CN102662026B - 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 detection method of Chinese medicine preparation, particularly the detection method of Lenin's preparation before a kind of Chinese medicine.
Background technology
Prostatitis Yiganning capsule is the exclusive product of Jin He Tibetan medicine incorporated company, records in Chinese patent drug provincial standard rising national standard part, standard number: WS-10627 (ZD-0627)-2002-2011Z.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 being made by the medicinal material of following weight proportion.Above 13 tastes, are ground into fine powder, sieve, and mix, and incapsulate, and make 1000.Have clearing heat and detoxicating, the effect of Huayu Tonglin.For the caused frequent micturition of hot malicious stasis blocking, urgent urination, odynuria belongs to traditional Chinese medical science stranguria person.
The existing quality standard about front Lenin's medicine only adopts TLC thin layer to differentiate the content of medicinal material shellac, an effective component gallic acid of HPLC mensuration simply, in prior art, also not yet find other quality determining methods for prostatitis Yiganning capsule, therefore existing quality determining method can not be controlled this product quality comprehensively and accurately, and quality standard has much room for improvement.
Summary of the invention
For the deficiencies in the prior art, the object of this invention is to provide the detection 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 identification method that detects myrobalan in Chinese medicine prostatitis Yiganning capsule and preparation thereof, safflower, Semen thlaspis, ZANGQIANCAO; Adopt high performance liquid chromatography; by changing the detection wavelength of UV-detector; thereby reach under same chromatographic condition, the content of gallic acid and hydroxyl radical carthamin yellow carthamus A is measured simultaneously; having strengthened on the basis of product controllability, saved analysis time, improved work efficiency; use gradient elution simultaneously; protect chromatographic column, extended the serviceable life of chromatographic column, reduced cost.
Term explanation:
Prostatitis Yiganning capsule is the nomenclature of drug that national standard for traditional Chinese medicines compilation (Chinese patent drug provincial standard rising national standard part) is recorded, standard number WS-10627 (ZD-0627)-2002-2011Z.
Other preparations that front Lenin's preparation comprises prostatitis Yiganning capsule and prepares with prostatitis Yiganning capsule bulk drug formula.
Technical scheme of the present invention is as follows:
Bulk drug consists of a detection method for the front Lenin's preparation of Chinese medicine 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 weight portions, and the method comprises one or more in following discriminating and/or content assaying method:
Differentiate:
A, myrobalan's discriminating
Get the front Lenin's preparation 3-10g of Chinese medicine, add absolute ethyl alcohol 25-50ml, ultrasonic processing 20-30min, adds zeyssatite 1-3g, mixes, and filters, and filtrate is concentrated into 2ml, as need testing solution, separately get myrobalan's control medicinal material 1-2g, add absolute ethyl alcohol 25-50ml, ultrasonic processing 20-30min, adds zeyssatite 1-3g, mixes, and filters, and filtrate is concentrated into 2ml, in contrast medicinal material solution, separately get gallic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast, according to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5-10 μ of above-mentioned solution l, put respectively on same silica gel g thin-layer plate, methenyl choloride-ethyl acetate-formic acid take volume parts ratio as 3-9:2-6:0.5-1.5 is as developping agent, launch, take out, dry, spray is take quality volume portion rate as 1% ferric trichloride ethanolic solution, be heated to spot colour developing clear, in test sample chromatogram, with reference substance and the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color,
The discriminating of B, safflower
Get the front Lenin's preparation 3-10g of Chinese medicine, adding volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, and jolting 10-20min, standing, get supernatant, as need testing solution; Separately get safflower control medicinal material 1g, adding volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, and jolting 10-20min, standing, get supernatant, in contrast medicinal material solution; According to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5-10 μ of above-mentioned solution l, put respectively on same silica gel g thin-layer plate, ethyl acetate-formic acid-water-methanol take volume parts ratio as 5-9:1-3:2-4:0.2-0.6 is as developping agent, launch, take out, dry, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color;
