CN102662026A - Quality detecting method for traditional Chinese medicine Qianliening preparation - Google Patents
Quality detecting method for traditional Chinese medicine Qianliening preparation Download PDFInfo
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Abstract
The invention discloses a quality detecting method for traditional Chinese medicine Qianliening preparation. In the method, the quality standard of the existing traditional Chinese medicine Qianliening preparation is improved, and thin layer chromatography of myrobalan, safflower, pennycress seeds and radix et rhizoma rubies is added. According to the invention, the content of gallic acid and the content of hydroxyl safflower yellow A are simultaneously measured under the same chromatographic condition by adopting high performance liquid chromatography through varying the detection wave length of an ultraviolet detector. The thin layer chromatography has obvious characteristic spots and strong specificity. The high performance liquid chromatography is simple and practicable, has better accuracy and precision and can effectively ensure the preparation quality.
Description
Technical field
The present invention relates to a kind of quality determining method of Chinese medicine preparation, the quality determining method of Lenin's preparation before particularly a kind of Chinese medicine.
Background technology
The prostatitis Yiganning capsule is that gold is scolded the exclusive product of Tibetan medicine incorporated company, records in Chinese patent drug provincial standard rising national standard part standard numbering: WS-10627 (ZD-0627)-2002-2011Z.The prostatitis Yiganning capsule is: Semen thlaspis 58.7g, pyrrosia lingua 41.2g, dandelion 41.2g, Chinese juniper 29.3g, myrobalan 29.3g, sword bean 22.8g, mango core 17.5g, Portugal 17.5g, bonduc 17.5g, shellac 11.4g, ZANGQIANCAO 17.5g, safflower 11.4g, the cardamom 5.9g that is processed by the medicinal material of following weight proportion.More than 13 the flavor, be ground into fine powder, sieve, mixing incapsulates, and processes 1000.Have clearing heat and detoxicating, the effect that stagnation resolvation is treating stranguria.Be used for the hot malicious stasis of blood and hinder caused frequent micturition, urgent urination, odynuria belong to traditional Chinese medical science stranguria person.
Existing quality standard about preceding Lenin's medicine only adopts the TLC thin layer to differentiate the content of medicinal material shellac, an effective component gallic acid of HPLC mensuration simply; Do not find other quality determining methods in the prior art as yet for the prostatitis Yiganning capsule yet; Therefore existing quality determining method can not be controlled this quality comprehensively and accurately, and quality standard has much room for improvement.
Summary of the invention
To the deficiency of prior art, the purpose of this invention is to provide the quality determining method of a kind of Chinese medicine prostatitis Yiganning capsule and preparation thereof.
Summary of the invention
The invention provides a kind of thin layer discrimination method that detects myrobalan in Chinese medicine prostatitis Yiganning capsule and the preparation thereof, safflower 、 Semen thlaspis, ZANGQIANCAO; Adopt high performance liquid chromatography,, simultaneously the content of gallic acid and hydroxyl radical carthamin yellow carthamus A is measured thereby reach under same chromatographic condition through changing the detection wavelength of UV-detector; On the basis that has strengthened the product controllability, practiced thrift analysis time, improved work efficiency; Use gradient elution simultaneously; Protect chromatographic column, prolonged the serviceable life of chromatographic column, reduced cost.
The term explanation:
The prostatitis Yiganning capsule is the nomenclature of drug of national standard for traditional Chinese medicines compilation (Chinese patent drug provincial standard rising national standard part) record, standard numbering WS-10627 (ZD-0627)-2002-2011Z.
Before Lenin's preparation comprise the prostatitis Yiganning capsule and with other preparations of prostatitis Yiganning capsule bulk drug formulation.
Technical scheme of the present invention is following:
A kind of bulk drug consists of the quality determining method of Semen thlaspis 58.7 weight portions, pyrrosia lingua 41.2 weight portions, dandelion 41.2 weight portions, Chinese juniper 29.3 weight portions, myrobalan's 29.3 weight portions, sword bean 22.8 weight portions, mango core 17.5 weight portions, Portugal 17.5 weight portions, bonduc 17.5 weight portions, shellac 11.4 weight portions, ZANGQIANCAO 17.5 weight portions, safflower 11.4 weight portions, the preceding Lenin's preparation of cardamom 5.9 parts by weight of Chinese traditional medicine, and this method comprises one or more in following discriminating and/or the content assaying method:
Differentiate:
A, myrobalan's discriminating
