CN101810752A - 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 the quality of 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 quality detection method of a kind of treatment.
Background technology
Prostatic hyperplasia is a kind of commonly encountered diseases, the frequently-occurring disease of elderly men, and sickness rate increases gradually with age growth.It mainly shows: frequent micturition, dysuria, acute urine retention or urinary incontinence; Necessary urethral catheterization of severe patient or hands art; Prostatitis also is urology department male commonly encountered diseases, frequently-occurring disease, mainly shows as urgent micturition, frequent micturition, dysurea, meeting pain over the perineum, 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 for the treatment of is disclosed, its be by Fructus Mori, Semen Euryales, Rhizoma Dioscoreae Septemlobae, Cherokee rose, Fructus Gardeniae etc. through being processed into active constituents of medicine and the medicine acceptable carrier by the capsule of certain proportioning through being processed into.
And the present invention is compositions such as Fructus Mori, Semen Euryales, Rhizoma Dioscoreae Septemlobae, Cherokee rose, Fructus Gardeniae, 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, pure and impure diuretic effect.Be quantitative target with the jasminoidin in the standard.Method about the assay of jasminoidin mostly 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 jasminoidin in the high effective liquid chromatography for measuring said preparation.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned deficiency of the prior art, provides a kind of treatment prostatitic Chinese medicine quality detection method.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the prostatitic Chinese medicine quality detection method of a kind of treatment, diligent those the sub-sheets of treatment prostatitis medicine-Xi Payimai are made by following medicinal materials in part by weight: 300～600 parts in Fructus Mori, 200～400 parts of 300～600 parts of Rhizoma Dioscoreae Septemlobaes of Semen Euryales, 200～500 parts of Fructus Rosae Laevigatae, 200～400 parts of Fructus Gardeniae;
The preparation method of diligent those the sub-sheets of treatment prostatitis medicine-Xi Payimai: Fructus Mori, Semen Euryales, Fructus Rosae Laevigatae and Fructus Gardeniae four Chinese medicine material are decocted with water 3 times, respectively decocted for first and second times 2 hours, decocted for the third time 1 hour, collecting decoction, leave standstill, filter, it is 1: 1 volume that filtrate is concentrated into the crude drug volume ratio, standby; Rhizoma Dioscoreae Septemlobae is ground into coarse powder, adds alcohol reflux 3 times, each 1 hour, filter, merging filtrate merges with above-mentioned reserve liquid, and adding ethanol is 70% to containing pure quality, leaves standstill 24 hours, filter, 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 carboxymethylstach sodium, mixing is granulated, drying adds magnesium stearate, mixing, compacting is wrapped film-coat, promptly in flakes;
It is characterized in that this Chinese medicine quality detection method may further comprise the steps:
(1) gets diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize, add water 30～50ml, supersound process 10～20 minutes is put coldly, filters, the n-butyl alcohol jolting that filtrate water is saturated is extracted 2 times, each 10～20ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 1ml dissolving, makes need testing solution; Other gets Fructus Mori control medicinal material 5g, add mass concentration and be 60% alcoholic solution 30ml, reflux 1 hour filters, and filtrate is concentrated into does not have the alcohol flavor, extract 2 times with water saturated n-butyl alcohol jolting, each 10～20ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 1ml dissolving, makes Fructus Mori control medicinal material solution; According to the thin layer chromatography test, draw each 5 μ l of need testing solution and Fructus Mori control medicinal material solution, put respectively on same silica gel g thin-layer plate, with percent by volume is that the upper solution of 15: 1: 4 ethyl acetate, glacial acetic acid and water is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of Fructus Mori control medicinal material chromatograph on, show identical blue-fluorescence speckle, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of Fructus Mori control medicinal material chromatograph on, show the speckle of same color;
(2) get Fructus Gardeniae control medicinal material 5g, add mass concentration and be 70% ethanol 30ml, reflux, extract, 1 hour filters, and evaporate to dryness in the filtrate water-bath, residue add methanol 1ml dissolving, make Fructus Gardeniae control medicinal material solution; Other gets the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains the 2mg jasminoidin, as the jasminoidin reference substance solution; Test according to thin layer chromatography, draw in Fructus Gardeniae control medicinal material solution, jasminoidin 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 developing solvent, launch, take out, dry, spray is with phosphomolybdic acid ethanol test solution, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with Fructus Gardeniae control medicinal material and the corresponding position of jasminoidin reference substance chromatograph on, show the speckle of same color;
(3) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize adds hydrochloric acid 10～20ml of 2mol/L, put in the water-bath heating hydrolysis 1.5～3 hours, put coldly, add 60～90 ℃ of petroleum ether 20～30ml, reflux, extract, 0.5～1 hour, divide and get petroleum ether liquid, water bath method, residue is made need testing solution with chloroform 3ml dissolving; Other gets the diosgenin reference substance, adds chloroform and makes the solution that every 1ml contains the 1mg diosgenin, as the diosgenin reference substance solution; Test according to thin layer chromatography, drawing each 5 μ l of need testing solution and diosgenin reference substance solution, put respectively on same silica gel g thin-layer plate, is that 93: 7 chloroform and acetone soln is developing solvent with percent by volume, launch, take out, dry, spray is with phosphomolybdic acid ethanol test solution, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with the corresponding position of diosgenin reference substance chromatograph on, show the speckle of same color;
