CN101810752B - Method for detecting quality of Chinese medicament for treating prostatitis - Google Patents
Method for detecting quality of Chinese medicament for treating prostatitis Download PDFInfo
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Abstract
The invention discloses a method for detecting a Chinese medicament for treating prostatitis. The method comprises the following steps of: identifying, inspecting the medicament for treating the prostatitis; and detecting extractum and content thereof. The method accurately detects the content of gardenoside by high performance liquid chromatography; the gardenia content of each tablet is based on the content of the geniposide (C17H24O10) and is no less than 3 mg/tablet. The method realizes accurate detection of the content of the gardenoside by the high performance liquid chromatography. The method has simple, accurate and advanced operation, and good linear relation, reproducibility, accuracy, stability and recovery rate and can more effectively control the quality of products.
Description
Technical field
The invention belongs to medicine quality detection technique field, relate to a kind of quality determining method of Chinese medicine, be specifically related to the prostatitic Chinese medicine detection method of a kind of treatment.
Background technology
Hyperplasia of prostate is a kind of common disease, the frequently-occurring disease of elderly men, and the incidence of disease increases with age growth gradually.It mainly shows: frequent micturition, dysuria, acute renal shutdown or the urinary incontinence; Severe patient must perhaps be performed the operation in urethral catheterization; Prostatitis also is urological department male sex common disease, frequently-occurring disease, mainly shows as urgent urination, frequent micturition, odynuria, perineum pain, and patient health has been caused great injury.
In the prior art; Application number is 200810167505.1; Name is called the patent of " prostatitic Chinese medicine preparation of a kind of treatment and preparation method thereof "; A kind of prostatitic Chinese medicine that is used to treat is disclosed, its be by mulberry fruit, Gorgon fruit, dioscoreae septemlobae,rhizoma, Cherokee rose, cape jasmine etc. through the active constituents of medicine be processed into and medicine acceptable carrier by the capsule of certain proportioning through being processed into.
And the present invention is compositions such as mulberry fruit, Gorgon fruit, dioscoreae septemlobae,rhizoma, Cherokee rose, cape jasmine, and through extraction, preparation production and processing gained Chinese medicine Film coated tablets, this Chinese medicine has evident in efficacy.Characteristics such as have no side effect.This product has the enhancing body trophicity, takes the photograph power and drainage power, the effect of pure and impure diuresis.Be quantitative target with the Gardenoside in the standard.Mostly method about the assay of Gardenoside is high performance liquid chromatography, high performance liquid chromatography have sensitivity, accurately, characteristics such as favorable reproducibility; So with reference to interrelated data, select content, as the content assaying method of control said preparation quality with Gardenoside in the high effective liquid chromatography for measuring said preparation.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of treatment prostatitic Chinese medicine detection method to above-mentioned deficiency of the prior art.
For solving the problems of the technologies described above; The technical scheme that the present invention adopts is: the prostatitic Chinese medicine detection method of a kind of treatment; Diligent those the sub-sheets of treatment prostatitis medicine-Xi Payimai are processed by following medicinal materials in part by weight: 300～600 parts in mulberry fruit, 300～600 parts of Gorgon fruits, 200～400 parts of dioscoreae septemlobae,rhizomas; 200～500 parts of the fruits of Cherokee rose, 200～400 parts on mast;
The preparation method of treatment prostatitis medicine-Xi Payimai diligent those sub-sheets: with mulberry fruit, Gorgon fruit, the fruit of Cherokee rose and the boiling of mast four traditional Chinese medicine material 3 times; Respectively decocted for first and second times 2 hours, and decocted collecting decoction for the third time 1 hour; Leave standstill; Filter, it is 1: 1 volume that filtrating is concentrated into the crude drug volume ratio, subsequent use; Dioscoreae septemlobae,rhizoma is ground into meal, adds alcohol reflux 3 times, each 1 hour, filter, merging filtrate merges with above-mentioned reserve liquid; Adding ethanol is 70% to containing pure quality, leaves standstill 24 hours, filter, and filtrate recycling ethanol, being concentrated into 55～60 ℃ of heat survey relative densities is 1.20～1.25, drying under reduced pressure; Pulverize, add appropriate amount of starch and carboxyrnethyl starch sodium, mixing is granulated drying; Add dolomol, mixing, compacting is wrapped film-coating in flakes, promptly gets;
It is characterized in that this Chinese medicine detection method may further comprise the steps:
(1) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize adds water 30～50ml; Sonicated 10～20 minutes is put coldly, filters; The normal butyl alcohol jolting that filtrate water is saturated is extracted 2 times, and each 10～20ml merges normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1ml dissolving, process need testing solution; Other gets mulberry fruit control medicinal material 5g, adds mass concentration and be 60% ethanolic solution 30ml, reflux 1 hour; Filter, filtrating is concentrated into does not have the alcohol flavor, extracts 2 times with water saturated normal butyl alcohol jolting; Each 10～20ml merges normal butyl alcohol liquid, evaporate to dryness; Residue adds methyl alcohol 1ml dissolving, processes mulberry fruit control medicinal material solution; According to thin-layered chromatography test, draw respectively 5 μ l of need testing solution and mulberry fruit control medicinal material solution, put respectively on same silica gel g thin-layer plate, be that the upper solution of 15: 1: 4 ethyl acetate, glacial acetic acid and water is a developping agent with percent by volume; Launch, take out, dry; Put under the 365nm ultraviolet lamp and inspect, in the test sample chromatogram, with the corresponding position of mulberry fruit control medicinal material chromatogram on; Show identical blue-fluorescence spot, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of mulberry fruit control medicinal material chromatogram on, show the spot of same color;
(2) get cape jasmine control medicinal material 5g, add mass concentration and be 70% ethanol 30ml, refluxing extraction 1 hour filters, and evaporate to dryness in the filtrating water-bath, residue add methyl alcohol 1ml dissolving, process cape jasmine control medicinal material solution; Other gets the Gardenoside reference substance, adds methyl alcohol and processes the solution that every 1ml contains the 2mg Gardenoside, as the Gardenoside reference substance solution; According to thin-layered chromatography test, draw in cape jasmine control medicinal material solution, Gardenoside reference substance solution and the step (1) each 5 μ l of need testing solution, put respectively on same silica gel g thin-layer plate; With percent by volume is that the upper solution of 15: 2: 4 ethyl acetate, glacial acetic acid and water is a developping agent, launches, and takes out; Dry; Spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃, in the test sample chromatogram; With cape jasmine control medicinal material and the corresponding position of Gardenoside reference substance chromatogram on, show the spot of same color;
(3) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize; Hydrochloric acid 10～the 20ml that adds 2mol/L put in the water-bath heating hydrolysis 1.5～3 hours, put cold; Add 60～90 ℃ of sherwood oil 20～30ml, refluxing extraction 0.5～1 hour is obtained sherwood oil liquid; Water bath method, residue is processed need testing solution with methenyl choloride 3ml dissolving; Other gets the diosgenin reference substance, adds methenyl choloride and processes the solution that every 1ml contains the 1mg diosgenin, as the diosgenin reference substance solution; According to the thin-layered chromatography test, draw each 5 μ l of need testing solution and diosgenin reference substance solution, put respectively on same silica gel g thin-layer plate; With percent by volume is that 93: 7 methenyl choloride and acetone soln is developping agent, launches, and takes out; Dry, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of diosgenin reference substance chromatogram on, show the spot of same color;
(4) assay of Gardenoside: prepare need testing solution and reference substance solution respectively, use high effective liquid chromatography for measuring;
Reference substance is: Gardenoside;
Chromatographic condition and system suitability are: be filling agent with the octadecylsilane chemically bonded silica; Second eyeball-redistilled water is a moving phase, the second eyeball: the percent by volume of redistilled water is 15～25: 75～85, and A is the second eyeball, and B is a redistilled water, A+B=100%; Ultraviolet monitor, the detection wavelength is 238nm, number of theoretical plate calculates by the Gardenoside peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of to take by weighing the Gardenoside reference substance, adds methyl alcohol and processes the reference substance solution that every 1ml contains 15 μ g Gardenosides;
The preparation of need testing solution: get 8～20 of diligent those sub-sheets of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize is got 0.1g, and it is fixed to claim; Put in the tool plug conical flask, add methyl alcohol 25ml, close plug, it is fixed to claim, sonicated 15～30 minutes; Put coldly, claim again decide weight, supply the weight that subtracts mistake, shake up filtration with methyl alcohol; Measure filtrating 10ml, put in the 25ml measuring bottle, add methyl alcohol, shake up, promptly get to scale; The power of sonicated is 250w, and frequency is 25KHz;
Determination method: draw each 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, calculate, promptly get.