Get the preceding Lenin's preparation 3-10g of Chinese medicine, add absolute ethyl alcohol 25-50ml, sonicated 20-30min adds zeyssatite 1-3g, and mixing filters, and filtrating is concentrated into 2ml, as need testing solution; Other gets myrobalan's control medicinal material 1-2g, adds absolute ethyl alcohol 25-50ml, and sonicated 20-30min adds zeyssatite 1-3g, and mixing filters, and filtrating is concentrated into 2ml, as control medicinal material solution; Other gets the gallic acid reference substance, adds methyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5-10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the methenyl choloride-ethyl acetate-formic acid that is 3-9:2-6:0.5-1.5, launches, and takes out; Dry; Spray is 1% ferric trichloride ethanolic solution with the mass and size portion rate, and it is clear to be heated to spot colour developing, in the test sample chromatogram; With reference substance and the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The discriminating of B, safflower
Get the preceding Lenin's preparation 3-10g of Chinese medicine, adding the volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, and jolting 10-20min leaves standstill, and gets supernatant, as need testing solution; Other gets safflower control medicinal material 1g, and adding the volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, and jolting 10-20min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5-10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the ethyl acetate-formic acid-water-methanol that is 5-9:1-3:2-4:0.2-0.6, launches, and takes out; Dry; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The discriminating of C 、 Semen thlaspis
Get the preceding Lenin's preparation 3-10g of Chinese medicine, adding the volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, and jolting 10-20min leaves standstill, and gets supernatant, as need testing solution; Qu Semen thlaspis control medicinal material 1g in addition, adding the volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, jolting 10-20min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5-10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the upper solution that is normal butyl alcohol-glacial acetic acid-water mixed solution of 2-6:0.5-1.5:3-7, launches, and takes out; Dry, spray is 10% ethanol solution of sulfuric acid with the volume parts ratio, and 100-105 ℃ to be heated to the spot colour developing clear; Put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
The discriminating of D, ZANGQIANCAO
Get the preceding Lenin's preparation 3-10g of Chinese medicine, add methyl alcohol 25-50ml, sonicated 20-30min filters, and filtrating is concentrated into 1ml, as need testing solution; Other gets ZANGQIANCAO control medicinal material 1-2g, adds methyl alcohol 25-50ml, and sonicated 20-30min filters, and filtrating is concentrated into 1ml, as need testing solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5-10 μ l of above-mentioned solution respectively, put on same silica gel g thin-layer plate; Is developping agent with volume parts than the sherwood oil-acetone that is 2-6:0.5-1.5, and the sherwood oil boiling range is 60～90 ℃, launches; Take out, dry, put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Assay:
According to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 D)
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With the acetonitrile is mobile phase A; Is Mobile phase B with volume parts than 1% glacial acetic acid aqueous solution; Adopt the gradient elution mode: 0min → 20min → 25min → 50min → 55min → 60min, according to the above-mentioned time period, acetonitrile, volume parts are carried out wash-out simultaneously than 1% glacial acetic acid aqueous solution; Wherein, acetonitrile: 1% → 1% → 24% → 24% → 100% → 1%; Volume parts is than 1% glacial acetic acid aqueous solution: 99% → 99% → 76% → 76% → 0% → 99%; Use the detection wavelength of 275nm in time at 0min → 20min; It is 403nm that 20min changes the detection wavelength, and 21min makes the detecting device balance, uses the detection wavelength of 403nm in 21min → 60min time.Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: get the gallic acid reference substance, the hydroxyl radical carthamin yellow carthamus A reference substance is an amount of; The accurate title, decide; Add volume parts and process the solution that every 1ml contains gallic acid 20 μ g, hydroxyl radical carthamin yellow carthamus A 0.2mg respectively, promptly get than 40-60% ethanol water;
The preparation of need testing solution: get the preceding Lenin's preparation powder 3g of Chinese medicine, cross sieve No. three, the accurate title, decide, and puts in the tool plug conical flask; The accurate volume parts that adds is than 40-60% ethanol water 50ml, and close plug claims to decide weight, sonicated 30 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake than 40-60% ethanol water, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 5-10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
Lenin's preparation is meant by prostatitis Yiganning capsule bulk drug prescription Semen thlaspis 58.7 weight portions, pyrrosia lingua 41.2 weight portions, dandelion 41.2 weight portions, Chinese juniper 29.3 weight portions, myrobalan's 29.3 weight portions, sword bean 22.8 weight portions, mango core 17.5 weight portions, Portugal 17.5 weight portions, bonduc 17.5 weight portions, shellac 11.4 weight portions, ZANGQIANCAO 17.5 weight portions, safflower 11.4 weight portions, cardamom 5.9 weight portions before described; Through cleaning; Remove impurity; Temperature is lower than 60 ℃ of dryings; Mix, micronizer is ground into 0.1-50 μ m superfine powder, presses common process; Add conventional auxiliary material and be prepared into clinical acceptable any formulation, comprise capsule, pill, micropill, dripping pill, tablet, soft capsule, particle or oral liquid.
