CN101274053B - Detection method of capsules for curing waist pain - Google Patents
Detection method of capsules for curing waist pain Download PDFInfo
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- CN101274053B CN101274053B CN2008100845977A CN200810084597A CN101274053B CN 101274053 B CN101274053 B CN 101274053B CN 2008100845977 A CN2008100845977 A CN 2008100845977A CN 200810084597 A CN200810084597 A CN 200810084597A CN 101274053 B CN101274053 B CN 101274053B
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- 239000002775 capsule Substances 0.000 title claims abstract description 44
- 208000002193 Pain Diseases 0.000 title claims abstract description 35
- 238000001514 detection method Methods 0.000 title claims description 9
- 239000000243 solution Substances 0.000 claims description 54
- 238000000034 method Methods 0.000 claims description 44
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 35
- 239000013558 reference substance Substances 0.000 claims description 32
- 238000012360 testing method Methods 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
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- XFSBVAOIAHNAPC-XTHSEXKGSA-N 16-Ethyl-1alpha,6alpha,19beta-trimethoxy-4-(methoxymethyl)-aconitane-3alpha,8,10alpha,11,18alpha-pentol, 8-acetate 10-benzoate Chemical compound O([C@H]1[C@]2(O)C[C@H]3[C@@]45C6[C@@H]([C@@]([C@H]31)(OC(C)=O)[C@@H](O)[C@@H]2OC)[C@H](OC)[C@@H]4[C@]([C@@H](C[C@@H]5OC)O)(COC)CN6CC)C(=O)C1=CC=CC=C1 XFSBVAOIAHNAPC-XTHSEXKGSA-N 0.000 claims description 11
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention relates to a lumbago relieving capsule which can relax tendons and activate collaterals, remove blood stasis, relieve pain, activate blood and remove rheumatism. The lumbago relieving capsule can be applied to rheumatoid arthritis, hypertrophic ixomyelitis, hypertrophic thoracic inflammation, cervical inflammation, sciatica and lumbar muscle strain. Since the lumbago relieving capsule contains toxic kusnezoff monkshood root, carefulness is needed during clinical use. The quality standard of current lumbago relieving capsules cannot totally meet the purpose of drug safety supervision. The lumbago relieving capsule of the invention aims at providing more perfect quality control method from qualitative and rational aspects.
Description
[technical field]
The invention belongs to technical field of Chinese medicines, be specifically related to the method for quality control of capsules for curing waist pain.
[background technology]
The function of capsules for curing waist pain cures mainly and comprises relaxing muscles and tendons and activating QI and blood in the collateral, stasis-dispelling and pain-killing, the wind dispelling of invigorating blood circulation.Be used for rheumatic arthritis, hypertrophy property spondylitis of lumbar vertebra, hypertrophy property thoracic vertebra is scorching, cervical spondylitis, sciatica, lumbar muscle strain.Its usage and dosage is oral, one time 2,3 times on the one, taking medicine after meal.
Capsules for curing waist pain should be noted following 3 clinically:
1, heart disease and the careful clothes of gastrointestinal upset person.
2, if occur feeling sick, vomit, suffer from abdominal pain, feel dizzy, dispute, extremity and whole body are numb, cold syndrome of the stomach, and the platycoria that continues, the dimness of vision, dyspnea, tetany, restless and gatism should be withdrawn, and removes hospital admission rapidly.
3, capsules for curing waist pain should not be in a large number, take for a long time.
The prescription of the capsules for curing waist pain that the present invention relates at present, method for making, shape and discrimination method are following:
[prescription] Radix Angelicae Dahuricae 78 gram Radix Aconiti Kusnezoffii (system) 52 gram Radix Angelicae Pubescentiss 52 grams
Herba Taxilli 26 gram Radix Dipsacis 52 gram Radix Achyranthis Bidentataes 52 grams
Windproof 52 grams of Radix Notoginseng 47 gram Radix Angelicae Sinensis 26 grams
Radix Clematidis 52 gram Radix Gentianae Macrophyllae 52 gram Rhizoma Drynariae 26 grams
River Cortex Acanthopanacis Radicis 52 gram Radix Stephaniae Tetrandrae 78 gram Caulis Piperis Kadsuraes 52 grams
The Flos Carthami 52 gram Cortexs Eucommiae 46 gram Tu Rhizoma Dioscoreae Septemlobae 26 grams
Radix Polygoni Multiflori 46 gram Rhizoma Homalomenaes 52 gram Radix Paeoniae Rubra 78 grams
Ramulus Cinnamomi 52 gram acetaminophen 100 grams
[method for making] above 23 flavors except that acetaminophen, are got Radix Angelicae Sinensis, Radix Notoginseng and the Radix Angelicae Dahuricae 39 grams, Radix Aconiti Kusnezoffii Preparata 26 grams are ground into coarse powder, 18 flavors such as the residue Radix Angelicae Dahuricae, Radix Aconiti Kusnezoffii Preparata and all the other Radix Angelicae Pubescentiss; The decocte with water secondary, collecting decoction filters, and filtrating is concentrated into the thick paste that relative density is 1.3～1.35 (80 ℃ of surveys); With above-mentioned coarse powder mix homogeneously, oven dry is ground into fine powder, adds acetaminophen; Mixing incapsulates, and processes 1000, promptly gets.