Optimal technical scheme of the present invention: the prostatitic Chinese medicine detection method of a kind of treatment, it is characterized in that, may further comprise the steps:
(1) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize adds water 50ml; Sonicated 20 minutes is put coldly, filters; The normal butyl alcohol jolting that filtrate water is saturated is extracted 2 times, and each 20ml merges normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1ml dissolving, process need testing solution; Other gets mulberry fruit control medicinal material 5g, adds mass concentration and be 60% ethanolic solution 30ml, reflux 1 hour; Filter, filtrating is concentrated into does not have the alcohol flavor, extracts 2 times with water saturated normal butyl alcohol jolting; Each 20ml merges normal butyl alcohol liquid, evaporate to dryness; Residue adds methyl alcohol 1ml dissolving, processes mulberry fruit control medicinal material solution; According to thin-layered chromatography test, draw respectively 5 μ l of need testing solution and mulberry fruit control medicinal material solution, put respectively on same silica gel g thin-layer plate, be that the upper solution of 15: 1: 4 ethyl acetate, glacial acetic acid and water is a developping agent with percent by volume; Launch, take out, dry; Put under the 365nm ultraviolet lamp and inspect, in the test sample chromatogram, with the corresponding position of mulberry fruit control medicinal material chromatogram on; Show identical blue-fluorescence spot, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of mulberry fruit control medicinal material chromatogram on, show the spot of same color;
(2) get cape jasmine control medicinal material 5g, add mass concentration and be 70% ethanol 30ml, refluxing extraction 1 hour filters, and evaporate to dryness in the filtrating water-bath, residue add methyl alcohol 1ml dissolving, process cape jasmine control medicinal material solution; Other gets the Gardenoside reference substance, adds methyl alcohol and processes the solution that every 1ml contains the 2mg Gardenoside, as the Gardenoside reference substance solution; According to thin-layered chromatography test, draw in cape jasmine control medicinal material solution, Gardenoside reference substance solution and the step (1) each 5 μ l of need testing solution, put respectively on same silica gel g thin-layer plate; With percent by volume is that the upper solution of 15: 2: 4 ethyl acetate, glacial acetic acid and water is a developping agent, launches, and takes out; Dry; Spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃, in the test sample chromatogram; With cape jasmine control medicinal material and the corresponding position of Gardenoside reference substance chromatogram on, show the spot of same color;
(3) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize; The hydrochloric acid 20ml that adds 2mol/L put in the water-bath heating hydrolysis 3 hours, put cold; Add 60～90 ℃ of sherwood oil 30ml, refluxing extraction 1 hour is obtained sherwood oil liquid; Water bath method, residue is processed need testing solution with methenyl choloride 3ml dissolving; Other gets the diosgenin reference substance, adds methenyl choloride and processes the solution that every 1ml contains the 1mg diosgenin, as the diosgenin reference substance solution; According to the thin-layered chromatography test, draw each 5 μ l of need testing solution and diosgenin reference substance solution, put respectively on same silica gel g thin-layer plate; With percent by volume is that 93: 7 methenyl choloride and acetone soln is developping agent, launches, and takes out; Dry, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of diosgenin reference substance chromatogram on, show the spot of same color;
(4) assay of Gardenoside: prepare need testing solution and reference substance solution respectively, use high effective liquid chromatography for measuring;
Reference substance is: Gardenoside;
Chromatographic condition and system suitability are: be filling agent with the octadecylsilane chemically bonded silica; Second eyeball-redistilled water is a moving phase, the second eyeball: the percent by volume of redistilled water is 15: 85, and A is the second eyeball, and B is a redistilled water, A+B=100%; Ultraviolet monitor, the detection wavelength is 238nm, number of theoretical plate calculates by the Gardenoside peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of to take by weighing the Gardenoside reference substance, adds methyl alcohol and processes the reference substance solution that every 1ml contains 15 μ g Gardenosides;
The preparation of need testing solution: get 8 of diligent those sub-sheets of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize is got 0.1g, and it is fixed to claim; Put in the tool plug conical flask, add methyl alcohol 25ml, close plug, it is fixed to claim, sonicated 20 minutes; Put coldly, claim again decide weight, supply the weight that subtracts mistake, shake up filtration with methyl alcohol; Measure filtrating 10ml, put in the 25ml measuring bottle, add methyl alcohol, shake up, promptly get to scale; The power of sonicated is 250w, and frequency is 25KHz;
Determination method: draw each 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, calculate, promptly get.
