orders, 5g, internal diameter 1cm), successively with chloroform, each 80ml eluting of chloroform-methanol (4: 1), collect eluent, reclaim solvent to doing, residue adds acetonitrile-methanol (20: 80) makes dissolving, and be transferred in the 10ml measuring bottle, add acetonitrile-methanol (20: 80) and be diluted to scale, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Embodiment 5 Runzao Zhiyang granular mass control methods
(1) get this product 3g, porphyrize adds chloroform 25ml, strong ammonia solution 2ml, and supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets Radix Sophorae Flavescentis control medicinal material 1g, shines medical material solution in pairs with legal system.Get the matrine reference substance again, add ethanol and make 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 above-mentioned need testing solution and each 5ul of control medicinal material solution, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-acetone-ethyl acetate-strong ammonia solution (2: 3: 4: 0.2) be developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get this product 3g, porphyrize adds methanol 30ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add water 10ml makes dissolving, uses ethyl acetate extraction 2 times, each 10ml, and combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Mori control medicinal material 2g, adds petroleum ether (60～90 ℃) 20ml, reflux 20 minutes, discard petroleum ether liquid, medicinal residues volatilize, and add ethanol 20ml, supersound process 20 minutes, filter, filtrate evaporate to dryness, residue add hot water 5ml stirring makes dissolving, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ethyl acetate-formic acid (5: 2: 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.
(3) content of matrine is measured: measure 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 amino bonded silica gel; With acetonitrile-methanol-3% phosphoric acid solution (95: 2: 3) is mobile phase; The detection wavelength is 205nm.
It is an amount of that the preparation precision of reference substance solution takes by weighing the matrine reference substance, adds acetonitrile and make the solution that every 1ml contains 50 μ g, promptly.
This product porphyrize is got in the preparation of need testing solution.Get 1g, the accurate title, decide, and puts in the 50ml measuring bottle, add strong ammonia solution 1ml, soak into, add methanol 45ml again, supersound process (power 200W frequency 50HKz) 20 minutes is put coldly, is diluted to scale with methanol, shake up, filter, precision is measured subsequent filtrate 15ml, cross neutral alumina post (100～200 orders, 3g, internal diameter 1cm), successively with chloroform, each 30ml eluting of chloroform-methanol (6: 5), collect eluent, reclaim solvent to doing, residue adds acetonitrile makes dissolving, and be transferred in the 10ml measuring bottle, add dilution in acetonitrile to scale, shake up, filter, get subsequent filtrate, promptly.
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.
Embodiment 6 Runzao Zhiyang drop pill method of quality control
(1) get this product 8 balls, crowded broken, add chloroform 25ml, strong ammonia solution 1ml, supersound process 40 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets Radix Sophorae Flavescentis control medicinal material 1g, shines medical material solution in pairs with legal system.Get the matrine reference substance again, add ethanol and make 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 above-mentioned need testing solution and each 5ul of control medicinal material solution, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-acetone-ethyl acetate-strong ammonia solution (2: 3: 4: 0.2) be developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get this product 8 balls, crowded broken, add methanol 20ml, supersound process 10 minutes filters, filtrate evaporate to dryness, residue add water 40ml makes dissolving, uses ethyl acetate extraction 2 times, each 40ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Mori control medicinal material 2g, adds petroleum ether (60～90 ℃) 60ml, reflux 50 minutes, discard petroleum ether liquid, medicinal residues volatilize, and add ethanol 40ml, supersound process 40 minutes, filter, filtrate evaporate to dryness, residue add hot water 5ml stirring makes dissolving, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ethyl acetate-formic acid (5: 2: 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.
(3) content of matrine is measured: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test are filler with amino bonded silica gel; With acetonitrile-methanol-3% phosphoric acid solution (92: 3: 5) is mobile phase; The detection wavelength is 212nm.
It is an amount of that the preparation precision of reference substance solution takes by weighing the matrine reference substance, adds methanol and make the solution that every 1ml contains 50 μ g, promptly.
This product 8 balls are got in the preparation of need testing solution, and are crowded broken, put in the 25ml measuring bottle, add strong ammonia solution 1ml, add methanol 20ml again, supersound process (power 250W frequency 40HKz) 40 minutes, put coldly, be diluted to scale, shake up with methanol, filter, precision is measured subsequent filtrate 20ml, crosses neutral alumina post (100～200 orders, 2g, internal diameter 1cm), successively with chloroform, each 20ml eluting of chloroform-methanol (3: 1) is collected eluent, reclaim solvent to doing, residue adds methanol makes dissolving, and is transferred in the 10ml measuring bottle, adds methanol and is diluted to scale, shake up, filter, get subsequent filtrate, promptly.
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.