[character] capsules for curing waist pain is a capsule, and content is the powder of taupe brown; Bitter in the mouth, sweet.
Capsules for curing waist pain is got in [discriminating] (1), puts microscopically and observes: stone cell is single be dispersed in or 2-5 in groups, type square, rectangle or ellipse, cell is big, wall is thick slightly, pit is obvious, accidental in the cell have a starch grain.The resin canal fragment is yellow, and diameter 60-128 micron contains in the tract and drips shape or block secretions.
(2) get capsules for curing waist pain content 0.6 gram, put in 50 milliliters of conical flasks, add 20 milliliters of dehydrated alcohol; Little boiling 3 minutes in water-bath filters, and filtrating is waved most ethanol; Add 10 milliliters of dilute hydrochloric acid, put in the water-bath and heated 30 minutes, put cold; Add 0.1mol/L sodium nitrite liquid number droplet, add alkaline betanaphthol test solution number droplet, promptly generate the scarlet deposition.
(3) get capsules for curing waist pain content 3 grams, add diethyl ether 30 milliliters and flooded 1 hour, jolting constantly, ether inclines; Residue volatilizes ether, adds 30 milliliters of supersound process of methanol 30 minutes, filters the filtrating evaporate to dryness; Residue adds water makes dissolving for 30 milliliters, extracts 2 times with water saturated n-butyl alcohol jolting, each 30 milliliters, merges n-butanol extracting liquid; With 50 milliliters of washings of ammonia solution, n-butanol layer is obtained in 50 milliliters of washings of water that n-butanol layer reuse n-butyl alcohol is saturated; Evaporate to dryness, residue add methanol makes dissolving for 1 milliliter, as need testing solution.
Other gets the ginsenoside Rg
1Reference substance is an amount of, adds methanol and processes per 1 milliliter of solution that contains 1 milligram, as reference substance solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; (15: 40: 22: 10) 10 ℃ of lower floor's solution with held were developing solvent with chloroform-ethyl acetate-methanol-water; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear under 105 ℃, to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(4) get capsules for curing waist pain content 5 grams, add diethyl ether 30 milliliters, water-bath refluxed 1 hour, filtered, and filtrating volatilizes, and residue adds ethyl acetate makes dissolving for 1 milliliter, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 0.5 gram, shines medical material solution in pairs with legal system.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 5 microlitre of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; With normal hexane-ethyl acetate (9: 1) is developing solvent, launches, and takes out; Dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph; With control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
The present invention relates to the Radix Aconiti Kusnezoffii that capsule contains is the tuber of ranunculaceae plant Aconitum kusnezoffii Reichb Aconitumkusnezoffii Reichb., contains aconitine (aconitine) and atisine alkali toxic alkaloids such as (atisine).All contain multiple alkaloid in the Radix Aconiti Kusnezoffii, its mesaconitine toxicity is maximum.Its toxicity shows as follows:
1. vascular system: uncomfortable in chest, cardiopalmus; Blood pressure drops (even can not surveying) and various types of arrhythmia; Comprise that sinus tachycardia, Dou Xingting are rich, atrial fibrillation, polyphyly ventricular premature contraction, the ventricular premature contraction that takes place frequently are premature ventricular beat, premature ventricular beat, ventricular tachycardia, chamber quiver, the conduction block of room property, left bundle branch block; And it is can cause shock, even dead.
2. nervous system: teleneuron and central nervous system are all had excited earlier back inhibitory action.Show as dispute, extremity and total numbness, oral cavity or whole body burn feeling, dizzy, pale complexion are perspired, extreme cold of the limbs, dysphoria, tic of the limbs is tetanic then, and is drowsiness, delirium, obnubilation.Quadriplegia appears in indivedual cases.