The discriminating of C, Semen thlaspis
Get the front Lenin's preparation 3-10g of Chinese medicine, adding volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, and jolting 10-20min, standing, get supernatant, as need testing solution, another Qu Semen thlaspis control medicinal material 1g, adding volume parts ratio is 80% acetone methanol solution 25-50ml, close plug, jolting 10-20min, standing, get supernatant, in contrast medicinal material solution, according to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5-10 μ of above-mentioned solution l, put respectively on same silica gel g thin-layer plate, upper solution take volume parts ratio as normal butyl alcohol-glacial acetic acid-water mixed solution of 2-6:0.5-1.5:3-7 is as developping agent, launch, take out, dry, spray is take volume parts ratio as 10% ethanol solution of sulfuric acid, 100-105 ℃ to be heated to spot colour developing clear, put under uviol lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
The discriminating of D, ZANGQIANCAO
Get the front Lenin's preparation 3-10g of Chinese medicine, add methyl alcohol 25-50ml, ultrasonic processing 20-30min, filters, and filtrate is concentrated into 1ml, as need testing solution; Separately get ZANGQIANCAO control medicinal material 1-2g, add methyl alcohol 25-50ml, ultrasonic processing 20-30min, filters, and filtrate is concentrated into 1ml, as need testing solution; According to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw respectively the each 5-10 μ of above-mentioned solution l, point is on same silica gel g thin-layer plate, sherwood oil-acetone take volume parts ratio as 2-6:0.5-1.5 is as developping agent, sherwood oil boiling range is 60～90 ℃, launch, take out, dry, put under uviol lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
Assay:
According to high performance liquid chromatography (appendix VI D of Chinese Pharmacopoeia version in 2010)
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile as mobile phase A, take volume parts than 1% glacial acetic acid aqueous solution as Mobile phase B, adopt gradient elution mode:
0min → 20min → 25min → 50min → 55min → 60min, according to the above-mentioned time period, acetonitrile, volume parts are carried out wash-out than 1% glacial acetic acid aqueous solution simultaneously, wherein, acetonitrile: 1% → 1% → 24% → 24% → 100% → 1%; Volume parts is than 1% glacial acetic acid aqueous solution: 99% → 99% → 76% → 76% → 0% → 99%, within 0min → 20min time, use the detection wavelength of 275nm, it is 403nm that 20min changes detection wavelength, and 21min makes detecting device balance, uses the detection wavelength of 403nm in 21min → 60min time.Number of theoretical plate calculates and should be not less than 2000 by gallic acid peak;
The preparation of reference substance solution: get gallic acid reference substance, hydroxyl radical carthamin yellow carthamus A reference substance is appropriate, accurately weighed, add volume parts and make respectively the solution of every 1ml containing gallic acid 20 μ g, hydroxyl radical carthamin yellow carthamus A 0.2mg than 40-60% ethanol water, obtain;
The preparation of need testing solution: get the front Lenin's preparation powder 3g of Chinese medicine, cross sieve No. three, accurately weighed, put in tool plug conical flask, precision adds volume parts than 40-60% ethanol water 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, weighed weight again, the weight of supplying less loss by volume parts than 40-60% ethanol water, shakes up, and filters, get subsequent filtrate, obtain;
Determination method: accurate reference substance solution and the each 5-10 μ of the need testing solution l of drawing respectively, injection liquid chromatography, measures, and obtains.
Described front Lenin's preparation refers to by prostatitis Yiganning capsule bulk drug formula 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 dry lower than 60 ℃, mix, micronizer is ground into 0.1-50 μ m Ultramicro-powder, technique routinely, add conventional auxiliary material to be prepared into clinical acceptable any formulation, comprise capsule, pill, micropill, dripping pill, tablet, soft capsule, particle or oral liquid.