Embodiment 7 Runzao Zhiyang oral liquid method of quality control
(1) get this product 20ml, add strong ammonia solution 0.5ml, use chloroform extraction 2 times, each 25ml, extracting solution evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets Radix Sophorae Flavescentis control medicinal material 1g, adds chloroform 25ml, strong ammonia solution 0.5ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, makes control medicinal material solution.Get the matrine reference substance again, add ethanol and make 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 above-mentioned need testing solution and each 5ul of control medicinal material solution, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-acetone-ethyl acetate-strong ammonia solution (2: 3: 4: 0.2) be developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get this product 20ml, use ethyl acetate extraction 2 times, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Mori control medicinal material 2g, adds petroleum ether (60～90 ℃) 30ml, reflux 30 minutes, discard petroleum ether liquid, medicinal residues volatilize, and add ethanol 30ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add hot water 10ml stirring makes dissolving, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ethyl acetate-formic acid (5: 2: 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.
(3) content of matrine is measured: measure 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 amino bonded silica gel; With acetonitrile-methanol-3% phosphoric acid solution (88: 4: 8) is mobile phase; The detection wavelength is 208nm.
It is an amount of that the preparation precision of reference substance solution takes by weighing the matrine reference substance, adds acetonitrile-methanol (95: 5) and make the solution that every 1ml contains 50 μ g, promptly.
The preparation precision of need testing solution is measured this product 10ml, puts in the 50ml measuring bottle, adds strong ammonia solution 1ml, add methanol 20ml again, supersound process (power 200W frequency 50HKz) 10 minutes is put cold, be diluted to scale with methanol, shake up, filter, precision is measured subsequent filtrate 10ml, cross neutral alumina post (100～200 orders, 5g, internal diameter 1cm), successively with chloroform, each 20ml eluting of chloroform-methanol (8: 3), collect eluent, reclaim solvent to doing, residue adds acetonitrile-methanol (95: 5) makes dissolving, and be transferred in the 10ml measuring bottle, add acetonitrile-methanol (95: 5) and be diluted to scale, shake up, filter, get subsequent filtrate, promptly.
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.
Claims (7)
1. the method for quality control of a Runzao Zhiyang tablet is characterized in that, this method comprises following all or part of content: content of matrine in the Folium Mori in the Radix Sophorae Flavescentis in the qualitative identification preparation, the qualitative identification preparation, the mensuration preparation.
2. method of quality control as claimed in claim 1 is characterized in that, one or more in may further comprise the steps:
(1) thin layer chromatography is differentiated Radix Sophorae Flavescentis: it is an amount of to get this product, removes film-coat, and porphyrize adds chloroform 25ml, strong ammonia solution 0.5ml, and supersound process 15-60 minute, filter, filtrate evaporate to dryness, residue add dehydrated alcohol 2ml makes dissolving, as need testing solution.Other gets Radix Sophorae Flavescentis control medicinal material 1g, shines medical material solution in pairs with legal system.Get the matrine reference substance again, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (the corresponding appendix of Chinese Pharmacopoeia), draw above-mentioned need testing solution and each 5ul of control medicinal material solution, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-acetone-ethyl acetate-strong ammonia solution (2: 3: 4: 0.2) be developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) thin layer chromatography is differentiated Folium Mori: it is an amount of to get this product, removes film-coat, porphyrize, add methanol 10～100ml, supersound process 10～60 minutes filters, the filtrate evaporate to dryness, residue adds water 10～100ml makes dissolving, uses ethyl acetate extraction 1～3 time, each 10～100ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Mori control medicinal material 2g, adds petroleum ether (60～90 ℃) heating and refluxing extraction, discards petroleum ether liquid, and medicinal residues volatilize, add the ethanol supersound process, filter, filtrate evaporate to dryness, residue add the hot water stirring makes dissolving, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (the corresponding appendix of Chinese Pharmacopoeia), draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ethyl acetate-formic acid (5: 2: 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.
(3) measure content of matrine in this product:
Measure according to high performance liquid chromatography (the corresponding appendix of Chinese Pharmacopoeia).
Chromatographic condition and system suitability test are filler with amino bonded silica gel; With acetonitrile-methanol-3% phosphoric acid solution is mobile phase; UV-detector.
It is an amount of that the preparation precision of reference substance solution takes by weighing the matrine reference substance, adds appropriate solvent and make the solution that every 1ml contains 50 μ g, promptly.
The preparation of need testing solution is got this product and is removed coating, porphyrize.Get in right amount, the accurate title, decide, and puts in the measuring bottle, adds strong ammonia solution and soak into, add the methanol supersound process again, put coldly, be diluted to scale, shake up with methanol, filter, precision is measured the subsequent filtrate of certain volume, crosses the neutral alumina post, successively with chloroform, chloroform-methanol (5～10: 1～5) an amount of eluting, collect eluent, reclaim solvent to doing, residue adds appropriate solvent makes dissolving, be transferred in the measuring bottle, and be diluted to scale, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
3. as claim 1 and the described method of quality control of claim 2, it is characterized in that, (3) the described mobile phase of content of matrine can be that (85～95: 2～8: 2～8), the best is acetonitrile-methanol-3% phosphoric acid solution (90: 5: 5) to acetonitrile-methanol-3% phosphoric acid solution in mensuration this product
4. as claim 1 and the described method of quality control of claim 2, it is characterized in that the used mensuration wavelength of the described UV-detector of content of matrine can be 200nm～220nm in (3) mensuration this product, the best is 210nm.