Preferably; A kind of bulk drug consists of the quality determining method of Semen thlaspis 58.7 weight portions, pyrrosia lingua 41.2 weight portions, dandelion 41.2 weight portions, Chinese juniper 29.3 weight portions, myrobalan's 29.3 weight portions, sword bean 22.8 weight portions, mango core 17.5 weight portions, Portugal 17.5 weight portions, bonduc 17.5 weight portions, shellac 11.4 weight portions, ZANGQIANCAO 17.5 weight portions, safflower 11.4 weight portions, cardamom 5.9 parts by weight of Chinese traditional medicine prostatitis Yiganning capsules, and this method comprises one or more in following discriminating and/or the content assaying method:
Differentiate:
A, myrobalan's discriminating
Get Chinese medicine prostatitis Yiganning capsule content 5g, add absolute ethyl alcohol 25ml, sonicated 30min adds zeyssatite 2g, and mixing filters, and filtrating is concentrated into 2ml, as need testing solution; Other gets myrobalan's control medicinal material 1g, adds absolute ethyl alcohol 25ml, and sonicated 30min adds zeyssatite 2g, and mixing filters, and filtrating is concentrated into 2ml, as control medicinal material solution; Other gets the gallic acid reference substance, adds methyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the methenyl choloride-ethyl acetate-formic acid that is 6:4:1, launches, and takes out; Dry; Spray is 1% ferric trichloride ethanolic solution with the mass and size portion rate, and it is clear to be heated to spot colour developing, in the test sample chromatogram; With reference substance and the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The discriminating of B, safflower
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding the volume parts ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as need testing solution; Other gets safflower control medicinal material 1g, and adding volume ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the ethyl acetate-formic acid-water-methanol that is 7:2:3:0.4, launches, and takes out; Dry; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The discriminating of C 、 Semen thlaspis
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding the volume parts ratio is 80% acetone soln 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as need testing solution; Qu Semen thlaspis control medicinal material 1g in addition, adding volume ratio is 80% acetone soln 30ml, close plug, jolting 15min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; The upper solution that with the volume ratio is normal butyl alcohol-glacial acetic acid-water mixed solution of 4:1:5 is a developping agent, launches, and takes out; Dry, spray is 10% ethanol solution of sulfuric acid with the volume parts ratio, and 105 ℃ to be heated to the spot colour developing clear; Put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
The discriminating of D, ZANGQIANCAO
Get Chinese medicine prostatitis Yiganning capsule content 5g, add methyl alcohol 30ml, sonicated 30min filters, and filtrating is concentrated into 1ml, as need testing solution; Other gets ZANGQIANCAO control medicinal material 1g, adds methyl alcohol 30ml, and sonicated 30min filters, and filtrating is concentrated into 1ml, as need testing solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 10 μ l of above-mentioned solution respectively, put on same silica gel g thin-layer plate; Is developping agent with volume parts than the sherwood oil-acetone that is 4:1, and the sherwood oil boiling range is 60～90 ℃, launches; Take out, dry, put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Assay:
According to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 D)
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With the acetonitrile is mobile phase A; Is Mobile phase B with volume parts than 1% glacial acetic acid aqueous solution; Adopt the gradient elution mode: 0min → 20min → 25min → 50min → 55min → 60min, according to the above-mentioned time period, acetonitrile, volume parts are carried out wash-out simultaneously than 1% glacial acetic acid aqueous solution; Wherein, acetonitrile: 1% → 1% → 24% → 24% → 100% → 1%; Volume parts is than 1% glacial acetic acid aqueous solution: 99% → 99% → 76% → 76% → 0% → 99%; Use the detection wavelength of 275nm in time at 0min → 20min; It is 403nm that 20min changes the detection wavelength, and 21min makes the detecting device balance, uses the detection wavelength of 403nm in 21min → 60min time.Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: get the gallic acid reference substance, the hydroxyl radical carthamin yellow carthamus A reference substance is an amount of; The accurate title, decide; Add volume parts and process the solution that contains gallic acid 20 μ g, hydroxyl radical carthamin yellow carthamus A 0.2mg among every 1ml respectively, promptly get than 50% ethanol water;
The preparation of need testing solution: get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, the accurate title, decide, and puts in the tool plug conical flask; The accurate volume parts that adds is than 50% ethanol water 50ml, and close plug claims to decide weight, sonicated 30 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake than 50% ethanol water, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
Myrobalan's content is with gallic acid (C in the Yiganning capsule of Chinese medicine of the present invention prostatitis
7H
6O
5) meter, must not be less than 2.0mg/g; Safflower content is with hydroxyl radical carthamin yellow carthamus A (C
27H
30O
15) meter, must not be less than 0.26mg/g.
The unit corresponding relation of weight portion described in this instructions and parts by volume is g/ml or kg/l.
Compared with prior art, advantage of the present invention is following:
Existing quality standard about preceding Lenin's medicine only adopts the TLC thin layer to differentiate the content of medicinal material shellac, an effective component gallic acid of HPLC mensuration simply, causes preceding Lenin's formulation products quality testing not accurate, and quality standard has much room for improvement.The present invention to existing Chinese medicine before Lenin's preparation quality standard carried out corresponding raising, on the basis of primary standard, increased the discriminating of myrobalan, safflower, Semen thlaspis, ZANGQIANCAO; The present invention adopts identical conditions, and the separation determination of a plurality of compositions as adopting high performance liquid chromatography, through changing the detection wavelength of UV-detector, thereby reaches under same chromatographic condition simultaneously the assay to gallic acid and hydroxyl radical carthamin yellow carthamus A.The result shows that method is simple and feasible, has accuracy and precision preferably, can guarantee this quality effectively.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1: identification experiment
Chinese medicine prostatitis Yiganning capsule is scolded Tibetan medicine medicine company incorporated company by the Qinghai gold and is provided.
A, myrobalan's discriminating
Get Chinese medicine prostatitis Yiganning capsule content 5g, add absolute ethyl alcohol 25ml, sonicated 30min adds zeyssatite 2g, and mixing filters, and filtrating is concentrated into 2ml, as need testing solution; Other gets myrobalan's control medicinal material 1g, adds absolute ethyl alcohol 25ml, and sonicated 30min adds zeyssatite 2g, and mixing filters, and filtrating is concentrated into 2ml, as control medicinal material solution; Other gets the gallic acid reference substance, adds methyl alcohol and processes solution that every 1ml contains 1mg as contrast solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride-ethyl acetate-formic acid is developping agent, and developping agent volume parts ratio is a developping agent for methenyl choloride-ethyl acetate-formic acid of getting (6:4:1), (5:5:0.8), (7:5:0.6) in the scope of 3-9:2-6:0.5-1.5 respectively, launches; Take out, dry, spray is 1% ferric trichloride ethanolic solution with the mass and size portion rate; It is clear to be heated to the spot colour developing; In the test sample chromatogram, with reference substance and the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Interpretation of result: under volume parts compares for methenyl choloride-ethyl acetate of 3-9:2-6:0.5-1.5-formic acid developping agent condition, have and launch effect preferably.Wherein, volume parts is more best than the developping agent expansion effect of methenyl choloride-ethyl acetate-formic acid of 6:4:1.