Preferably, bulk drug consists of a detection method for the Chinese medicine prostatitis Yiganning capsule 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 weight portions, and the method comprises one or more in following discriminating and/or content assaying method:
Differentiate:
A, myrobalan's discriminating
Get Chinese medicine prostatitis Yiganning capsule content 5g, add absolute ethyl alcohol 25ml, ultrasonic processing 30min, adds zeyssatite 2g, mixes, and filters, and filtrate is concentrated into 2ml, as need testing solution, separately get myrobalan's control medicinal material 1g, add absolute ethyl alcohol 25ml, ultrasonic processing 30min, adds zeyssatite 2g, mixes, and filters, and filtrate is concentrated into 2ml, in contrast medicinal material solution, separately get gallic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast, according to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, methenyl choloride-ethyl acetate-formic acid take volume parts ratio as 6:4:1 is as developping agent, launch, take out, dry, spray is take quality volume portion rate as 1% ferric trichloride ethanolic solution, be heated to spot colour developing clear, in test sample chromatogram, with reference substance and the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color,
The discriminating of B, safflower
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding volume parts ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min, standing, get supernatant, as need testing solution; Separately get safflower control medicinal material 1g, adding volume ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min, standing, get supernatant, in contrast medicinal material solution; According to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, ethyl acetate-formic acid-water-methanol take volume parts ratio as 7:2:3:0.4, as developping agent, launches, and takes out, dry, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color;
The discriminating of C, Semen thlaspis
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding volume parts ratio is 80% acetone soln 30ml, close plug, and jolting 15min, standing, get supernatant, as need testing solution, another Qu Semen thlaspis control medicinal material 1g, adding volume ratio is 80% acetone soln 30ml, close plug, jolting 15min, standing, get supernatant, in contrast medicinal material solution, according to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, the upper solution of the normal butyl alcohol-glacial acetic acid-water mixed solution take volume ratio as 4:1:5 is developping agent, launch, take out, dry, spray is take volume parts ratio as 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to spot colour developing clear, put under uviol lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
The discriminating of D, ZANGQIANCAO
Get Chinese medicine prostatitis Yiganning capsule content 5g, add methyl alcohol 30ml, ultrasonic processing 30min, filters, and filtrate is concentrated into 1ml, as need testing solution; Separately get ZANGQIANCAO control medicinal material 1g, add methyl alcohol 30ml, ultrasonic processing 30min, filters, and filtrate is concentrated into 1ml, as need testing solution; According to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw respectively the each 10 μ l of above-mentioned solution, point is on same silica gel g thin-layer plate, sherwood oil-acetone take volume parts ratio as 4:1 is as developping agent, sherwood oil boiling range is 60～90 ℃, launch, take out, dry, put under uviol lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
Assay:
According to high performance liquid chromatography (appendix VI D of Chinese Pharmacopoeia version in 2010)
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile as mobile phase A, take volume parts than 1% glacial acetic acid aqueous solution as Mobile phase B, adopt gradient elution mode:
0min → 20min → 25min → 50min → 55min → 60min, according to the above-mentioned time period, acetonitrile, volume parts are carried out wash-out than 1% glacial acetic acid aqueous solution simultaneously, wherein, acetonitrile: 1% → 1% → 24% → 24% → 100% → 1%; Volume parts is than 1% glacial acetic acid aqueous solution: 99% → 99% → 76% → 76% → 0% → 99%, within 0min → 20min time, use the detection wavelength of 275nm, it is 403nm that 20min changes detection wavelength, and 21min makes detecting device balance, uses the detection wavelength of 403nm in 21min → 60min time.Number of theoretical plate calculates and should be not less than 2000 by gallic acid peak;
The preparation of reference substance solution: get gallic acid reference substance, hydroxyl radical carthamin yellow carthamus A reference substance is appropriate, accurately weighed, add volume parts and make respectively the solution containing gallic acid 20 μ g, hydroxyl radical carthamin yellow carthamus A 0.2mg in every 1ml than 50% ethanol water, obtain;
The preparation of need testing solution: get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, accurately weighed, put in tool plug conical flask, precision adds volume parts than 50% ethanol water 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, weighed weight again, the weight of supplying less loss by volume parts than 50% ethanol water, shakes up, and filters, get subsequent filtrate, obtain;
Determination method: accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and obtains;
In the Yiganning capsule of Chinese medicine of the present invention prostatitis, myrobalan's content, in gallic acid (C7H6O5), must not be less than 2.0mg/g; Safflower content, in hydroxyl radical carthamin yellow carthamus A (C27H30O15), must not be less than 0.26mg/g.
The unit corresponding relation of the 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 as follows:
The existing quality standard about front Lenin's medicine only adopts TLC thin layer to differentiate the content of medicinal material shellac, an effective component gallic acid of HPLC mensuration simply, causes the quality testing of front Lenin's formulation products 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 multiple compositions, as adopted high performance liquid chromatography, by changing the detection wavelength of UV-detector, thereby reaches under same chromatographic condition the assay to gallic acid and hydroxyl radical carthamin yellow carthamus A simultaneously.Result shows that method is simple and feasible, has good accuracy and precision, can effectively guarantee this product quality.
Following experimental example and embodiment are used for further illustrating 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 Qinghai gold and is provided.