3. digestive system: sialorrhea, dysphagia, nausea and vomiting, even spit out white foams, or vomiting coffee appearance gastric content, separate the black loose stool; Stomachache, diarrhoea, tenesmus, the performance of similar dysentery.There is report to cause toxic hepatitis secondary cirrhotic ascites.
4. respiratory system: breathe hard, dyspnea, cyanosis etc. finally can be dead because of respiratory paralysis.
5. urinary system: oliguria, dysuria, urine retention, even acute renal failure.
Thereby the aconitine content in the control finished capsule product is extremely important.The quality standard of at present existing capsules for curing waist pain is only with its quality of microscopical identification method control; Reason at aspects such as experimental check or processing; Sometimes the microscopic features of indivedual medical material tissues can't be seen, are difficult to its down fixed against regulation judgement, because Radix Aconiti Kusnezoffii is hypertoxic medicine; The index components aconitine does not have suitable detection method in the finished capsule product, and does not have detection method qualitatively in the quality standard yet; This all is the deficiency in the current standard.
Originally have only qualitative method in the quality standard of capsules for curing waist pain, do not have quantitative analytical method, this also is a deficiency that exists at present.
[summary of the invention]
The object of the present invention is to provide control capsules for curing waist pain mesaconitine qualitative method and and the quantitative method of quality control of peoniflorin.
Method of quality control particularly of the present invention is: get capsules for curing waist pain content 6.0 grams, put in 500 milliliters of tool plug conical flasks, add 60 milliliters of strong ammonia solutions, make moistening; Add diethyl ether 200 milliliters, supersound process 40 minutes is put coldly, obtains ether solution; Volatilize, residue adds dehydrated alcohol to be made dissolving and is settled to 2 milliliters, and as need testing solution, it is an amount of that precision takes by weighing the aconitine reference substance in addition; Add dehydrated alcohol and process per 1 milliliter of solution that contains 1 milligram, as reference substance solution, according to the test of an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography; Draw each 5 microlitre of above-mentioned need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with ethyl acetate-acetone-strong ammonia solution (40: 2: 0.3); Launch, take out, dry; Spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on the speckle that occurs should be less than the speckle of reference substance.
Method of quality control particularly of the present invention is: get capsules for curing waist pain content 6.0 grams, put in 500 milliliters of tool plug conical flasks, add 60 milliliters of strong ammonia solutions, make moistening; Add diethyl ether 200 milliliters, supersound process 40 minutes is put coldly, obtains ether solution; Volatilize, residue adds dehydrated alcohol to be made dissolving and is settled to 2 milliliters, as need testing solution; It is an amount of that precision takes by weighing the aconitine reference substance in addition, adds dehydrated alcohol and process per 1 milliliter of solution that contains 1 milligram, as reference substance solution; According to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography test, draw respectively 5 microlitres of above-mentioned need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; Be made into developing solvent with ethyl acetate-acetone-strong ammonia solution according to 40: 2: 0.3 ratio, launch, take out; Dry, spray does not occur speckle with rare bismuth potassium iodide test solution on the corresponding position of chromatograph.
Above-mentioned method of quality control also adopts following method:
Every of the capsules for curing waist pain that the present invention relates to contains Radix Paeoniae Rubra with peoniflorin (C
23H
28O
11) meter be no less than 0.3 milligram.
Above-mentioned method of quality control preferably adopts following method:
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; Acetonitrile-0.05% phosphate aqueous solution (14: 86) is a mobile phase, detects wavelength 230nm, flow velocity: 1.0 ml/min; Number of theoretical plate is pressed the peoniflorin peak and is calculated, and should be not less than 3000.
The preparation of reference substance solution: the peoniflorin reference substance of getting drying under reduced pressure to constant weight is an amount of, and accurate the title decides, and adds 50% methanol and processes per 1 milliliter of solution that contains 60 micrograms, promptly gets.
The preparation of need testing solution: the content of getting under the capsules for curing waist pain content uniformity item is an amount of, and porphyrize is got about 3 grams, and accurate the title decides, and puts in the tool plug conical flask.Precision adds 50 milliliters of 50% methanol, and close plug claims to decide weight.Ultrasonic (power 200W, frequency 26.5KHz) handled 30 minutes, put coldly, claimed decide weight, added 50% methanol and supplied and subtract weight loss, shook up, and filtration promptly gets.
Algoscopy: accurate respectively reference substance solution and each 10 microlitre of need testing solution drawn, inject chromatograph of liquid, measure, promptly get.