The discriminating of B, safflower
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding the volume parts ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as need testing solution; Other gets safflower control medicinal material 1g, and adding volume ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; With ethyl acetate-formic acid-water-methanol is developping agent; Developping agent volume parts ratio is a developping agent for ethyl acetate-formic acid-water-methanol of getting (7:2:3:0.4), (6:2:4:0.5), (9:1:4:0.2) in the scope of 5-9:1-3:2-4:0.2-0.6 respectively, launches, and takes out; Dry; In the test sample chromatogram, with reference substance and the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Interpretation of result: under volume parts compares for ethyl acetate-formic acid of 3-9:2-6:0.5-1.5-water-methanol developping agent condition, have and launch effect preferably.Wherein, volume parts is more best than the developping agent expansion effect of ethyl acetate-formic acid-water-methanol of 7:2:3:0.4.
The discriminating of C 、 Semen thlaspis
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding the volume parts ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as need testing solution; Qu Semen thlaspis control medicinal material 1g in addition, adding the volume parts ratio is 80% water acetone soln 30ml, close plug, jolting 15min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Upper solution with normal butyl alcohol-glacial acetic acid-water mixed solution is a developping agent, and developping agent volume parts ratio is a developping agent for the upper solution of getting normal butyl alcohol-glacial acetic acid-water mixed solution of (4:1:5), (5:1.2:3), (2:0.6:6) in the scope of 2-6:0.5-1.5:3-7 respectively, launches; Take out; Dry, spray is 10% ethanol solution of sulfuric acid with the mass and size portion rate, and 105 ℃ to be heated to the spot colour developing clear; Put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Interpretation of result: volume parts than upper solution developping agent condition for normal butyl alcohol-glacial acetic acid of 2-6:0.5-1.5:3-7-water mixed solution under, have and launch effect preferably.Wherein, volume parts is more best than the developping agent expansion effect of the upper solution of normal butyl alcohol-glacial acetic acid-water mixed solution of 4:1:5.
The discriminating of D, ZANGQIANCAO
Get Chinese medicine prostatitis Yiganning capsule content 5g, add methyl alcohol 30ml, sonicated 30min filters, and filtrating is concentrated into 1ml, as need testing solution; Other gets ZANGQIANCAO control medicinal material 1g, adds methyl alcohol 30ml, and sonicated 30min filters, and filtrating is concentrated into 1ml, as need testing solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 10 μ l of above-mentioned solution respectively, put on same silica gel g thin-layer plate; With sherwood oil-acetone is developping agent, and the sherwood oil boiling range is 60～90 ℃, and developping agent volume parts ratio is a developping agent for sherwood oil-acetone of getting (4:1), (5:0.5), (2:1.5) in the scope of 2-6:0.5-1.5 respectively; Launch; Take out, dry, put under the uviol lamp 365nm and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of identical face.
Interpretation of result: under volume parts compares for the sherwood oil of 2-6:0.5-1.5-acetone developping agent condition, have and launch effect preferably.Wherein, volume parts is more best than the developping agent expansion effect of sherwood oil-acetone of 4:1.
Experimental example 2: assay experiment
1, instrument, reagent and confession test agent
Instrument: the L-2100 of Hitachi pump, the L-2400 of Hitachi UV-detector, Tianjin, island AUW-220D type electronic balance.
Reference substance: gallic acid reference substance (Nat'l Pharmaceutical & Biological Products Control Institute) lot number: 110831-200803, hydroxyl radical carthamin yellow carthamus A reference substance (Nat'l Pharmaceutical & Biological Products Control Institute) lot number: 111637-200905.
Sample: prostatitis Yiganning capsule (the Qinghai gold is scolded Tibetan medicine medicine company incorporated company and provided), lot number: 20110216,20110217,20110218.
2, detect the selection of wavelength
Get gallic acid, hydroxyl radical carthamin yellow carthamus A reference substance solution respectively, in 200～500nm wavelength coverage, carry out UV scanning.According to ultraviolet absorpting spectrum, selected 275nm is the detection wavelength of gallic acid, and selected 403nm is the detection wavelength of hydroxyl radical carthamin yellow carthamus A.Detect wavelength change and see table 1.
Table 1 detects the wavelength change table
3, moving phase is selected
Gallic acid and hydroxyl radical carthamin yellow carthamus A polarity differ bigger, adopt isocratic elution to be difficult to two kinds of compositions are carried out wash-out simultaneously, so select gradient elution to carry out chromatographic resolution.
Use methanol-water, find when the acetonitrile-water system is carried out chromatographic resolution, the peak hangover is serious.After water added acid, peak shape was greatly improved.Experimental result shows that when using acetonitrile-volume parts to carry out gradient elution than 1% glacial acetic acid aqueous solution as moving phase, gallic acid and hydroxyl radical carthamin yellow carthamus A all can reach separating effect preferably.Therefore confirm that mobile phase A is an acetonitrile, Mobile phase B is that volume parts is than 1% glacial acetic acid aqueous solution.
4, the selection of gradient elution time
Acetonitrile-volume parts is 0～5:100～95 o'clock than 1% glacial acetic acid aqueous solution at the volume parts ratio, gallic acid peak retention time and degree of separation appropriate; Acetonitrile-volume parts is 20～30:80～70 o'clock than 1% glacial acetic acid aqueous solution at the volume parts ratio, and hydroxyl radical carthamin yellow carthamus A begins wash-out, peak retention time and degree of separation appropriate.Through discovering, when carrying out wash-out by table 2, the degree of separation of gallic acid and hydroxyl radical carthamin yellow carthamus A and adjacent peak is all greater than 1.5, and separating effect is better, satisfies and detects requirement.See accompanying drawing 1 and accompanying drawing 2.
