CN102119985A - Quality control method of gout treating tablet - Google Patents
Quality control method of gout treating tablet Download PDFInfo
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- CN102119985A CN102119985A CN 201110005524 CN201110005524A CN102119985A CN 102119985 A CN102119985 A CN 102119985A CN 201110005524 CN201110005524 CN 201110005524 CN 201110005524 A CN201110005524 A CN 201110005524A CN 102119985 A CN102119985 A CN 102119985A
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Abstract
The invention discloses a quality control method of a gout treating tablet, which comprises the steps of experiment on chromatographic conditions and system suitability, preparation of reference substance solution and preparation of test article solution, and comprises the following concrete steps of: taking about 2g of the gout treating tablet; precisely adding 25ml of methanol; carrying out heating reflux for 30 minutes; cooling; weighing; complementing the weight loss with methanol; shaking uniformly; filtering; precisely weighing 2ml of subsequent filtrate; putting into a 50ml round bottom flask; volatilizing the methanol; adding 10ml of sulfuric acid solution the concentration of which is 2.5mol/L; carrying out ultrasonic treatment for 5 minutes; adding 10ml of chloroform; carrying out heating reflux for 1 hour; respectively taking the chloroform solutions; extracting the acid solution twice with chloroform in a shaking way; mixing the chloroform solutions; dehydrating; volatilizing the chloroform; precisely adding 10ml of methanol into the residues; slightly heating for dissolving; cooling; complementing the weight loss with methanol; shaking uniformly; filtering; taking the subsequent filtrate; precisely sucking 20mul of reference substance solution and 20mul of test article solution respectively; injecting into a liquid chromatograph; and measuring. The invention not only can ensure the drug effect of products but also can stabilize the quality of products.
Description
Technical field
The invention belongs to the field of quality control of Chinese medicine preparation, particularly the method for quality control of gout relaxing tablet.
Background technology
Gout relaxing tablet is made up of Radix Et Rhizoma Rhei, Semen Plantaginis, Rhizoma Alismatis, Radix Cyathulae, Radix Stephaniae Tetrandrae five tastes medicine, has heat clearing away, dampness removing, and detoxicating functions is used for the goat due to the dampness and heat stasis.Radix Et Rhizoma Rhei is a principal agent in the prescription, is mainly used in eliminating fire and detoxication.And emodin and chrysophanol are one of effective ingredient in the prescription in the Radix Et Rhizoma Rhei, and what of its content directly have influence on the drug effect of product.As the Rhizoma Alismatis and the Radix Glycyrrhizae two flavor medicines of raw material, it is not differentiated then and can the steady quality of product be exerted an influence.Therefore the quality control standard of former gout relaxing tablet is too simple, can not effectively control the quality of product.
Summary of the invention
A kind of drug effect that can guarantee product that the objective of the invention is to overcome above-mentioned shortcoming and provide can make the method for quality control of the gout relaxing tablet of constant product quality again.
The method of quality control of a kind of gout relaxing tablet of the present invention comprises the steps:
(1) chromatographic condition and system suitability experiment: with the octadecylsilane chemically bonded silica is filler; With methanol-0.1% phosphoric acid (85: 15) is mobile phase; The detection wavelength is 254nm.Number of theoretical plate calculates by the emodin peak should be not less than 1500;
(2) preparation of reference substance solution: precision takes by weighing emodin, each is an amount of for the chrysophanol reference substance, adds methanol respectively and makes the solution that 1ml contains emodin 4 μ g, contains chrysophanol 40 μ g, promptly;
(3) preparation of need testing solution: get 20 of this product, remove film-coat, porphyrize is got about 2g, the accurate title, decide, and puts in the tool plug conical flask, accurate methanol 25ml, the close plug of adding, claim to decide weight, reflux 30 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 2ml, puts in the 50ml round-bottomed flask, fling to methanol, add 2.5mol/L sulfuric acid solution 10ml, ultrasonic (power 260w, frequency 40KHz) handled 5 minutes, add chloroform 10ml again, reflux 1 hour, put cold, in the dislocation separatory funnel, with a small amount of chloroform washing container, washing liquid is incorporated in the separatory funnel, divides and gets chloroform liquid, and acid solution is extracted 2 times with the chloroform jolting, each 8ml merges chloroform liquid, uses anhydrous sodium sulfate dehydration, chloroform liquid moves in the 100ml conical flask, flings to chloroform, and the residue precision adds methanol 10ml, claim to decide weight, slight fever makes dissolving, puts cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, get subsequent filtrate, promptly;
(4) accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Every of this product contains Radix Et Rhizoma Rhei with emodin (C
15H
10O
5) and chrysophanol (C
15H
10O
4) the total amount meter, must not be less than 0.30mg.