A, myrobalan's discriminating
Get Chinese medicine prostatitis Yiganning capsule content 5g, add absolute ethyl alcohol 25ml, ultrasonic processing 30min, adds zeyssatite 2g, mixes, and filters, and filtrate is concentrated into 2ml, as need testing solution, separately get myrobalan's control medicinal material 1g, add absolute ethyl alcohol 25ml, ultrasonic processing 30min, adds zeyssatite 2g, mixes, and filters, and filtrate is concentrated into 2ml, in contrast medicinal material solution, separately get gallic acid reference substance, add methyl alcohol and make the solution in contrast solution of every 1ml containing 1mg, according to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, take methenyl choloride-ethyl acetate-formic acid as developping agent, developping agent volume parts is than getting respectively (6:4:1) in the scope for 3-9:2-6:0.5-1.5, (5:5:0.8), (7:5:0.6) methenyl choloride-ethyl acetate-formic acid is developping agent, launch, take out, dry, spray is take quality volume portion rate as 1% ferric trichloride ethanolic solution, be heated to spot colour developing clear, in test sample chromatogram, with reference substance and the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.
Interpretation of result: than being under methenyl choloride-ethyl acetate-formic acid developping agent condition of 3-9:2-6:0.5-1.5, have good expansion effect in volume parts.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 volume parts ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min, standing, get supernatant, as need testing solution, separately get safflower control medicinal material 1g, adding volume ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min, standing, get supernatant, in contrast medicinal material solution, according to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, take ethyl acetate-formic acid-water-methanol as developping agent, developping agent volume parts is than getting respectively (7:2:3:0.4) in the scope for 5-9:1-3:2-4:0.2-0.6, (6:2:4:0.5), (9:1:4:0.2) ethyl acetate-formic acid-water-methanol is developping agent, launch, take out, dry, in test sample chromatogram, with reference substance and the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.
Interpretation of result: than being under ethyl acetate-formic acid-water-methanol developping agent condition of 3-9:2-6:0.5-1.5, have good expansion effect in volume parts.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 volume parts ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min, standing, get supernatant, as need testing solution, another Qu Semen thlaspis control medicinal material 1g, adding volume parts ratio is 80% water acetone soln 30ml, close plug, jolting 15min, standing, get supernatant, in contrast medicinal material solution, according to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, take the upper solution of normal butyl alcohol-glacial acetic acid-water mixed solution as developping agent, developping agent volume parts is than getting respectively (4:1:5) in the scope for 2-6:0.5-1.5:3-7, (5:1.2:3), (2:0.6:6) upper solution of normal butyl alcohol-glacial acetic acid-water mixed solution is developping agent, launch, take out, dry, spray is take quality volume portion rate as 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to spot colour developing clear, put under uviol lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
Interpretation of result: than being under the upper solution developping agent condition of normal butyl alcohol-glacial acetic acid-water mixed solution of 2-6:0.5-1.5:3-7, have good expansion effect in volume parts.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, ultrasonic processing 30min, filters, and filtrate is concentrated into 1ml, as need testing solution, separately get ZANGQIANCAO control medicinal material 1g, add methyl alcohol 30ml, ultrasonic processing 30min, filters, and filtrate is concentrated into 1ml, as need testing solution, according to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw respectively the each 10 μ l of above-mentioned solution, point is on same silica gel g thin-layer plate, take sherwood oil-acetone as developping agent, sherwood oil boiling range is 60～90 ℃, developping agent volume parts is than getting respectively (4:1) in the scope for 2-6:0.5-1.5, (5:0.5), (2:1.5) sherwood oil-acetone is developping agent, launch, take out, dry, put under uviol lamp 365nm and inspect.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious identical face.
Interpretation of result: than being under sherwood oil-acetone developping agent condition of 2-6:0.5-1.5, have good expansion effect in volume parts.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 test sample
Instrument: the L-2100 of Hitachi pump, the L-2400 of Hitachi UV-detector, Shimadzu 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 (Qinghai gold is scolded Tibetan medicine medicine company incorporated company and provided), lot number: 20110216,20110217,20110218.
2, detect the selection of wavelength
Get respectively gallic acid, hydroxyl radical carthamin yellow carthamus A reference substance solution, in 200～500nm wavelength coverage, carry out UV scanning.According to ultraviolet absorpting spectrum, the detection wavelength that selected 275nm is gallic acid, the detection wavelength that selected 403nm is hydroxyl radical carthamin yellow carthamus A.Detect wavelength variations in Table 1.