Method of quality control of the present invention provides the qualitative checking method of the relevant aconitine of capsules for curing waist pain; Be this rheumatic arthritis that is widely used in, hypertrophy property spondylitis of lumbar vertebra, hypertrophy property thoracic vertebra is scorching; Cervical spondylitis; Sciatica, the medicine of lumbar muscle strain provides authentication method more safely and effectively, for medicine actual production, field of circulation quality monitoring and clinical practice provide effective guarantee.
In addition, method of quality control of the present invention also provides the quantitative detecting method of capsules for curing waist pain first, is this rheumatic arthritis that is widely used in; Hypertrophy property spondylitis of lumbar vertebra; Hypertrophy property thoracic vertebra is scorching, cervical spondylitis, sciatica; The medicine of lumbar muscle strain provides authentication method more safely and effectively, for medicine actual production, field of circulation quality monitoring and clinical practice provide effective guarantee.
[specific embodiment]
Experimental example 1
The capsules for curing waist pain of 5 lot numbers of random choose (lot number is: 20070712-1,20070824-1,20070911-1,20071015-1,20071112-1).
Get the capsular content 6.0g of above 5 lot numbers, put in 500 milliliters of tool plug conical flasks, add 60 milliliters of strong ammonia solutions, make moistening; Add diethyl ether 200 milliliters, supersound process 40 minutes is put coldly, obtains ether solution; Volatilize, residue adds dehydrated alcohol to be made dissolving and is settled to 2 milliliters, as need testing solution.It is an amount of that precision takes by weighing the aconitine reference substance in addition, adds dehydrated alcohol and process per 1 milliliter of solution that contains 1 milligram, as reference substance solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005); Draw each 5 microlitre of above-mentioned need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with ethyl acetate-acetone-strong ammonia solution (40: 2: 0.3); Launch; Take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on the speckle that occurs should or speckle appear less than the speckle of reference substance.Concrete experimental result sees the following form 1.
The testing result of table 1 capsules for curing waist pain mesaconitine
Method of quality control of the present invention provides the qualitative checking method of the relevant aconitine of capsules for curing waist pain; Be this rheumatic arthritis that is widely used in, hypertrophy property spondylitis of lumbar vertebra, hypertrophy property thoracic vertebra is scorching; Cervical spondylitis; Sciatica, the medicine of lumbar muscle strain provides authentication method more safely and effectively, for medicine actual production, field of circulation quality monitoring and clinical practice provide effective guarantee.
Experimental example 2
The capsules for curing waist pain of 5 lot numbers of random choose (lot number is: 20070712-1,20070824-1,20070911-1,20071015-1,20071112-1).
Measure according to HPLC (Chinese Pharmacopoeia version appendix in 2005 VID).
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filler; Acetonitrile-0.05% phosphate aqueous solution (14: 86) is a mobile phase, detects wavelength 230nm, flow velocity: 1.0 ml/min; Number of theoretical plate is pressed the peoniflorin peak and is calculated, and should be not less than 3000.
It is an amount of that the peoniflorin reference substance of drying under reduced pressure to constant weight is got in the preparation of reference substance solution, accurately claims surely, adds 50% methanol and process per 1 milliliter of solution that contains 60 micrograms, promptly gets.
The content that the preparation of need testing solution is got under the capsules for curing waist pain content uniformity item is an amount of, and porphyrize is got about 3g, and accurate the title decides, and puts in the tool plug conical flask.Precision adds 50 milliliters of 50% methanol, and close plug claims to decide weight.Ultrasonic (power 200W, frequency 26.5KHz) handled 30 minutes, put coldly, claimed decide weight, added 50% methanol and supplied and subtract weight loss, shook up, and filtration promptly gets.
Accurate respectively reference substance solution and each 10 microlitre of need testing solution drawn of algoscopy inject chromatograph of liquid, measure, and promptly get.Concrete experimental data sees the following form 2.
The testing result of peoniflorin in table 2 capsules for curing waist pain
Method of quality control of the present invention provides the quantitative detecting method of capsules for curing waist pain first; Be this rheumatic arthritis that is widely used in, hypertrophy property spondylitis of lumbar vertebra, hypertrophy property thoracic vertebra is scorching; Cervical spondylitis; Sciatica, the medicine of lumbar muscle strain provides authentication method more safely and effectively, for medicine actual production, field of circulation quality monitoring and clinical practice provide effective guarantee.