The method of quality control of above-mentioned gout relaxing tablet also comprises microscopical identification: get this product, put microscopically and observe: the endosperm cell wall thickness is full of tiny aleurone grain.Stone cell is oval or closely square, wall thickness.Calcium oxalate cluster crystal is big, diameter 60~140 μ m.The wavy bending of endodermis cell anticlinal wall, thicker, lignify has sparse microgroove hole.
The method of quality control of above-mentioned gout relaxing tablet comprises that also the thin layer of Radix Et Rhizoma Rhei is differentiated: get 5 of this product, remove film-coat, porphyrize is got 0.3g, adds methanol 20ml, supersound process 10 minutes filters, and gets filtrate 5ml, evaporate to dryness, residue add 2.5mol/L sulfuric acid solution 10ml makes dissolving, adds chloroform 10ml again, reflux 30 minutes, cooling divides and gets chloroform liquid, be concentrated into 1ml, as need testing solution.Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether (60~90 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
The method of quality control of above-mentioned gout relaxing tablet comprises that also the thin layer of Rhizoma Alismatis is differentiated: get this product powder 0.2g, add ethyl acetate 1ml, jolting 3 minutes, centrifugal 15 minutes (3500 rev/mins) get supernatant, add water 0.5ml, jolting 1 minute, standing demix, ethyl acetate layer is as need testing solution.Other gets Rhizoma Alismatis control medicinal material 0.2g, adds ethyl acetate 1ml, hot bath jolting 1 minute, and centrifugal 15 minutes (3500 rev/mins) get supernatant, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-formic acid (3: 1.5: 0.2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ are heated to clear spot.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The method of quality control of above-mentioned gout relaxing tablet comprises that also the thin layer of Radix Cyathulae is differentiated: get 20 of this product, remove film-coat, porphyrize is got 2g, adds methanol 20ml, supersound process 20 minutes filters, and gets filtrate 10ml, evaporate to dryness, residue add 2.5mol/L sulfuric acid solution 10ml, add chloroform 10ml again, reflux 30 minutes is put coldly, divides and to get chloroform liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Other gets Radix Cyathulae control medicinal material 1g, shines medical material solution in pairs with legal system.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol (40: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
The present invention compared with prior art has tangible beneficial effect, by above technical scheme as can be known, comprises the thin layer discrimination method of Radix Et Rhizoma Rhei, Rhizoma Alismatis and Radix Cyathulae, the content assaying method of emodin and chrysophanol.Can measure the content of emodin and chrysophanol, can effectively contain medical materials such as Radix Et Rhizoma Rhei, Rhizoma Alismatis and Radix Cyathulae in the discriminating product again.Can guarantee the drug effect of product, can make constant product quality again, produce, make technology controlling and process rationally strict more, thereby control product quality effectively thereby better instruct.
Description of drawings
Fig. 1: emodin standard curve;
Fig. 2: chrysophanol standard curve;
Fig. 3: emodin, chrysophanol mixing reference substance high-efficient liquid phase chromatogram;
Fig. 4: gout relaxing tablet test sample high-efficient liquid phase chromatogram;
The specific embodiment
The below routine by experiment beneficial effect that further specifies the inventive method.