Table 2 eluent gradient table
5, the preparation of reference substance solution
Get the gallic acid reference substance, the hydroxyl radical carthamin yellow carthamus A reference substance is an amount of, accurate claims surely, adds volume parts and processes the mixed solution that every 1ml contains gallic acid 0.2mg, hydroxyl radical carthamin yellow carthamus A 10 μ g than 50% ethanolic solution, promptly get.
6, test sample preparation
6.1 method for distilling is selected
Take medicine capsule contents Qianliening powder 3g, over the 3rd screen, accurately weighed, set stoppered Erlenmeyer flask, precision volume fraction greater than 50% ethanol solution 50ml, Mesa, said that given the weight, respectively, ultrasound, reflux , vibration Oscillating treatment 30min, let cool, then weighed and the weight ratio with a volume fraction of 50% ethanol solution weight loss supplement, shake, filtration, the filtrate obtained, that is, too.The result sees table 3.
Table 3 method for distilling is investigated test findings
The result shows that gallic acid, hydroxyl radical carthamin yellow carthamus A content that ultrasonic Extraction is measured are the highest, so confirm that method for distilling is a ultrasonic Extraction.
6.2 extracting solvent selects
Get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, the accurate title, decide, and puts in the tool plug conical flask; Accurate respectively adding volume parts is than 40%, 50%, 60% ethanol water 50ml, and close plug claims to decide weight, sonicated 30min; Put coldly, claim again to decide weight, supply the weight that subtracts mistake with volume parts than 40%, 50%, 60% ethanol water respectively, shake up; Filter, get subsequent filtrate, promptly get.The result sees table 4.
Table 4 extracts solvent and investigates test findings
The result shows, the gallic acid that volume parts is surveyed than 50% ethanol water, hydroxyl radical carthamin yellow carthamus A content are higher, so select for use volume parts than the extraction solvent of 50% ethanol water as test sample.
6.3 extraction time is selected
Get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, the accurate title, decide, and puts in the tool plug conical flask; The accurate volume parts that adds is than 50% ethanol water 50ml, and close plug claims to decide weight, respectively sonicated 20,30,40min; Put coldly, claim again to decide weight, supply the weight that subtracts mistake than 50% ethanol water, shake up with volume parts; Filter, get subsequent filtrate, promptly get.The result sees table 5.
Table 5 extraction time investigation test findings
| Extraction time (min) | 20 | 30 | 40 |
| Gallic acid content (mg/ grain) | 0.912 | 0.915 | 0.915 |
| Sydroxy carthamin content (mg/ grain) | 0.0786 | 0.0788 | 0.0785 |
The result shows that gallic acid, hydroxyl radical carthamin yellow carthamus A extract fully basically when extraction time is 20min, be extraction time in order to guarantee that 30min is selected in the test sample extraction fully.
7, the investigation of the preparation of typical curve and linear relationship
Precision is measured gallic acid reference substance stock solution solution (337.6 μ g/ml) and hydroxyl radical carthamin yellow carthamus A reference substance stock solution solution (26.8 μ g/ml) 1ml, 3ml, 5ml, 8ml, 10ml; Put respectively in the 10ml volumetric flask, volume parts is diluted to scale than 50% ethanol water, shakes up; Each accurate sample introduction 10 μ l; With peak area (A) is ordinate, and reference substance concentration (C) is horizontal ordinate, carries out linear regression.See table 6, table 7 and accompanying drawing 3 and accompanying drawing 4.
Table 6 gallic acid linear relationship is investigated the result
Regression equation: A=15682C-16290
Related coefficient: R=0.9996
Table 7 hydroxyl radical carthamin yellow carthamus A linear relationship is investigated the result
Regression equation: A=11344C-3478.5
Related coefficient: R=0.9998
The result shows: gallic acid is in 33.76 μ g/ml～337.60 μ g/ml scopes, and linear relationship is good; Hydroxyl radical carthamin yellow carthamus A is in 2.68～26.80 μ g/ml scopes, and linear relationship is good.
8, precision test
Accurate gallic acid, the hydroxyl radical carthamin yellow carthamus A mixing contrast solution 10 μ l of drawing inject liquid chromatograph, METHOD FOR CONTINUOUS DETERMINATION 6 times, and the record peak area also calculates relative standard deviation.The result shows: instrument precision is good.See table 8, table 9.
Table 8 gallic acid Precision test result
Table 9 hydroxyl radical carthamin yellow carthamus A Precision test result
9, stability test
After the need testing solution preparation was accomplished, the accurate 10 μ l that draw injected liquid chromatograph, and the record peak area was whenever measured once at a distance from 2 hours later on, investigated 8 hours, calculated the relative standard deviation of peak area.The result shows: it is stable that need testing solution was measured the result in 8 hours.See table 10, table 11.
Table 10 sample stability gallic acid test findings
Table 11 sample stability hydroxyl radical carthamin yellow carthamus A test findings
10, replica test
Get same lot sample article, replication 6 times, gallic acid, hydroxyl radical carthamin yellow carthamus A content in the calculation sample.The result shows that analytical approach repeatability is good.See table 12, table 13.
Table 12 gallic acid replica test result
Table 13 hydroxyl radical carthamin yellow carthamus A replica test result
11, recovery test
Precision takes by weighing 6 parts of same lot sample article, and accurate gallic acid, the hydroxyl radical carthamin yellow carthamus A reference substance of adding measured its content, calculate recovery rate.The result shows that it is accurate that this assay method is measured the result.See table 14, table 15.