The present invention compared with prior art has the following advantages: the present invention passes through high performance liquid chromatography; Realized accurate mensuration to Gardenoside content; This method is easy and simple to handle; Accurately advanced, linear relationship, reappearance, precision, stability, the recovery are all better, quality that can more effective control product.
Embodiment
Embodiment
(1) qualitative detection research
1, diligent those the sub-sheet 2g of Xi Payimai remove film-coating, and porphyrize adds water 50ml, ultrasonic 20 minutes; Put coldly, filter, the normal butyl alcohol jolting that filtrate water is saturated is extracted 2 times, each 20ml; Merge normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.Simultaneously, get other medicinal material that does not contain mulberry fruit, process negative control solution according to diligent those sub-sheet preparation technologies of Xi Payimai and test sample preparation method.Other gets mulberry fruit control medicinal material 5g, adds 60% ethanolic solution 30ml, and reflux 1 hour filters, and filtrating is concentrated into does not have the alcohol flavor, extracts 2 times with water saturated normal butyl alcohol jolting, processes control medicinal material solution with method for making.According to the thin-layered chromatography test, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; With ethyl acetate: glacial acetic acid: the percent by volume of water is that 15: 1: 4 upper solution is a developping agent, launches, and takes out; Dry, put that (365nm) inspects under the ultraviolet lamp.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical blue-fluorescence spot, negative control solution is noiseless; Spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color, negative control solution is noiseless.
2, get the prescription medicinal material that does not contain cape jasmine, process negative control solution according to diligent those sub-sheet preparation technologies of Xi Payimai and test sample preparation method.Get cape jasmine control medicinal material 5g, add 70% ethanol 30ml, refluxing extraction 1 hour, filtrating, evaporate to dryness in the filtrating water-bath, residue add methyl alcohol 1ml dissolving, process control medicinal material solution.Other gets the Gardenoside reference substance, adds methyl alcohol and processes the solution that every 1ml contains 2mg, as reference substance solution.According to the thin-layered chromatography test, draw each the 5 μ l of need testing solution in above-mentioned three kinds of solution and the step 1, put respectively on same silica gel g thin-layer plate; With ethyl acetate: glacial acetic acid: the percent by volume of water is that 15: 2: 4 upper solution is a developping agent; Launch, take out, dry; Spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃.In the test sample chromatogram, with control medicinal material and the corresponding position of reference substance chromatogram on, show the spot of same color, negative control solution is noiseless.