Table 1 detects wavelength variations table
3, mobile phase is selected
Gallic acid and hydroxyl radical carthamin yellow carthamus A polarity differ larger, adopt isocratic elution to be difficult to two kinds of compositions to carry out wash-out simultaneously, therefore select gradient elution to carry out chromatographic resolution.
Discovery while using methanol-water, acetonitrile-water system to carry out chromatographic resolution, peak hangover is serious.Water adds after acid, and peak shape is greatly improved.Experimental result shows, while using acetonitrile-volume parts to carry out gradient elution than 1% glacial acetic acid aqueous solution for mobile phase, gallic acid and hydroxyl radical carthamin yellow carthamus A all can reach good separating effect.Therefore determine that mobile phase A is 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 volume parts ratio, and gallic acid peak retention time and degree of separation are all suitable; Acetonitrile-volume parts is 20～30:80～70 o'clock than 1% glacial acetic acid aqueous solution at volume parts ratio, and hydroxyl radical carthamin yellow carthamus A starts wash-out, and peak retention time and degree of separation are all suitable.By research, find, while 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, meets testing requirement.See accompanying drawing 1 and accompanying drawing 2.
Table 2 eluent gradient table
5, the preparation of reference substance solution
Get gallic acid reference substance, hydroxyl radical carthamin yellow carthamus A reference substance is appropriate, accurately weighed, adds volume parts and makes every 1ml containing the mixed solution of gallic acid 0.2mg, hydroxyl radical carthamin yellow carthamus A 10 μ g than 50% ethanolic solution, obtain.
6, test sample preparation
6.1 extracting method are selected
Get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, accurately weighed, put in tool plug conical flask, precision adds volume parts than 50% ethanol water 50ml, close plug, weighed weight, ultrasonic, backflow, Zhen Oscillating processes 30min respectively, lets cool, weighed weight again, the weight of supplying less loss by volume parts than 50% ethanol water, shakes up, and filters, get subsequent filtrate, obtain.The results are shown in Table 3.
Table 3 extracting method is investigated test findings
| Extracting method | Ultrasonic | Reflux | Jolting |
| Gallic acid content (mg/ grain) | 0.911 | 0.815 | 0.658 |
| Sydroxy carthamin content (mg/ grain) | 0.0799 | 0.0586 | 0.0419 |
Result shows, gallic acid, hydroxyl radical carthamin yellow carthamus A content that ultrasonic extraction is measured are the highest, therefore determine that extracting method is ultrasonic extraction.
6.2 extract solvent selects
Get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, accurately weighed, put in tool plug conical flask, precision adds volume parts than 40%, 50%, 60% ethanol water 50ml, close plug respectively, weighed weight, ultrasonic processing 30min, lets cool, weighed weight again, the weight of supplying respectively less loss by volume parts than 40%, 50%, 60% ethanol water, shakes up, and filters, get subsequent filtrate, obtain.The results are shown in Table 4.
Table 4 extracts solvent and investigates test findings
Result shows, gallic acid, hydroxyl radical carthamin yellow carthamus A content that volume parts is surveyed than 50% ethanol water are higher, thus select volume parts than 50% ethanol water the extraction solvent as test sample.
6.3 extraction times were selected
Get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, accurately weighed, put in tool plug conical flask, precision adds volume parts than 50% ethanol water 50ml, close plug, weighed weight, respectively ultrasonic processing 20,30,40min, let cool, weighed weight again, the weight of supplying less loss by volume parts than 50% ethanol water, shakes up, and filters, get subsequent filtrate, obtain.The results are shown in Table 5.
Table 5 extraction time is investigated 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 |
Result shows, gallic acid, hydroxyl radical carthamin yellow carthamus A substantially extract completely when extraction time is 20min, in order to guarantee that test sample extracts that to select 30min be completely extraction time.
7, the preparation of typical curve and the investigation of linear relationship
Precision measures 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 10ml volumetric flask, volume parts is diluted to scale than 50% ethanol water, shake up, each accurate sample introduction 10 μ l, take peak area (A) as ordinate, reference substance concentration (C) is horizontal ordinate, carries out linear regression.In Table 6, table 7 and accompanying drawing 3 and accompanying drawing 4.