Table 14 gallic acid recovery test result
Table 15 hydroxyl radical carthamin yellow carthamus A recovery test result
12, sample determination
Get it filled three batches of thing prostatitis Yiganning capsules are measured and are also calculated gallic acid, hydroxyl radical carthamin yellow carthamus A content, result such as following table 16.
Table 16 sample size is measured the result
Following embodiment all can realize the described effect of above-mentioned experimental example.
Description of drawings:
Fig. 1 is that gallic acid, hydroxyl radical carthamin yellow carthamus A mix the contrast high-efficient liquid phase chromatogram;
Fig. 2 is a medicine prostatitis Yiganning capsule high-efficient liquid phase chromatogram;
Fig. 3 is the gallic acid linear relationship chart;
Fig. 4 is the hydroxyl radical carthamin yellow carthamus A linear relationship chart;
Wherein, the horizontal ordinate of Fig. 1, Fig. 2 is the time, unit: minute (Minutes); Ordinate is a voltage, unit: volt (Volts).
Embodiment
Below in conjunction with embodiment the present invention is done detailed elaboration, but be not limited to the embodiment of these concrete records.The prostatitis Yiganning capsule that is detected is scolded Tibetan medicine medicine company incorporated company product for the Qinghai gold and is sold.
Embodiment 1: the discrimination method of Chinese medicine prostatitis Yiganning capsule
A, myrobalan's discriminating
Get Chinese medicine prostatitis Yiganning capsule content 5g, add absolute ethyl alcohol 25ml, sonicated 30min adds zeyssatite 2g, and mixing filters, and filtrating is concentrated into 2ml, as need testing solution; Other gets myrobalan's control medicinal material 1g, adds absolute ethyl alcohol 25ml, and sonicated 30min adds zeyssatite 2g, and mixing filters, and filtrating is concentrated into 2ml, as control medicinal material solution; Other gets the gallic acid reference substance, adds methyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the methenyl choloride-ethyl acetate-formic acid that is 6:4:1, launches, and takes out; Dry; Spray is 1% ferric trichloride ethanolic solution with the mass and size portion rate, and it is clear to be heated to spot colour developing, in the test sample chromatogram; With reference substance and the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The discriminating of B, safflower
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding the volume parts ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as need testing solution; Other gets safflower control medicinal material 1g, and adding volume ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the ethyl acetate-formic acid-water-methanol that is 7:2:3:0.4, launches, and takes out; Dry; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The discriminating of C 、 Semen thlaspis
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding the volume parts ratio is 80% acetone soln 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as need testing solution; Qu Semen thlaspis control medicinal material 1g in addition, adding volume ratio is 80% acetone soln 30ml, close plug, jolting 15min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; The upper solution that with the volume ratio is normal butyl alcohol-glacial acetic acid-water mixed solution of 4:1:5 is a developping agent, launches, and takes out; Dry, spray is 10% ethanol solution of sulfuric acid with the volume parts ratio, and 105 ℃ to be heated to the spot colour developing clear; Put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
The discriminating of D, ZANGQIANCAO
Get Chinese medicine prostatitis Yiganning capsule content 5g, add methyl alcohol 30ml, sonicated 30min filters, and filtrating is concentrated into 1ml, as need testing solution; Other gets ZANGQIANCAO control medicinal material 1g, adds methyl alcohol 30ml, and sonicated 30min filters, and filtrating is concentrated into 1ml, as need testing solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 10 μ l of above-mentioned solution respectively, put on same silica gel g thin-layer plate; Is developping agent with volume parts than the sherwood oil-acetone that is 4:1, and the sherwood oil boiling range is 60～90 ℃, launches; Take out, dry, put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Embodiment 2: the content assaying method of Chinese medicine prostatitis Yiganning capsule
According to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 D)
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With the acetonitrile is mobile phase A; Is Mobile phase B with volume parts than 1% glacial acetic acid aqueous solution; Adopt the gradient elution mode: 0min → 20min → 25min → 50min → 55min → 60min, according to the above-mentioned time period, acetonitrile, volume parts are carried out wash-out simultaneously than 1% glacial acetic acid aqueous solution; Wherein, acetonitrile: 1% → 1% → 24% → 24% → 100% → 1%; Volume parts is than 1% glacial acetic acid aqueous solution: 99% → 99% → 76% → 76% → 0% → 99%; Use the detection wavelength of 275nm in time at 0min → 20min; It is 403nm that 20min changes the detection wavelength, and 21min makes the detecting device balance, uses the detection wavelength of 403nm in 21min → 60min time.Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: get the gallic acid reference substance, the hydroxyl radical carthamin yellow carthamus A reference substance is an amount of; The accurate title, decide; Add volume parts and process the solution that every 1ml contains gallic acid 20 μ g, hydroxyl radical carthamin yellow carthamus A 0.2mg respectively, promptly get than 50% ethanol water.
The preparation of need testing solution: get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, the accurate title, decide, and puts in the tool plug conical flask; The accurate volume parts that adds is than 50% ethanol water 50ml, and close plug claims to decide weight, sonicated 30 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake than 50% ethanol water, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
Myrobalan's content is with gallic acid (C in the preceding Lenin's preparation of Chinese medicine of the present invention
7H
6O
5) meter, be 2.1mg/g; Safflower content is with hydroxyl radical carthamin yellow carthamus A (C
27H
30O
15) meter, be 0.283mg/g.