(4) assay of jasminoidin: prepare need testing solution and reference substance solution respectively, use high effective liquid chromatography for measuring;
Reference substance is: jasminoidin;
Chromatographic condition and system suitability are: be filler with the octadecylsilane chemically bonded silica; Second eyeball-redistilled water is a mobile 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%; Ultra-violet monitor, the detection wavelength is 238nm, number of theoretical plate calculates by the jasminoidin peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of to take by weighing the jasminoidin reference substance, adds methanol and makes the reference substance solution that every 1ml contains 15 μ g jasminoidins;
The preparation of need testing solution: get 8～20 of diligent those sub-sheets of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize is got 0.1g, it is fixed to claim, puts in the tool plug conical flask, adds methanol 25ml, close plug, it is fixed to claim, supersound process 15～30 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, measure filtrate 10ml, put in the 25ml measuring bottle, add methanol to scale, shake up, promptly; The power of supersound process is 250w, and frequency is 25KHz;
Algoscopy: draw each 10 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid, measure, calculate, promptly.
The preferred technical solution of the present invention: the prostatitic Chinese medicine quality detection method of a kind of treatment, it is characterized in that, may further comprise the steps:
(1) gets diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize, add water 50ml, supersound process 20 minutes is put coldly, filters, the n-butyl alcohol jolting that filtrate water is saturated is extracted 2 times, each 20ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 1ml dissolving, makes need testing solution; Other gets Fructus Mori control medicinal material 5g, add mass concentration and be 60% alcoholic solution 30ml, reflux 1 hour filters, and filtrate is concentrated into does not have the alcohol flavor, extract 2 times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 1ml dissolving, makes Fructus Mori control medicinal material solution; According to the thin layer chromatography test, draw each 5 μ l of need testing solution and Fructus Mori control medicinal material solution, put respectively on same silica gel g thin-layer plate, with percent by volume is that the upper solution of 15: 1: 4 ethyl acetate, glacial acetic acid and water is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of Fructus Mori control medicinal material chromatograph on, show identical blue-fluorescence speckle, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of Fructus Mori control medicinal material chromatograph on, show the speckle of same color;
(2) get Fructus Gardeniae control medicinal material 5g, add mass concentration and be 70% ethanol 30ml, reflux, extract, 1 hour filters, and evaporate to dryness in the filtrate water-bath, residue add methanol 1ml dissolving, make Fructus Gardeniae control medicinal material solution; Other gets the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains the 2mg jasminoidin, as the jasminoidin reference substance solution; Test according to thin layer chromatography, draw in Fructus Gardeniae control medicinal material solution, jasminoidin 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 developing solvent, launch, take out, dry, spray is with phosphomolybdic acid ethanol test solution, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with Fructus Gardeniae control medicinal material and the corresponding position of jasminoidin reference substance chromatograph on, show the speckle of same color;
(3) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize adds the hydrochloric acid 20ml of 2mol/L, put in the water-bath heating hydrolysis 3 hours, put coldly, add 60～90 ℃ of petroleum ether 30ml, reflux, extract, 1 hour, divide and get petroleum ether liquid, water bath method, residue is made need testing solution with chloroform 3ml dissolving; Other gets the diosgenin reference substance, adds chloroform and makes the solution that every 1ml contains the 1mg diosgenin, as the diosgenin reference substance solution; Test according to thin layer chromatography, drawing each 5 μ l of need testing solution and diosgenin reference substance solution, put respectively on same silica gel g thin-layer plate, is that 93: 7 chloroform and acetone soln is developing solvent with percent by volume, launch, take out, dry, spray is with phosphomolybdic acid ethanol test solution, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with the corresponding position of diosgenin reference substance chromatograph on, show the speckle of same color;
(4) assay of jasminoidin: prepare need testing solution and reference substance solution respectively, use high effective liquid chromatography for measuring;
Reference substance is: jasminoidin;
Chromatographic condition and system suitability are: be filler with the octadecylsilane chemically bonded silica; Second eyeball-redistilled water is a mobile 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%; Ultra-violet monitor, the detection wavelength is 238nm, number of theoretical plate calculates by the jasminoidin peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of to take by weighing the jasminoidin reference substance, adds methanol and makes the reference substance solution that every 1ml contains 15 μ g jasminoidins;
The preparation of need testing solution: get 8 of diligent those sub-sheets of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize is got 0.1g, it is fixed to claim, puts in the tool plug conical flask, adds methanol 25ml, close plug, it is fixed to claim, supersound process 20 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, measure filtrate 10ml, put in the 25ml measuring bottle, add methanol to scale, shake up, promptly; The power of supersound process is 250w, and frequency is 25KHz;
Algoscopy: draw each 10 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid, measure, calculate, promptly.