Table 6 gallic acid linear relationship is investigated result
Regression equation: A=15682C-16290
Related coefficient: R=0.9996
Table 7 hydroxyl radical carthamin yellow carthamus A linear relationship is investigated result
Regression equation: A=11344C-3478.5
Related coefficient: R=0.9998
Result shows: gallic acid is within the scope of 33.76 μ g/ml～337.60 μ g/ml, and linear relationship is good; Hydroxyl radical carthamin yellow carthamus A is within the scope of 2.68～26.80 μ g/ml, 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, injection liquid chromatography, METHOD FOR CONTINUOUS DETERMINATION 6 times, records peak area and calculates relative standard deviation.Result shows: instrument precision is good.In 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 prepared by need testing solution, the accurate 10 μ l that draw, injection liquid chromatography, records peak area, measures once every 2 hours later, investigates 8 hours, calculates the relative standard deviation of peak area.Result shows: in need testing solution 8 hours, measurement result is stable.In 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 batch sample, replication 6 times, gallic acid, hydroxyl radical carthamin yellow carthamus A content in calculation sample.Result shows, analytical approach repeatability is good.In 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 6 parts of same batch samples, and precision adds gallic acid, hydroxyl radical carthamin yellow carthamus A reference substance, measures its content, calculate recovery rate.Result shows, this assay method measurement result is accurate.In 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, measure and calculate gallic acid, hydroxyl radical carthamin yellow carthamus A content, and result is as following table 16.
Table 16 sample size measurement result
| Lot number | Gallic acid (mg/ grain) | Hydroxyl radical carthamin yellow carthamus A (mg/ grain) |
| 20110216 | 0.917 | 0.0776 |
| 20110217 | 0.926 | 0.0757 |
| 20110218 | 0.908 | 0.0769 |
Following embodiment all can realize the effect described in above-mentioned experimental example.
Accompanying drawing explanation:
Fig. 1 is that gallic acid, hydroxyl radical carthamin yellow carthamus A mix contrast high-efficient liquid phase chromatogram;
Fig. 2 is medicine prostatitis Yiganning capsule high-efficient liquid phase chromatogram;
Fig. 3 is gallic acid linear relationship chart;
Fig. 4 is 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 voltage, unit: volt (Volts).
Embodiment
Below in conjunction with embodiment, the present invention is done to detailed elaboration, but be not limited to these concrete embodiment recording.The prostatitis Yiganning capsule detecting be Qinghai gold scold Tibetan medicine medicine company incorporated company produce sell.
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, ultrasonic processing 30min, adds zeyssatite 2g, mixes, and filters, and filtrate is concentrated into 2ml, as need testing solution, separately get myrobalan's control medicinal material 1g, add absolute ethyl alcohol 25ml, ultrasonic processing 30min, adds zeyssatite 2g, mixes, and filters, and filtrate is concentrated into 2ml, in contrast medicinal material solution, separately get gallic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast, according to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, methenyl choloride-ethyl acetate-formic acid take volume parts ratio as 6:4:1 is as developping agent, launch, take out, dry, spray is take quality volume portion rate as 1% ferric trichloride ethanolic solution, be heated to spot colour developing clear, in test sample chromatogram, with reference substance and the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color,
The discriminating of B, safflower
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding volume parts ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min, standing, get supernatant, as need testing solution; Separately get safflower control medicinal material 1g, adding volume ratio is 80% acetone methanol solution 30ml, close plug, and jolting 15min, standing, get supernatant, in contrast medicinal material solution; According to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, ethyl acetate-formic acid-water-methanol take volume parts ratio as 7:2:3:0.4, as developping agent, launches, and takes out, dry, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color;
The discriminating of C, Semen thlaspis
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding volume parts ratio is 80% acetone soln 30ml, close plug, and jolting 15min, standing, get supernatant, as need testing solution, another Qu Semen thlaspis control medicinal material 1g, adding volume ratio is 80% acetone soln 30ml, close plug, jolting 15min, standing, get supernatant, in contrast medicinal material solution, according to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw the each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, the upper solution of the normal butyl alcohol-glacial acetic acid-water mixed solution take volume ratio as 4:1:5 is developping agent, launch, take out, dry, spray is take volume parts ratio as 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to spot colour developing clear, put under uviol lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
The discriminating of D, ZANGQIANCAO
Get Chinese medicine prostatitis Yiganning capsule content 5g, add methyl alcohol 30ml, ultrasonic processing 30min, filters, and filtrate is concentrated into 1ml, as need testing solution; Separately get ZANGQIANCAO control medicinal material 1g, add methyl alcohol 30ml, ultrasonic processing 30min, filters, and filtrate is concentrated into 1ml, as need testing solution; According to thin-layered chromatography (appendix VI B of < < Pharmacopoeia of People's Republic of China > > version in 2010), test, draw respectively the each 10 μ l of above-mentioned solution, point is on same silica gel g thin-layer plate, sherwood oil-acetone take volume parts ratio as 4:1 is as developping agent, sherwood oil boiling range is 60～90 ℃, launch, take out, dry, put under uviol lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