3, get 8～20 of diligent those sub-sheets of Xi Payimai (preferred 8), remove film-coating, porphyrize; Add 2mol/L hydrochloric acid 20ml and put in the water-bath heating hydrolysis 3 hours, put coldly, add 60～90 ℃ of sherwood oil 30ml refluxing extraction 1 hour; Obtain sherwood oil liquid; Water bath method, residue is with methenyl choloride 3ml dissolving, as need testing solution.Simultaneously, get other medicinal material that does not contain dioscoreae septemlobae,rhizoma, process negative control solution according to diligent those sub-sheet preparation technologies of Xi Payimai and test sample preparation method.Other gets the diosgenin reference substance, adds methenyl choloride and processes the solution that every 1ml contains 1mg, as need testing solution.According to thin-layered chromatography test, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with the percent by volume of methenyl choloride-acetone be 93: 7 be developping agent, launch, taking-up is dried.Spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color, negative control solution is noiseless.
(2) detection by quantitative research
1, the investigation of extraction time: get diligent 20 of those sub-sheets of Xi Payimai (lot number 20040506), remove film-coating, porphyrize is got 0.1g, 6 parts; The accurate title, decide, and puts respectively in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, and close plug, the accurate title, decide; Sonicated (power 250w, frequency 25KHz) different time is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methyl alcohol; Shake up, filter, precision is measured subsequent filtrate 10ml, puts in the 25ml measuring bottle, adds methyl alcohol to scale; Shake up, get the subsequent filtrate sample introduction, measure, try to achieve Gardenoside content, the result sees table 1.
Table 1 sonicated different time test findings
Above result shows, sonicated 20 minutes, and recording Gardenoside content (or ratio of peak area and sampling amount) no longer increases, in order to guarantee to extract fully, so confirm that the sonicated time is 20 minutes.
2, the investigation of chromatographic condition
2.1 the selection of moving phase: second eyeball-redistilled water (the two percent by volume is 15: 85).
2.2 with the octadecylsilane chemically bonded silica is filling agent; Second eyeball-redistilled water (the two percent by volume is 15: 85) is a moving phase, and A is the second eyeball, and B is a redistilled water, A+B=100%; Ultraviolet monitor, the detection wavelength is 238nm, number of theoretical plate calculates by the Gardenoside peak should be not less than 1500;
2.3 the reference substance solution preparation: it is an amount of that precision takes by weighing the Gardenoside reference substance, adds methyl alcohol and process the solution that every 1ml contains 15 μ g, promptly gets.
2.4 the preparation of need testing solution: get 20 of diligent those sub-sheets of Xi Payimai, remove film-coating, porphyrize is got 0.1g, and accurate the title decides, and puts in the tool plug conical flask; The accurate methyl alcohol 25ml that adds, close plug, the accurate title, decide, and sonicated (power 250w, frequency 25KHz) 20 minutes is put cold; Claim to decide weight again, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 10ml; Put in the 25ml measuring bottle, add methyl alcohol, shake up, filter, promptly get with 0.45 μ m miillpore filter to scale.
3, methodological study
3.1 negative control test: get the prescription medicinal material that does not contain cape jasmine, process the negative control sample, process negative control solution by the need testing solution compound method again according to diligent those sub-sheet preparation technologies of Xi Payimai and test sample preparation method.The accurate 10 μ l that draw inject liquid chromatograph.Can find out that from chromatogram no chromatographic peak occurs in the Gardenoside position, so negative control does not disturb Gardenoside to measure.
3.2 linear relationship is investigated: precision takes by weighing Gardenoside reference substance 15.2014mg; Adding methyl alcohol processes every ml in right amount and contains Gardenoside 15.2 μ g reference substance solution; Get reference substance solution 2 μ l, 4 μ l, 7.5 μ l, 10 μ l, 15 μ l, 20 μ l respectively; The sequentially determining peak area carries out linear regression with sample size to peak area, and the result sees table 2.
Table 2 linear test result
Regression equation: y=47561x+216.54, R=0.9992.
The result shows: the Gardenoside sample size in 0.0304～0.304 μ g scope internal linear relation better.
3.3 precision test: get above-mentioned reference substance solution 10 μ l,, repeat sample introduction respectively 6 times, measure peak area in accordance with the law with need testing solution 10 μ l.The result shows that precision is good, sees table 3.
Table 3 Precision test result
3.4 stability test: get with a need testing solution, measured peak area with 0 hour, 2 hours, 4 hours, 6 hours, 12 hours, 24 hours respectively, the result sees table 4.