The present invention compared with prior art has the following advantages: the present invention passes through high performance liquid chromatography, realized accurate mensuration to jasminoidin content, this method is easy and simple to handle, accurately advanced, linear relationship, repeatability, precision, stability, the response rate are all better, quality that can more effective control product.
The specific embodiment
Embodiment
(1) qualitative detection research
1, diligent those the sub-sheet 2g of Xi Payimai remove film-coat, and porphyrize adds water 50ml, ultrasonic 20 minutes, put coldly, filter, the n-butyl alcohol jolting that filtrate water is saturated is extracted 2 times, each 20ml, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Simultaneously, get other medical material that does not contain Fructus Mori, make negative control solution according to diligent those sub-sheet preparation technologies of Xi Payimai and test sample preparation method.Other gets Fructus Mori control medicinal material 5g, adds 60% alcoholic solution 30ml, and reflux 1 hour filters, and filtrate is concentrated into does not have the alcohol flavor, extracts 2 times with water saturated n-butyl alcohol jolting, makes control medicinal material solution with method for making.According to the thin layer 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 developing solvent, launches, and takes out, dry, put that (365nm) inspects under the ultra-violet lamp.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical blue-fluorescence speckle, negative control solution is noiseless; Spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color, negative control solution is noiseless.
2, get the prescription medical material that does not contain Fructus Gardeniae, make negative control solution according to diligent those sub-sheet preparation technologies of Xi Payimai and test sample preparation method.Get Fructus Gardeniae control medicinal material 5g, add 70% ethanol 30ml, reflux, extract, 1 hour, filtrate, evaporate to dryness in the filtrate water-bath, residue add methanol 1ml dissolving, make control medicinal material solution.Other gets the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography, 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 developing solvent, launch, take out, dry, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color, negative control solution is noiseless.
3, get 8～20 of diligent those sub-sheets of Xi Payimai (preferred 8), remove film-coat, porphyrize, add 2mol/L hydrochloric acid 20ml and put in the water-bath heating hydrolysis 3 hours, put coldly, add 60～90 ℃ of petroleum ether 30ml reflux, extract, 1 hour, divide and get petroleum ether liquid, water bath method, residue is with chloroform 3ml dissolving, as need testing solution.Simultaneously, get other medical material that does not contain Rhizoma Dioscoreae Septemlobae, make 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 chloroform and makes the solution that every 1ml contains 1mg, as need testing solution.According to thin layer 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 chloroform-acetone be 93: 7 be developing solvent, launch, taking-up is dried.Spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle 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-coat, porphyrize, get 0.1g, 6 parts, the accurate title, decide, put in the tool plug conical flask accurate methanol 25ml, the close plug of adding respectively, the accurate title, decided supersound process (power 250w, frequency 25KHz) different time, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 10ml, puts in the 25ml measuring bottle, add methanol to scale, shake up, get the subsequent filtrate sample introduction, measure, try to achieve jasminoidin content, the results are shown in Table 1.
Table 1 supersound process different time result of the test
Above result shows, supersound process 20 minutes, and recording jasminoidin content (or ratio of peak area and sampling amount) no longer increases, in order to guarantee to extract fully, so determine that the supersound process time is 20 minutes.