5. as claim 1 and the described method of quality control of claim 2, it is characterized in that, (3) the described appropriate solvent of content of matrine can be methanol or acetonitrile or both any ratios in mensuration this product, (20～95: be good 80～5), the best is acetonitrile-methanol (80: 20) with acetonitrile-methanol.
6. as claim 1 and the described method of quality control of claim 2, also can be used for the quality control of other Runzao Zhiyang preparations, the sampling amount amount of regularlying sample of various preparations and deciding.
7. other Runzao Zhiyang preparations as claimed in claim 6 are meant in Runzao Zhiyang capsule prescription ratio, with the preparation that prior preparation method is made, comprise clinical or pharmaceutically acceptable common formulations such as tablet, capsule, granule, drop pill, oral liquid, syrup, soft extract, buccal tablet, pill, powder, suppository, patch, injection.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102000140A (en) * | 2010-11-08 | 2011-04-06 | 承德燕峰药业有限责任公司 | Novel method for synchronously quantifying matrine and oxymatrine in kuh-seng and preparations of kuh-seng |
| CN102349956A (en) * | 2011-10-18 | 2012-02-15 | 贵州同济堂制药有限公司 | Compound extract for moisturizeing pathogenic dryness and relieving itching and preparation thereof |
| CN104634884A (en) * | 2013-11-11 | 2015-05-20 | 河北以岭医药研究院有限公司 | Method for determining content of matrine in traditional Chinese medicine composition |
| CN108562685A (en) * | 2018-06-26 | 2018-09-21 | 成都中医药大学 | A kind of sealwort, mulberry leaf and radix polygonati officinalis compatibe drug composition quality detection method |
| CN109900827A (en) * | 2019-03-26 | 2019-06-18 | 陕西省食品药品监督检验研究院 | Survey the methods for commenting method to identify prepared fleece flower root based on one more |
| CN110208420A (en) * | 2019-06-26 | 2019-09-06 | 贵州中医药大学 | A kind of quality determining method of the yellow bitter cream of compound |
| CN112180024A (en) * | 2020-09-30 | 2021-01-05 | 西安雨田农业科技股份有限公司 | Quality control method of traditional Chinese medicine compound preparation for treating piglet diarrhea |
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- 2009-05-18 CN CNA2009101140709A patent/CN101574439A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102000140A (en) * | 2010-11-08 | 2011-04-06 | 承德燕峰药业有限责任公司 | Novel method for synchronously quantifying matrine and oxymatrine in kuh-seng and preparations of kuh-seng |
| CN102349956A (en) * | 2011-10-18 | 2012-02-15 | 贵州同济堂制药有限公司 | Compound extract for moisturizeing pathogenic dryness and relieving itching and preparation thereof |
| CN102349956B (en) * | 2011-10-18 | 2013-03-13 | 贵州同济堂制药有限公司 | Compound extract for moisturizeing pathogenic dryness and relieving itching and preparation thereof |
| CN104634884A (en) * | 2013-11-11 | 2015-05-20 | 河北以岭医药研究院有限公司 | Method for determining content of matrine in traditional Chinese medicine composition |
| CN108562685A (en) * | 2018-06-26 | 2018-09-21 | 成都中医药大学 | A kind of sealwort, mulberry leaf and radix polygonati officinalis compatibe drug composition quality detection method |
| CN108562685B (en) * | 2018-06-26 | 2020-05-12 | 成都中医药大学 | Quality detection method for rhizoma polygonati, folium mori and radix polygonati officinalis combined pharmaceutical composition |
| CN109900827A (en) * | 2019-03-26 | 2019-06-18 | 陕西省食品药品监督检验研究院 | Survey the methods for commenting method to identify prepared fleece flower root based on one more |
| CN109900827B (en) * | 2019-03-26 | 2022-02-11 | 陕西省食品药品监督检验研究院 | Method for identifying radix polygoni multiflori preparata based on one-test-multiple evaluation method |
| CN110208420A (en) * | 2019-06-26 | 2019-09-06 | 贵州中医药大学 | A kind of quality determining method of the yellow bitter cream of compound |
| CN112180024A (en) * | 2020-09-30 | 2021-01-05 | 西安雨田农业科技股份有限公司 | Quality control method of traditional Chinese medicine compound preparation for treating piglet diarrhea |
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