Embodiment 2: the content assaying method of Chinese medicine prostatitis Yiganning capsule
According to high performance liquid chromatography (appendix VI D of Chinese Pharmacopoeia version in 2010)
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile as mobile phase A, take volume parts than 1% glacial acetic acid aqueous solution as Mobile phase B, adopt gradient elution mode:
0min → 20min → 25min → 50min → 55min → 60min, according to the above-mentioned time period, acetonitrile, volume parts are carried out wash-out than 1% glacial acetic acid aqueous solution simultaneously, wherein, acetonitrile: 1% → 1% → 24% → 24% → 100% → 1%; Volume parts is than 1% glacial acetic acid aqueous solution: 99% → 99% → 76% → 76% → 0% → 99%, within 0min → 20min time, use the detection wavelength of 275nm, it is 403nm that 20min changes detection wavelength, and 21min makes detecting device balance, uses the detection wavelength of 403nm in 21min → 60min time.Number of theoretical plate calculates and should be not less than 2000 by gallic acid peak;
The preparation of reference substance solution: get gallic acid reference substance, hydroxyl radical carthamin yellow carthamus A reference substance is appropriate, accurately weighed, add volume parts and make respectively the solution of every 1ml containing gallic acid 20 μ g, hydroxyl radical carthamin yellow carthamus A 0.2mg than 50% ethanol water, obtain.
The preparation of need testing solution: get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, accurately weighed, put in tool plug conical flask, precision adds volume parts than 50% ethanol water 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, weighed weight again, the weight of supplying less loss by volume parts than 50% ethanol water, shakes up, and filters, get subsequent filtrate, obtain;
Determination method: accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and obtains;
In the front Lenin's preparation of Chinese medicine of the present invention, myrobalan's content is with gallic acid (C
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. the detection method of Lenin's preparation before a Chinese medicine, the bulk drug of preparation consists 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 weight portions, it is characterized in that, the method comprises one or both in following discriminating and/or content assaying method:
The discriminating of Semen thlaspis:
Get the front Lenin's preparation 3-10g of Chinese medicine, adding volume parts ratio is 80% acetone methanol solution 25-50mL, close plug, and jolting 10-20min, standing, get supernatant, as need testing solution, another Qu Semen thlaspis control medicinal material 1g, adding volume parts ratio is 80% acetone methanol solution 25-50mL, close plug, jolting 10-20min, standing, get supernatant, in contrast medicinal material solution, according to appendix VI B test of thin-layered chromatography < < Pharmacopoeia of People's Republic of China > > version in 2010, draw the each 5-10 μ of above-mentioned solution l, put respectively on same silica gel g thin-layer plate, upper solution take volume parts ratio as normal butyl alcohol-glacial acetic acid-water mixed solution of 2-6:0.5-1.5:3-7 is as developping agent, launch, take out, dry, spray is take volume parts ratio as 10% ethanol solution of sulfuric acid, 100-105 ℃ to be heated to spot colour developing clear, put under uviol lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
Assay:
According to appendix VI D of high performance liquid chromatography Chinese Pharmacopoeia version in 2010;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile as mobile phase A, take volume parts than 1% glacial acetic acid aqueous solution as Mobile phase B, adopt gradient elution mode:
0min → 20min → 25min → 50min → 55min → 60min, according to the above-mentioned time period, acetonitrile, volume parts are carried out wash-out than 1% glacial acetic acid aqueous solution simultaneously, wherein, acetonitrile: 1% → 1% → 24% → 24% → 100% → 1%; Volume parts is than 1% glacial acetic acid aqueous solution: 99% → 99% → 76% → 76% → 0% → 99%, within 0min → 20min time, use the detection wavelength of 275nm, it is 403nm that 20min changes detection wavelength, and 21min makes detecting device balance, uses the detection wavelength of 403nm in 21min → 60min time; Number of theoretical plate calculates and should be not less than 2000 by gallic acid peak;
The preparation of reference substance solution: get gallic acid reference substance, hydroxyl radical carthamin yellow carthamus A reference substance is appropriate, accurately weighed, add volume parts and make respectively the solution of every 1mL containing gallic acid 20 μ g, hydroxyl radical carthamin yellow carthamus A 0.2mg than 40-60% ethanol water, obtain;
The preparation of need testing solution: get the front Lenin's preparation powder 3g of Chinese medicine, cross sieve No. three, accurately weighed, put in tool plug conical flask, precision adds volume parts than 40-60% ethanol water 50mL, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, weighed weight again, the weight of supplying less loss by volume parts than 40-60% ethanol water, shakes up, and filters, get subsequent filtrate, obtain;
Determination method: accurate reference substance solution and the each 5-10 μ of the need testing solution l of drawing respectively, injection liquid chromatography, measures, and obtains.