Claims (5)
1. the detection method of a capsules for curing waist pain is characterized in that adopting following method: get capsules for curing waist pain content 6.0 grams, put in 500 milliliters of tool plug conical flasks, add 60 milliliters of strong ammonia solutions; Make moisteningly, add diethyl ether 200 milliliters, supersound process 40 minutes is put cold; Obtain ether solution, volatilize, residue adds dehydrated alcohol to be made dissolving and is settled to 2 milliliters, as need testing solution; It is an amount of that precision takes by weighing the aconitine reference substance in addition, adds dehydrated alcohol and process per 1 milliliter of solution that contains 1 milligram, as reference substance solution; According to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography test, draw respectively 5 microlitres of above-mentioned need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; Be made into developing solvent with ethyl acetate-acetone-strong ammonia solution according to 40: 2: 0.3 ratio, launch, take out; Dry, spray is with rare bismuth potassium iodide test solution, and the speckle that on the corresponding position of chromatograph, occurs is less than the speckle of reference substance.
2. the detection method of a capsules for curing waist pain is characterized in that adopting following method: get capsules for curing waist pain content 6.0 grams, put in 500 milliliters of tool plug conical flasks, add 60 milliliters of strong ammonia solutions; Make moisteningly, add diethyl ether 200 milliliters, supersound process 40 minutes is put cold; Obtain ether solution, volatilize, residue adds dehydrated alcohol to be made dissolving and is settled to 2 milliliters, as need testing solution; It is an amount of that precision takes by weighing the aconitine reference substance in addition, adds dehydrated alcohol and process per 1 milliliter of solution that contains 1 milligram, as reference substance solution; According to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography test, draw respectively 5 microlitres of above-mentioned need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; Be made into developing solvent with ethyl acetate-acetone-strong ammonia solution according to 40: 2: 0.3 ratio, launch, take out; Dry, spray does not occur speckle with rare bismuth potassium iodide test solution on the corresponding position of chromatograph.
3. according to claim 1 or 2 arbitrary described detection methods, it is characterized in that peoniflorin is no less than 0.3 milligram in the every capsules of said capsules for curing waist pain.
4. detection method according to claim 3 is characterized in that said peoniflorin adopts high effective liquid chromatography for measuring.
5. detection method according to claim 4 is characterized in that the method for said HPLC is:
Use octadecylsilane chemically bonded silica to be filler, acetonitrile-0.05% phosphate aqueous solution is made into mobile phase according to 14: 86 ratio, detects wavelength 230nm, flow velocity: 1.0 ml/min, number of theoretical plate are pressed the peoniflorin peak and are calculated, and should be not less than 3000;
The preparation of reference substance solution, the peoniflorin reference substance of getting drying under reduced pressure to constant weight is an amount of, and accurate the title, decide, and adds 50% methanol and process per 1 milliliter of solution that contains 60 micrograms;
The preparation of need testing solution, the content of getting under the capsules for curing waist pain content uniformity item is an amount of, and porphyrize is got about 3 grams, and accurate the title, decide, and puts in the tool plug conical flask; Precision adds 50 milliliters of 50% methanol, and close plug claims to decide weight; Supersound process 30 minutes is put coldly, claims decide weight, adds 50% methanol and supplies and subtract weight loss, shakes up filtration;
Algoscopy, accurate respectively reference substance solution and each 10 microlitre of need testing solution drawn inject chromatograph of liquid, measure.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1813953A (en) * | 2005-12-02 | 2006-08-09 | 王衡新 | Chinese medicine formulation for promoting blood circulation to arrest pain, and its preparing method and quality control method |
| CN101199677A (en) * | 2007-11-20 | 2008-06-18 | 广西万寿堂药业有限公司 | Chinese medicine agent for treating injuries from falls, rheumatoid arthritis and preparing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1813953A (en) * | 2005-12-02 | 2006-08-09 | 王衡新 | Chinese medicine formulation for promoting blood circulation to arrest pain, and its preparing method and quality control method |
| CN101199677A (en) * | 2007-11-20 | 2008-06-18 | 广西万寿堂药业有限公司 | Chinese medicine agent for treating injuries from falls, rheumatoid arthritis and preparing method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 王绪等.高效液相色谱法测定腰息痛胶囊中对乙酰氨基酚的含量.《辽宁中医杂志》.2007,第34卷(第06期), * |
| 黄玮.HPLC法测定腰息痛胶囊中对乙酰氨基酚的含量.《西北药学杂志》.2007,第22卷(第02期), * |
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