Experimental example:
(1) linear relationship is investigated
Emodin, chrysophanol mixing contrast solution 20 μ l that precision is measured variable concentrations inject chromatograph of liquid, carry out emodin, chrysophanol mensuration, with emodin, chrysophanol peak area A
Emodin, A
Greatly Yellow phenol, to emodin, chrysophanol concentration C
Emodin, C
ChrysophanolCarry out linear regression, equation of linear regression: A
Emodin=80252C
Emodin-1589, A
Chrysophanol=118109C
Chrysophanol+ 25266, the emodin range of linearity: 0.0200~0.3200 μ g, the chrysophanol range of linearity: 0.2016~3.2256 μ g, emodin correlation coefficient r=0.9999, chrysophanol correlation coefficient r=0.9999, former point equation A is crossed in match
Emodin=80107C
Emodin, A
Chrysophanol=118337C
Chrysophanol, according to experimental result, emodin is in 0.0200~0.3200 μ g scope, and chrysophanol is in 0.2016~3.2256 μ g scope, and peak area and sample size are good linear relationship.。The results are shown in following table and Fig. 1,2.
(2) precision test
Precision is measured emodin, chrysophanol mixes reference substance solution (4 μ g/ml, 40.32 μ g/ml) 20 μ l and injects chromatograph of liquid, repeat sample introduction 5 times, with the calculated by peak area of emodin, chrysophanol, emodin RSD is 0.44%, chrysophanol RSD is 0.18%, the results are shown in following table.
Measure number of times | 1 | 2 | 3 | 4 | 5 | On average | RSD |
The emodin area | 317843 | 318656 | 321257 | 320039 | 318392 | 319237 | 0.44 |
The chrysophanol peak area | 4762083 | 4767557 | 4777311 | 4768272 | 4754159 | 4765876 | 0.18 |
(3) replica test
Get same lot number test sample, prepare 5 parts of need testing solutions according to [assay] method, with the calculated by peak area of emodin, chrysophanol, emodin RSD=1.24%, chrysophanol RSD=1.43%.The results are shown in following table.
(4) stability test
Precision is measured same need testing solution, and according to the form below official hour sample introduction is surveyed 6 times altogether, and with emodin, chrysophanol calculated by peak area, the result shows, test sample in 10h, no significant change before and after emodin, the chrysophanol peak area integrated value.
(5) average recovery test
Get the about 1g of this product, 6 parts, the accurate title, decide, and accurate adding contains emodin 18 μ g/ml, chrysophanol 90 μ g/ml and mixes reference substance solution 25ml, reaches [assay] method according to the test sample processing method, carries out emodin, chrysophanol assay, the results are shown in following table.
Result of the test shows that emodin application of sample average recovery rate is 98.68%, and RSD is 1.15%; Chrysophanol application of sample average recovery rate is 96.00%, and RSD is 1.97%, reaches standard-required, and method is feasible.
(6) three batch sample assays
Press the assay operation, measure the emodin of 3 lot number preparations, the content of chrysophanol, the results are shown in following table.
Embodiment:
The method of quality control of gout relaxing tablet comprises:
1, microscopical identification:
Get this product, put microscopically and observe: the endosperm cell wall thickness is full of tiny aleurone grain.Stone cell is oval or closely square, wall thickness.Calcium oxalate cluster crystal is big, diameter 60~140 μ m.The wavy bending of endodermis cell anticlinal wall, thicker, lignify has sparse microgroove hole.