Claims (3)
1. a bulk drug consists of the quality determining method of Lenin's preparation before Semen thlaspis 58.7 weight portions, pyrrosia lingua 41.2 weight portions, dandelion 41.2 weight portions, Chinese juniper 29.3 weight portions, myrobalan's 29.3 weight portions, sword bean 22.8 weight portions, mango core 17.5 weight portions, Portugal 17.5 weight portions, bonduc 17.5 weight portions, shellac 11.4 weight portions, ZANGQIANCAO 17.5 weight portions, safflower 11.4 weight portions, cardamom 5.9 parts by weight of Chinese traditional medicine; It is characterized in that this method comprises one or more in following discriminating and/or the content assaying method:
Differentiate:
A, myrobalan's discriminating
Get the preceding Lenin's preparation 3-10g of Chinese medicine, add absolute ethyl alcohol 25-50ml, sonicated 20-30min adds zeyssatite 1-3g, and mixing filters, and filtrating is concentrated into 2ml, as need testing solution; Other gets myrobalan's control medicinal material 1-2g, adds absolute ethyl alcohol 25-50ml, and sonicated 20-30min adds zeyssatite 1-3g, and mixing filters, and filtrating is concentrated into 2ml, as control medicinal material solution; Other gets the gallic acid reference substance, adds methyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5-10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the methenyl choloride-ethyl acetate-formic acid that is 3-9:2-6:0.5-1.5, launches, and takes out; Dry; Spray is 1% ferric trichloride ethanolic solution with the mass and size portion rate, and it is clear to be heated to spot colour developing, in the test sample chromatogram; With reference substance and the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The discriminating of B, safflower
Get the preceding Lenin's preparation 3-10g of Chinese medicine, adding the volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, and jolting 10-20min leaves standstill, and gets supernatant, as need testing solution; Other gets safflower control medicinal material 1g, and adding the volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, and jolting 10-20min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5-10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the ethyl acetate-formic acid-water-methanol that is 5-9:1-3:2-4:0.2-0.6, launches, and takes out; Dry; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The discriminating of C 、 Semen thlaspis
Get the preceding Lenin's preparation 3-10g of Chinese medicine, adding the volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, and jolting 10-20min leaves standstill, and gets supernatant, as need testing solution; Qu Semen thlaspis control medicinal material 1g in addition, adding the volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, jolting 10-20min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5-10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the upper solution that is normal butyl alcohol-glacial acetic acid-water mixed solution of 2-6:0.5-1.5:3-7, launches, and takes out; Dry, spray is 10% ethanol solution of sulfuric acid with the volume parts ratio, and 100-105 ℃ to be heated to the spot colour developing clear; Put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
The discriminating of D, ZANGQIANCAO
Get the preceding Lenin's preparation 3-10g of Chinese medicine, add methyl alcohol 25-50ml, sonicated 20-30min filters, and filtrating is concentrated into 1ml, as need testing solution; Other gets ZANGQIANCAO control medicinal material 1-2g, adds methyl alcohol 25-50ml, and sonicated 20-30min filters, and filtrating is concentrated into 1ml, as need testing solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5-10 μ l of above-mentioned solution respectively, put on same silica gel g thin-layer plate; Is developping agent with volume parts than the sherwood oil-acetone that is 2-6:0.5-1.5, and the sherwood oil boiling range is 60～90 ℃, launches; Take out, dry, put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
Assay:
According to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 D)
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With the acetonitrile is mobile phase A; Is Mobile phase B with volume parts than 1% glacial acetic acid aqueous solution; Adopt the gradient elution mode: 0min → 20min → 25min → 50min → 55min → 60min, according to the above-mentioned time period, acetonitrile, volume parts are carried out wash-out simultaneously than 1% glacial acetic acid aqueous solution; Wherein, acetonitrile: 1% → 1% → 24% → 24% → 100% → 1%; Volume parts is than 1% glacial acetic acid aqueous solution: 99% → 99% → 76% → 76% → 0% → 99%; Use the detection wavelength of 275nm in time at 0min → 20min; It is 403nm that 20min changes the detection wavelength, and 21min makes the detecting device balance, uses the detection wavelength of 403nm in 21min → 60min time; Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: get the gallic acid reference substance, the hydroxyl radical carthamin yellow carthamus A reference substance is an amount of; The accurate title, decide; Add volume parts and process the solution that every 1ml contains gallic acid 20 μ g, hydroxyl radical carthamin yellow carthamus A 0.2mg respectively, promptly get than 40-60% ethanol water;
The preparation of need testing solution: get the preceding Lenin's preparation powder 3g of Chinese medicine, cross sieve No. three, the accurate title, decide, and puts in the tool plug conical flask; The accurate volume parts that adds is than 40-60% ethanol water 50ml, and close plug claims to decide weight, sonicated 30 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake than 40-60% ethanol water, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 5-10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
2. the quality determining method of Lenin's preparation before a kind of Chinese medicine as claimed in claim 1; It is characterized in that described preceding Lenin's preparation is meant by prostatitis Yiganning capsule bulk drug prescription Semen thlaspis 58.7 weight portions, pyrrosia lingua 41.2 weight portions, dandelion 41.2 weight portions, Chinese juniper 29.3 weight portions, myrobalan's 29.3 weight portions, sword bean 22.8 weight portions, mango core 17.5 weight portions, Portugal 17.5 weight portions, bonduc 17.5 weight portions, shellac 11.4 weight portions, ZANGQIANCAO 17.5 weight portions, safflower 11.4 weight portions, cardamom 5.9 weight portions; Through cleaning; Remove impurity; Temperature is lower than 60 ℃ of dryings; Mix, micronizer is ground into 0.1-50 μ m superfine powder, presses common process; Add conventional auxiliary material and be prepared into clinical acceptable any formulation, comprise capsule, pill, micropill, dripping pill, tablet, soft capsule, particle or oral liquid.