2, the investigation of chromatographic condition
2.1 the selection of mobile phase: second eyeball-redistilled water (the two percent by volume is 15: 85).
2.2 with the octadecylsilane chemically bonded silica is filler; Second eyeball-redistilled water (the two percent by volume is 15: 85) is a mobile phase, and A is the second eyeball, and B is a redistilled water, A+B=100%; Ultra-violet monitor, the detection wavelength is 238nm, number of theoretical plate calculates by the jasminoidin 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 jasminoidin reference substance, adds methanol and make the solution that every 1ml contains 15 μ g, promptly.
2.4 the preparation of need testing solution: get 20 of diligent those sub-sheets of Xi Payimai, remove film-coat, porphyrize is got 0.1g, the accurate title, decide, and puts in the tool plug conical flask, accurate methanol 25ml, the close plug of adding, the accurate title, decide, and supersound process (power 250w, frequency 25KHz) 20 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methanol, precision is measured subsequent filtrate 10ml, puts in the 25ml measuring bottle, adds methanol to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly.
3, methodological study
3.1 negative control test: get the prescription medical material that does not contain Fructus Gardeniae, make the negative control sample, make 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 chromatograph of liquid.No chromatographic peak occurs in the jasminoidin position as can be seen from chromatogram, so negative control does not disturb jasminoidin to measure.
3.2 linear relationship is investigated: precision takes by weighing jasminoidin reference substance 15.2014mg, adding methanol makes every ml in right amount and contains jasminoidin 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, with sample size peak area is carried out linear regression, the results are shown in Table 2.
Table 2 linear test result
Regression equation: y=47561x+216.54, R=0.9992.
The result shows: the jasminoidin 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 results are shown in Table 4.
Table 4 stability test result
Test shows: test sample is better at 24 hours internal stabilities.
3.5 repeatability: get 6 parts of same batch samples (lot number 20040506), measure, the results are shown in Table 5 by the text method.
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 response rate by method under text [assay] item respectively, the results are shown in Table 6.
Table 6 recovery test result
3.7 Fructus Gardeniae medical 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, the results are shown in Table 7.
Table 7 Fructus Gardeniae medical material contains quantity research
The 6 batches of Fructus Gardeniae medical material sample sizes between 2.93%～3.88%, in order to guarantee finished product content, in conjunction with requirement under Fructus Gardeniae item of version Chinese Pharmacopoeia in 2005, determine that content limit must not be lower than 1.8% in jasminoidin
3.8 sample determination and limit are determined: get each 2 parts of 4 batch samples, measure, the results are shown in Table 8 by method under text [assay] item.
Table 8 sample size measurement result
According to 3 batch sample measured datas, consider factors such as crude drug source, preparation production, storage, tentative diligent those every of sub-sheets of Xi Payimai contain Fructus Gardeniae with jasminoidin (C
17H
24O
10) meter, must not be less than the 3.0mg/ sheet.
Claims (2)
1. treat prostatitic Chinese medicine quality detection method for one kind, diligent those the sub-sheets of treatment prostatitis medicine-Xi Payimai are made by following medicinal materials in part by weight: 300～600 parts in Fructus Mori, 300～600 parts of Semen Euryaless, 200～400 parts of Rhizoma Dioscoreae Septemlobaes, 200～500 parts of Fructus Rosae Laevigatae, 200～400 parts of Fructus Gardeniae;
The preparation method of diligent those the sub-sheets of treatment prostatitis medicine-Xi Payimai: Fructus Mori, Semen Euryales, Fructus Rosae Laevigatae and Fructus Gardeniae four Chinese medicine material are decocted with water 3 times, respectively decocted for first and second times 2 hours, decocted for the third time 1 hour, collecting decoction, leave standstill, filter, it is 1: 1 volume that filtrate is concentrated into the crude drug volume ratio, standby; Rhizoma Dioscoreae Septemlobae is ground into coarse powder, adds alcohol reflux 3 times, each 1 hour, filter, merging filtrate merges with above-mentioned reserve liquid, and adding ethanol is 70% to containing pure quality, leaves standstill 24 hours, filter, 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 carboxymethylstach sodium, mixing is granulated, drying adds magnesium stearate, mixing, compacting is wrapped film-coat, promptly in flakes;