2, the discriminating of Radix Et Rhizoma Rhei:
Get 5 of this product, remove film-coat, porphyrize, get 0.3g, add methanol 20ml, supersound process 10 minutes, filter, get filtrate 5ml, evaporate to dryness, residue adds 2.5mol/L sulfuric acid solution 10ml makes dissolving, adds chloroform 10ml again, reflux 30 minutes, cooling, divide and get chloroform liquid, be concentrated into 1ml, as need testing solution.Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether (60~90 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
3, the discriminating of Rhizoma Alismatis:
Get this product powder 0.2g, add ethyl acetate 1ml, jolting 3 minutes, centrifugal 15 minutes (3500 rev/mins) get supernatant, add water 0.5ml, jolting 1 minute, standing demix, ethyl acetate layer is as need testing solution.Other gets Rhizoma Alismatis control medicinal material 0.2g, adds ethyl acetate 1ml, hot bath jolting 1 minute, and centrifugal 15 minutes (3500 rev/mins) get supernatant, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-formic acid (3: 1.5: 0.2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ are heated to clear spot.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
2, Radix Cyathulae is differentiated:
Get 20 of this product, remove film-coat, porphyrize, get 2g, add methanol 20ml, supersound process 20 minutes, filter, get filtrate 10ml, evaporate to dryness, residue adds 2.5mol/L sulfuric acid solution 10ml, adds chloroform 10ml again, reflux 30 minutes, put coldly, divide and to get chloroform liquid, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution.Other gets Radix Cyathulae control medicinal material 1g, shines medical material solution in pairs with legal system.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol (40: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
3, the assay of emodin, chrysophanol
(1) chromatographic condition and system suitability experiment: with the octadecylsilane chemically bonded silica is filler; With methanol-0.1% phosphoric acid (85: 15) is mobile phase; The detection wavelength is 254nm.Number of theoretical plate calculates by the emodin peak should be not less than 1500;
(2) preparation of reference substance solution: precision takes by weighing emodin, each is an amount of for the chrysophanol reference substance, adds methanol respectively and makes the solution that 1ml contains emodin 4 μ g, contains chrysophanol 40 μ g, promptly;
(3) preparation of need testing solution: get 20 of this product, remove film-coat, porphyrize is got about 2g, the accurate title, decide, and puts in the tool plug conical flask, accurate methanol 25ml, the close plug of adding, claim to decide weight, reflux 30 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 2ml, puts in the 50ml round-bottomed flask, fling to methanol, add 2.5mol/L sulfuric acid solution 10ml, ultrasonic (power 260w, frequency 40KHz) handled 5 minutes, add chloroform 10ml again, reflux 1 hour, put cold, in the dislocation separatory funnel, with a small amount of chloroform washing container, washing liquid is incorporated in the separatory funnel, divides and gets chloroform liquid, and acid solution is extracted 2 times with the chloroform jolting, each 8ml merges chloroform liquid, uses anhydrous sodium sulfate dehydration, chloroform liquid moves in the 100ml conical flask, flings to chloroform, and the residue precision adds methanol 10ml, claim to decide weight, slight fever makes dissolving, puts cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, get subsequent filtrate, promptly;
(4) accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Every of this product contains Radix Et Rhizoma Rhei with emodin (C
15H
10O
5) and chrysophanol (C
15H
10O
4) the total amount meter, must not be less than 0.30mg.
Claims (6)
1. the method for quality control of a gout relaxing tablet comprises the steps:
(1) chromatographic condition and system suitability experiment: with the octadecylsilane chemically bonded silica is filler; With methanol: 0.1% phosphoric acid=85: 15 is mobile phase; The detection wavelength is 254nm, and number of theoretical plate calculates by the emodin peak should be not less than 1500;
(2) preparation of reference substance solution: precision takes by weighing emodin, each is an amount of for the chrysophanol reference substance, adds methanol respectively and makes the solution that 1ml contains emodin 4 μ g, contains chrysophanol 40 μ g, promptly;
(3) preparation of need testing solution: get 20 of this product, remove film-coat, porphyrize is got about 2g, the accurate title, decide, and puts in the tool plug conical flask, accurate methanol 25ml, the close plug of adding, claim to decide weight, reflux 30 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 2ml, puts in the 50ml round-bottomed flask, fling to methanol, add 2.5mol/L sulfuric acid solution 10ml, power 260w, the supersound process of frequency 40KHz 5 minutes adds chloroform 10ml again, reflux 1 hour, put cold, in the dislocation separatory funnel, with a small amount of chloroform washing container, washing liquid is incorporated in the separatory funnel, divides and gets chloroform liquid, and acid solution is extracted 2 times with the chloroform jolting, each 8ml merges chloroform liquid, uses anhydrous sodium sulfate dehydration, chloroform liquid moves in the 100ml conical flask, flings to chloroform, and the residue precision adds methanol 10ml, claim to decide weight, slight fever makes dissolving, puts cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, get subsequent filtrate, promptly;
(4) accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
2. the method for quality control of gout relaxing tablet as claimed in claim 1, wherein the microscopical identification method is: get this product, put microscopically and observe: the endosperm cell wall thickness is full of tiny aleurone grain, stone cell is oval or closely square, wall thickness, calcium oxalate cluster crystal is big, diameter 60~140 μ m, the wavy bending of endodermis cell anticlinal wall, thicker, lignify has sparse microgroove hole.