Table 4 stability test result
Test shows: test sample is better at 24 hours internal stabilities.
3.5 repeatability: get with 6 parts of lot sample article (lot number 20040506), measure by the text method, the result sees table 5.
Table 5 sample reproducible test results
3.6 recovery test: get totally 6 parts of the about 0.1g of sample powder (lot number 20040506) of known content, accurately claim surely, place tool plug conical flask respectively, the accurate respectively reference substance solution (mg/ml) that adds.Measure the recovery by method under text [assay] item respectively, the result sees table 6.
Table 6 recovery test result
3.7 cape jasmine medicinal material assay and limit are definite: 6 batches of the material sample powder of getting it filled respectively, about 0.1g, the accurate title, decide, and measures by method under text [assay] item, and the result sees table 7.
Table 7 cape jasmine medicinal material contains quantity research
The 6 batches of cape jasmine medicinal material sample sizes between 2.93%～3.88%, in order to guarantee finished product content, in conjunction with requirement under cape jasmine item of version Chinese Pharmacopoeia in 2005, confirm that content limit must not be lower than 1.8% in Gardenoside
3.8 sample determination and limit are confirmed: get each 2 parts of 4 lot sample article, measure by method under text [assay] item, the result sees table 8.
Table 8 sample size is measured the result
According to 3 lot sample article measured datas, consider factors such as crude drug source, preparation production, storage, tentative diligent those every of sub-sheets of Xi Payimai contain cape jasmine with Gardenoside (C
17H
240
10) meter, must not be less than the 3.0mg/ sheet.
Claims (2)
1. treat prostatitic Chinese medicine detection method for one kind; Diligent those the sub-sheets of treatment prostatitis medicine-Xi Payimai are processed by following medicinal materials in part by weight: 300～600 parts in mulberry fruit, 300～600 parts of Gorgon fruits, 200～400 parts of dioscoreae septemlobae,rhizomas; 200～500 parts of the fruits of Cherokee rose, 200～400 parts on mast;
The preparation method of treatment prostatitis medicine-Xi Payimai diligent those sub-sheets: with mulberry fruit, Gorgon fruit, the fruit of Cherokee rose and the boiling of mast four traditional Chinese medicine material 3 times; Respectively decocted for first and second times 2 hours, and decocted collecting decoction for the third time 1 hour; Leave standstill; Filter, it is 1: 1 volume that filtrating is concentrated into the crude drug volume ratio, subsequent use; Dioscoreae septemlobae,rhizoma is ground into meal, adds alcohol reflux 3 times, each 1 hour, filter, merging filtrate merges with above-mentioned reserve liquid; Adding ethanol is 70% to containing pure quality, leaves standstill 24 hours, filter, and filtrate recycling ethanol, being concentrated into 55～60 ℃ of heat survey relative densities is 1.20～1.25, drying under reduced pressure; Pulverize, add appropriate amount of starch and carboxyrnethyl starch sodium, mixing is granulated drying; Add dolomol, mixing, compacting is wrapped film-coating in flakes, promptly gets;
It is characterized in that this Chinese medicine detection method may further comprise the steps:
(1) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize adds water 30～50ml; Sonicated 10～20 minutes is put coldly, filters; The normal butyl alcohol jolting that filtrate water is saturated is extracted 2 times, and each 10～20ml merges normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1ml dissolving, process need testing solution; Other gets mulberry fruit control medicinal material 5g, adds mass concentration and be 60% ethanolic solution 30ml, reflux 1 hour; Filter, filtrating is concentrated into does not have the alcohol flavor, extracts 2 times with water saturated normal butyl alcohol jolting; Each 10～20ml merges normal butyl alcohol liquid, evaporate to dryness; Residue adds methyl alcohol 1ml dissolving, processes mulberry fruit control medicinal material solution; According to thin-layered chromatography test, draw respectively 5 μ l of need testing solution and mulberry fruit control medicinal material solution, put respectively on same silica gel g thin-layer plate, be that the upper solution of 15: 1: 4 ethyl acetate, glacial acetic acid and water is a developping agent with percent by volume; Launch, take out, dry; Put under the 365nm ultraviolet lamp and inspect, in the test sample chromatogram, with the corresponding position of mulberry fruit control medicinal material chromatogram on; Show identical blue-fluorescence spot, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of mulberry fruit control medicinal material chromatogram on, show the spot of same color;