3. the quality determining method of Lenin's preparation before a kind of Chinese medicine as claimed in claim 1 is characterized in that this method comprises one or more in following discriminating and/or the content assaying method:
Differentiate:
A, myrobalan's discriminating
Get Chinese medicine prostatitis Yiganning capsule content 5g, add absolute ethyl alcohol 25ml, sonicated 30min adds zeyssatite 2g, and mixing filters, and filtrating is concentrated into 2ml, as need testing solution; Other gets myrobalan's control medicinal material 1g, adds absolute ethyl alcohol 25ml, and sonicated 30min adds zeyssatite 2g, and mixing filters, and filtrating is concentrated into 2ml, as control medicinal material solution; Other gets the gallic acid reference substance, adds methyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the methenyl choloride-ethyl acetate-formic acid that is 6:4:1, launches, and takes out; Dry; Spray is 1% ferric trichloride ethanolic solution with the mass and size portion rate, and it is clear to be heated to spot colour developing, in the test sample chromatogram; With reference substance and the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The discriminating of B, safflower
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding the volume parts ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as need testing solution; Other gets safflower control medicinal material 1g, and adding volume ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; Is developping agent with volume parts than the ethyl acetate-formic acid-water-methanol that is 7:2:3:0.4, launches, and takes out; Dry; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The discriminating of C 、 Semen thlaspis
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding the volume parts ratio is 80% acetone soln 30ml, close plug, and jolting 15min leaves standstill, and gets supernatant, as need testing solution; Qu Semen thlaspis control medicinal material 1g in addition, adding volume ratio is 80% acetone soln 30ml, close plug, jolting 15min leaves standstill, and gets supernatant, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate; The upper solution that with the volume ratio is normal butyl alcohol-glacial acetic acid-water mixed solution of 4:1:5 is a developping agent, launches, and takes out; Dry, spray is 10% ethanol solution of sulfuric acid with the volume parts ratio, and 105 ℃ to be heated to the spot colour developing clear; Put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
The discriminating of D, ZANGQIANCAO
Get Chinese medicine prostatitis Yiganning capsule content 5g, add methyl alcohol 30ml, sonicated 30min filters, and filtrating is concentrated into 1ml, as need testing solution; Other gets ZANGQIANCAO control medicinal material 1g, adds methyl alcohol 30ml, and sonicated 30min filters, and filtrating is concentrated into 1ml, as need testing solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 10 μ l of above-mentioned solution respectively, put on same silica gel g thin-layer plate; Is developping agent with volume parts than the sherwood oil-acetone that is 4:1, and the sherwood oil boiling range is 60～90 ℃, launches; Take out, dry, put under the uviol lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
Assay:
According to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 D)
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With the acetonitrile is mobile phase A; Is Mobile phase B with volume parts than 1% glacial acetic acid aqueous solution; Adopt the gradient elution mode: 0min → 20min → 25min → 50min → 55min → 60min, according to the above-mentioned time period, acetonitrile, volume parts are carried out wash-out simultaneously than 1% glacial acetic acid aqueous solution; Wherein, acetonitrile: 1% → 1% → 24% → 24% → 100% → 1%; Volume parts is than 1% glacial acetic acid aqueous solution: 99% → 99% → 76% → 76% → 0% → 99%; Use the detection wavelength of 275nm in time at 0min → 20min; It is 403nm that 20min changes the detection wavelength, and 21min makes the detecting device balance, uses the detection wavelength of 403nm in 21min → 60min time; Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: get the gallic acid reference substance, the hydroxyl radical carthamin yellow carthamus A reference substance is an amount of; The accurate title, decide; Add volume parts and process the solution that every 1ml contains gallic acid 20 μ g, hydroxyl radical carthamin yellow carthamus A 0.2mg respectively, promptly get than 50% ethanol water;
The preparation of need testing solution: get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, the accurate title, decide, and puts in the tool plug conical flask; The accurate volume parts that adds is than 50% ethanol water 50ml, and close plug claims to decide weight, sonicated 30 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake than 50% ethanol water, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
Myrobalan's content is with gallic acid (C in the Yiganning capsule of Chinese medicine of the present invention prostatitis
7H
6O
5) meter, must not be less than 2.0mg/g; Safflower content is with hydroxyl radical carthamin yellow carthamus A (C
27H
30O
15) meter, must not be less than 0.26mg/g.
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|---|---|---|---|---|
| CN102841095A (en) * | 2012-09-27 | 2012-12-26 | 山东阿如拉药物研究开发有限公司 | Quality testing method for Liuwei Mingmu preparation of Tibetan medicine composition |
| CN102841095B (en) * | 2012-09-27 | 2015-04-15 | 山东金诃药物研究开发有限公司 | Quality testing method for Liuwei Mingmu preparation of Tibetan medicine composition |
| CN106198789A (en) * | 2016-06-24 | 2016-12-07 | 中国人民解放军第三〇七医院 | Cowherb red tablet quality control method |
| CN110988159A (en) * | 2019-11-25 | 2020-04-10 | 通化卫京药业股份有限公司 | Method for measuring contents of multiple components of Jingyaokang capsule |
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| CN102662026B (en) | 2014-04-30 |
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