It is characterized in that this Chinese medicine quality detection method may further comprise the steps:
(1) gets diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize, add water 30～50ml, supersound process 10～20 minutes is put coldly, filters, the n-butyl alcohol jolting that filtrate water is saturated is extracted 2 times, each 10～20ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 1ml dissolving, makes need testing solution; Other gets Fructus Mori control medicinal material 5g, add mass concentration and be 60% alcoholic solution 30ml, reflux 1 hour filters, and filtrate is concentrated into does not have the alcohol flavor, extract 2 times with water saturated n-butyl alcohol jolting, each 10～20ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 1ml dissolving, makes Fructus Mori control medicinal material solution; According to the thin layer chromatography test, draw each 5 μ l of need testing solution and Fructus Mori control medicinal material solution, put respectively on same silica gel g thin-layer plate, with percent by volume is that the upper solution of 15: 1: 4 ethyl acetate, glacial acetic acid and water is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of Fructus Mori control medicinal material chromatograph on, show identical blue-fluorescence speckle, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of Fructus Mori control medicinal material chromatograph on, show the speckle of same color;
(2) get Fructus Gardeniae control medicinal material 5g, add mass concentration and be 70% ethanol 30ml, reflux, extract, 1 hour filters, and evaporate to dryness in the filtrate water-bath, residue add methanol 1ml dissolving, make Fructus Gardeniae control medicinal material solution; Other gets the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains the 2mg jasminoidin, as the jasminoidin reference substance solution; Test according to thin layer chromatography, draw in Fructus Gardeniae control medicinal material solution, jasminoidin 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 developing solvent, launch, take out, dry, spray is with phosphomolybdic acid ethanol test solution, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with Fructus Gardeniae control medicinal material and the corresponding position of jasminoidin reference substance chromatograph on, show the speckle of same color;
(3) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize adds hydrochloric acid 10～20ml of 2mol/L, put in the water-bath heating hydrolysis 1.5～3 hours, put coldly, add 60～90 ℃ of petroleum ether 20～30ml, reflux, extract, 0.5～1 hour, divide and get petroleum ether liquid, water bath method, residue is made need testing solution with chloroform 3ml dissolving; Other gets the diosgenin reference substance, adds chloroform and makes the solution that every 1ml contains the 1mg diosgenin, as the diosgenin reference substance solution; Test according to thin layer chromatography, drawing each 5 μ l of need testing solution and diosgenin reference substance solution, put respectively on same silica gel g thin-layer plate, is that 93: 7 chloroform and acetone soln is developing solvent with percent by volume, launch, take out, dry, spray is with phosphomolybdic acid ethanol test solution, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with the corresponding position of diosgenin reference substance chromatograph on, show the speckle of same color;
(4) assay of jasminoidin: prepare need testing solution and reference substance solution respectively, use high effective liquid chromatography for measuring;
Reference substance is: jasminoidin;
Chromatographic condition and system suitability are: be filler with the octadecylsilane chemically bonded silica; Second eyeball-redistilled water is a mobile 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%; Ultra-violet monitor, the detection wavelength is 238nm, number of theoretical plate calculates by the jasminoidin peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of to take by weighing the jasminoidin reference substance, adds methanol and makes the reference substance solution that every 1ml contains 15 μ g jasminoidins;
The preparation of need testing solution: get 8～20 of diligent those sub-sheets of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize is got 0.1g, it is fixed to claim, puts in the tool plug conical flask, adds methanol 25ml, close plug, it is fixed to claim, supersound process 15～30 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, measure filtrate 10ml, put in the 25ml measuring bottle, add methanol to scale, shake up, promptly; The power of supersound process is 250w, and frequency is 25KHz;
Algoscopy: draw each 10 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid, measure, calculate, promptly.