(2) get cape jasmine control medicinal material 5g, add mass concentration and be 70% ethanol 30ml, refluxing extraction 1 hour filters, and evaporate to dryness in the filtrating water-bath, residue add methyl alcohol 1ml dissolving, process cape jasmine control medicinal material solution; Other gets the Gardenoside reference substance, adds methyl alcohol and processes the solution that every 1ml contains the 2mg Gardenoside, as the Gardenoside reference substance solution; According to thin-layered chromatography test, draw in cape jasmine control medicinal material solution, Gardenoside reference substance solution and the step (1) each 5 μ l of need testing solution, put respectively on same silica gel g thin-layer plate; With percent by volume is that the upper solution of 15: 2: 4 ethyl acetate, glacial acetic acid and water is a developping agent, launches, and takes out; Dry; Spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃, in the test sample chromatogram; With cape jasmine control medicinal material and the corresponding position of Gardenoside reference substance chromatogram on, show the spot of same color;
(3) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize; Hydrochloric acid 10～the 20ml that adds 2mol/L put in the water-bath heating hydrolysis 1.5～3 hours, put cold; Add 60～90 ℃ of sherwood oil 20～30ml, refluxing extraction 0.5～1 hour is obtained sherwood oil liquid; Water bath method, residue is processed need testing solution with methenyl choloride 3ml dissolving; Other gets the diosgenin reference substance, adds methenyl choloride and processes the solution that every 1ml contains the 1mg diosgenin, as the diosgenin reference substance solution; According to the thin-layered chromatography test, draw each 5 μ l of need testing solution and diosgenin reference substance solution, put respectively on same silica gel g thin-layer plate; With percent by volume is that 93: 7 methenyl choloride and acetone soln is developping agent, launches, and takes out; Dry, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of diosgenin reference substance chromatogram on, show the spot of same color;
(4) assay of Gardenoside: prepare need testing solution and reference substance solution respectively, use high effective liquid chromatography for measuring;
Reference substance is: Gardenoside;
Chromatographic condition and system suitability are: be filling agent with the octadecylsilane chemically bonded silica; Second eyeball-redistilled water is a moving phase, the second eyeball: the percent by volume of redistilled water is 15～25: 75～85, and A is the second eyeball, and B is a redistilled water, A+B=100%; Ultraviolet monitor, the detection wavelength is 238nm, number of theoretical plate calculates by the Gardenoside peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of to take by weighing the Gardenoside reference substance, adds methyl alcohol and processes the reference substance solution that every 1ml contains 15 μ g Gardenosides;
The preparation of need testing solution: get 8～20 of diligent those sub-sheets of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize is got 0.1g, and it is fixed to claim; Put in the tool plug conical flask, add methyl alcohol 25ml, close plug, it is fixed to claim, sonicated 15～30 minutes; Put coldly, claim again decide weight, supply the weight that subtracts mistake, shake up filtration with methyl alcohol; Measure filtrating 10ml, put in the 25ml measuring bottle, add methyl alcohol, shake up, promptly get to scale; The power of sonicated is 250w, and frequency is 25KHz;
Determination method: draw each 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, calculate, promptly get.