2. the detection method of Lenin's preparation before a kind of Chinese medicine as claimed in claim 1, it is characterized in that described front Lenin's preparation refers to by prostatitis Yiganning capsule bulk drug formula 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 dry lower than 60 ℃, mix, micronizer is ground into 0.1-50 μ m Ultramicro-powder, technique routinely, add conventional auxiliary material to be prepared into clinical acceptable any formulation, comprise capsule, pill, micropill, dripping pill, tablet, soft capsule, particle or oral liquid.
3. the detection method of Lenin's preparation before a kind of Chinese medicine as claimed in claim 1, is characterized in that the method comprises one or both in following discriminating and/or content assaying method:
The discriminating of Semen thlaspis:
Get Chinese medicine prostatitis Yiganning capsule content 5g, adding volume parts ratio is 80% acetone soln 30mL, close plug, and jolting 15min, standing, get supernatant, as need testing solution, another Qu Semen thlaspis control medicinal material 1g, adding volume ratio is 80% acetone soln 30mL, close plug, jolting 15min, standing, get supernatant, in contrast medicinal material solution, according to appendix VI B test of thin-layered chromatography < < Pharmacopoeia of People's Republic of China > > version in 2010, draw the each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, the upper solution of the normal butyl alcohol-glacial acetic acid-water mixed solution take volume ratio as 4:1:5 is developping agent, launch, take out, dry, spray is take volume parts ratio as 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to spot colour developing clear, put under uviol lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color,
Assay:
According to appendix VI D of high performance liquid chromatography Chinese Pharmacopoeia version in 2010;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile as mobile phase A, take volume parts than 1% glacial acetic acid aqueous solution as Mobile phase B, adopt gradient elution mode:
0min → 20min → 25min → 50min → 55min → 60min, according to the above-mentioned time period, acetonitrile, volume parts are carried out wash-out than 1% glacial acetic acid aqueous solution simultaneously, wherein, acetonitrile: 1% → 1% → 24% → 24% → 100% → 1%; Volume parts is than 1% glacial acetic acid aqueous solution: 99% → 99% → 76% → 76% → 0% → 99%, within 0min → 20min time, use the detection wavelength of 275nm, it is 403nm that 20min changes detection wavelength, and 21min makes detecting device balance, uses the detection wavelength of 403nm in 21min → 60min time; Number of theoretical plate calculates and should be not less than 2000 by gallic acid peak;
The preparation of reference substance solution: get gallic acid reference substance, hydroxyl radical carthamin yellow carthamus A reference substance is appropriate, accurately weighed, add volume parts and make respectively the solution of every 1mL containing gallic acid 20 μ g, hydroxyl radical carthamin yellow carthamus A 0.2mg than 50% ethanol water, obtain;
The preparation of need testing solution: get Chinese medicine prostatitis Yiganning capsule content powder 3g, cross sieve No. three, accurately weighed, put in tool plug conical flask, precision adds volume parts than 50% ethanol water 50mL, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, weighed weight again, the weight of supplying less loss by volume parts than 50% ethanol water, shakes up, and filters, get subsequent filtrate, obtain;
Determination method: accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and obtains.
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| 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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