2. the prostatitic Chinese medicine quality detection method of a kind of treatment according to claim 1 is characterized in that, may further comprise the steps:
(1) gets diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize, add water 50ml, supersound process 20 minutes is put coldly, filters, the n-butyl alcohol jolting that filtrate water is saturated is extracted 2 times, each 20ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 1ml dissolving, makes need testing solution; Other gets Fructus Mori control medicinal material 5g, add mass concentration and be 60% alcoholic solution 30ml, reflux 1 hour filters, and filtrate is concentrated into does not have the alcohol flavor, extract 2 times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 1ml dissolving, makes Fructus Mori control medicinal material solution; According to the thin layer chromatography test, draw each 5 μ l of need testing solution and Fructus Mori control medicinal material solution, put respectively on same silica gel g thin-layer plate, with percent by volume is that the upper solution of 15: 1: 4 ethyl acetate, glacial acetic acid and water is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of Fructus Mori control medicinal material chromatograph on, show identical blue-fluorescence speckle, spray is with phosphomolybdic acid ethanol test solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of Fructus Mori control medicinal material chromatograph on, show the speckle of same color;
(2) get Fructus Gardeniae control medicinal material 5g, add mass concentration and be 70% ethanol 30ml, reflux, extract, 1 hour filters, and evaporate to dryness in the filtrate water-bath, residue add methanol 1ml dissolving, make Fructus Gardeniae control medicinal material solution; Other gets the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains the 2mg jasminoidin, as the jasminoidin reference substance solution; Test according to thin layer chromatography, draw in Fructus Gardeniae control medicinal material solution, jasminoidin 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 developing solvent, launch, take out, dry, spray is with phosphomolybdic acid ethanol test solution, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with Fructus Gardeniae control medicinal material and the corresponding position of jasminoidin reference substance chromatograph on, show the speckle of same color;
(3) get diligent those the sub-sheet 2g of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize adds the hydrochloric acid 20ml of 2mol/L, put in the water-bath heating hydrolysis 3 hours, put coldly, add 60～90 ℃ of petroleum ether 30ml, reflux, extract, 1 hour, divide and get petroleum ether liquid, water bath method, residue is made need testing solution with chloroform 3ml dissolving; Other gets the diosgenin reference substance, adds chloroform and makes the solution that every 1ml contains the 1mg diosgenin, as the diosgenin reference substance solution; Test according to thin layer chromatography, drawing each 5 μ l of need testing solution and diosgenin reference substance solution, put respectively on same silica gel g thin-layer plate, is that 93: 7 chloroform and acetone soln is developing solvent with percent by volume, launch, take out, dry, spray is with phosphomolybdic acid ethanol test solution, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with the corresponding position of diosgenin reference substance chromatograph on, show the speckle of same color;
(4) assay of jasminoidin: prepare need testing solution and reference substance solution respectively, use high effective liquid chromatography for measuring;
Reference substance is: jasminoidin;
Chromatographic condition and system suitability are: be filler with the octadecylsilane chemically bonded silica; Second eyeball-redistilled water is a mobile 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%; Ultra-violet monitor, the detection wavelength is 238nm, number of theoretical plate calculates by the jasminoidin peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of to take by weighing the jasminoidin reference substance, adds methanol and makes the reference substance solution that every 1ml contains 15 μ g jasminoidins;
The preparation of need testing solution: get 8 of diligent those sub-sheets of treatment prostatitis medicine-Xi Payimai, remove film-coat, porphyrize is got 0.1g, it is fixed to claim, puts in the tool plug conical flask, adds methanol 25ml, close plug, it is fixed to claim, supersound process 20 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, measure filtrate 10ml, put in the 25ml measuring bottle, add methanol to scale, shake up, promptly; The power of supersound process is 250w, and frequency is 25KHz;
Algoscopy: draw each 10 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid, measure, calculate, promptly.
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| CN105709014A (en) * | 2016-04-06 | 2016-06-29 | 陕西东泰制药有限公司 | Traditional Chinese medicine composition for treating prostatitis and prostatic hyperplasia and preparation method of traditional Chinese medicine composition |
| CN107228833A (en) * | 2017-04-21 | 2017-10-03 | 东莞微领生物科技有限公司 | A kind of total saponin of sapindusmukerossi quick detection kit and detection method |
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| CN101361885A (en) * | 2008-10-09 | 2009-02-11 | 陕西东泰制药有限公司 | Chinese traditional medicine composition for treating the prostatitis and preparation method thereof |
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| CN101037460A (en) * | 2007-04-06 | 2007-09-19 | 福州大学 | Isolation and purification method of geniposide |
| CN101361885A (en) * | 2008-10-09 | 2009-02-11 | 陕西东泰制药有限公司 | Chinese traditional medicine composition for treating the prostatitis and preparation method thereof |
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| CN105709014A (en) * | 2016-04-06 | 2016-06-29 | 陕西东泰制药有限公司 | Traditional Chinese medicine composition for treating prostatitis and prostatic hyperplasia and preparation method of traditional Chinese medicine composition |
| CN107228833A (en) * | 2017-04-21 | 2017-10-03 | 东莞微领生物科技有限公司 | A kind of total saponin of sapindusmukerossi quick detection kit and detection method |
| CN107228833B (en) * | 2017-04-21 | 2020-07-17 | 东莞微领生物科技有限公司 | Rapid detection kit and detection method for total saponins of soapberry |
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