3. the method for quality control of gout relaxing tablet as claimed in claim 1, wherein the thin layer discrimination method of Radix Et Rhizoma Rhei is: get 5 of this product, remove film-coat, porphyrize is got 0.3g, adds methanol 20ml, supersound process 10 minutes, filter, get filtrate 5ml, evaporate to dryness, residue adds 2.5mol/L sulfuric acid solution 10ml makes dissolving, add chloroform 10ml again, reflux 30 minutes, cooling, divide and get chloroform liquid, be concentrated into 1ml, as need testing solution, other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shine medical material solution in pairs with legal system, according to the thin layer chromatography test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 60~90 ℃ of petroleum ether: Ethyl formate: the upper solution of formic acid=15: 5: 1 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 control medicinal material chromatograph on, show the fluorescence speckle of same color.
4. the method for quality control of gout relaxing tablet as claimed in claim 1, wherein the thin layer discrimination method of Rhizoma Alismatis is: get this product powder 0.2g, add ethyl acetate 1ml, jolting 3 minutes, rotating speed was 3500 rev/mins in centrifugal 15 minutes, got supernatant, added water 0.5ml, jolting 1 minute, standing demix, ethyl acetate layer are as need testing solution, and other gets Rhizoma Alismatis control medicinal material 0.2g, add ethyl acetate 1ml, hot bath jolting 1 minute, centrifugal 15 minutes, 3500 rev/mins of rotating speeds, get supernatant, medical material solution according to the thin layer chromatography test, is drawn each 5 μ l of above-mentioned two kinds of solution in contrast, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: formic acid=3: 1.5: 0.2 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ are heated to clear spot, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
5. the method for quality control of gout relaxing tablet as claimed in claim 1, wherein the thin layer discrimination method of Radix Cyathulae is: get 20 of this product, remove film-coat, porphyrize is got 2g, adds methanol 20ml, supersound process 20 minutes filters, and gets filtrate 10ml, evaporate to dryness, residue adds 2.5mol/L sulfuric acid solution 10ml, adds chloroform 10ml again, reflux 30 minutes, put cold, divide and get chloroform liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution, other gets Radix Cyathulae control medicinal material 1g, shines medical material solution in pairs with legal system, according to the thin layer chromatography test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: methanol=40: 1 is developing solvent, launches, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
6. the method for quality control of gout relaxing tablet as claimed in claim 1, wherein: every of this product contains the total amount of Radix Et Rhizoma Rhei in emodin and chrysophanol, must not be less than 0.30mg.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1698701A (en) * | 2005-05-13 | 2005-11-23 | 一笑堂(湖南)制药有限公司 | Gout relaxing tablet and preparation method thereof |
CN1706453A (en) * | 2005-05-16 | 2005-12-14 | 广州固志医药科技开发有限公司 | Gout resisting Chinese medicine composition and its prepn process |
CN101167902A (en) * | 2007-11-12 | 2008-04-30 | 修正药业集团股份有限公司 | Method for preparing traditional Chinese medicine preparation for treating gout |
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2011
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Publication number | Priority date | Publication date | Assignee | Title |
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CN1698701A (en) * | 2005-05-13 | 2005-11-23 | 一笑堂(湖南)制药有限公司 | Gout relaxing tablet and preparation method thereof |
CN1706453A (en) * | 2005-05-16 | 2005-12-14 | 广州固志医药科技开发有限公司 | Gout resisting Chinese medicine composition and its prepn process |
CN101167902A (en) * | 2007-11-12 | 2008-04-30 | 修正药业集团股份有限公司 | Method for preparing traditional Chinese medicine preparation for treating gout |
Non-Patent Citations (3)
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《中外健康文摘(医药月刊)》 20070615 李静 痛风舒片的含量测定的方法学研究 , 第06期 2 * |
《国家中成药标准汇编 中成药地方标准上升国家标准部分 经络肢体 脑系分册》 20021231 国家药品监督管理局 痛风舒胶囊 680 , 1 * |
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Application publication date: 20110713 |