2. the prostatitic Chinese medicine detection method of a kind of treatment according to claim 1 is characterized in that, may further comprise the steps:
(1) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize adds water 50ml; Sonicated 20 minutes is put coldly, filters; The normal butyl alcohol jolting that filtrate water is saturated is extracted 2 times, and each 20ml merges normal butyl alcohol liquid; Evaporate to dryness, residue add methyl alcohol 1ml dissolving, process need testing solution; Other gets mulberry fruit control medicinal material 5g, adds mass concentration and be 60% ethanolic solution 30ml, reflux 1 hour; Filter, filtrating is concentrated into does not have the alcohol flavor, extracts 2 times with water saturated normal butyl alcohol jolting; Each 20ml merges normal butyl alcohol liquid, evaporate to dryness; Residue adds methyl alcohol 1ml dissolving, processes mulberry fruit control medicinal material solution; According to thin-layered chromatography test, draw respectively 5 μ l of need testing solution and mulberry fruit control medicinal material solution, put respectively on same silica gel g thin-layer plate, be that the upper solution of 15: 1: 4 ethyl acetate, glacial acetic acid and water is a developping agent with percent by volume; Launch, take out, dry; Put under the 365nm ultraviolet lamp and inspect, in the test sample chromatogram, with the corresponding position of mulberry fruit control medicinal material chromatogram on; Show identical blue-fluorescence spot, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of mulberry fruit control medicinal material chromatogram on, show the spot of same color;
(2) get cape jasmine control medicinal material 5g, add mass concentration and be 70% ethanol 30ml, refluxing extraction 1 hour filters, and evaporate to dryness in the filtrating water-bath, residue add methyl alcohol 1ml dissolving, process cape jasmine control medicinal material solution; Other gets the Gardenoside reference substance, adds methyl alcohol and processes the solution that every 1ml contains the 2mg Gardenoside, as the Gardenoside reference substance solution; According to thin-layered chromatography test, draw in cape jasmine control medicinal material solution, Gardenoside reference substance solution and the step (1) each 5 μ l of need testing solution, put respectively on same silica gel g thin-layer plate; With percent by volume is that the upper solution of 15: 2: 4 ethyl acetate, glacial acetic acid and water is a developping agent, launches, and takes out; Dry; Spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the spot colour developing at 105 ℃, in the test sample chromatogram; With cape jasmine control medicinal material and the corresponding position of Gardenoside reference substance chromatogram on, show the spot of same color;
(3) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize; The hydrochloric acid 20ml that adds 2mol/L put in the water-bath heating hydrolysis 3 hours, put cold; Add 60～90 ℃ of sherwood oil 30ml, refluxing extraction 1 hour is obtained sherwood oil liquid; Water bath method, residue is processed need testing solution with methenyl choloride 3ml dissolving; Other gets the diosgenin reference substance, adds methenyl choloride and processes the solution that every 1ml contains the 1mg diosgenin, as the diosgenin reference substance solution; According to the thin-layered chromatography test, draw each 5 μ l of need testing solution and diosgenin reference substance solution, put respectively on same silica gel g thin-layer plate; With percent by volume is that 93: 7 methenyl choloride and acetone soln is developping agent, launches, and takes out; Dry, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of diosgenin reference substance chromatogram on, show the spot of same color;
(4) assay of Gardenoside: prepare need testing solution and reference substance solution respectively, use high effective liquid chromatography for measuring;
Reference substance is: Gardenoside;
Chromatographic condition and system suitability are: be filling agent with the octadecylsilane chemically bonded silica; Second eyeball-redistilled water is a moving phase, the second eyeball: the percent by volume of redistilled water is 15: 85, and A is the second eyeball, and B is a redistilled water, A+B=100%; Ultraviolet monitor, the detection wavelength is 238nm, number of theoretical plate calculates by the Gardenoside peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of to take by weighing the Gardenoside reference substance, adds methyl alcohol and processes the reference substance solution that every 1ml contains 15 μ g Gardenosides;
The preparation of need testing solution: get 8 of diligent those sub-sheets of treatment prostatitis medicine-Xi Payimai, remove film-coating, porphyrize is got 0.1g, and it is fixed to claim; Put in the tool plug conical flask, add methyl alcohol 25ml, close plug, it is fixed to claim, sonicated 20 minutes; Put coldly, claim again decide weight, supply the weight that subtracts mistake, shake up filtration with methyl alcohol; Measure filtrating 10ml, put in the 25ml measuring bottle, add methyl alcohol, shake up, promptly get to scale; The power of sonicated is 250w, and frequency is 25KHz;
Determination method: draw each 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, calculate, promptly get.
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