CN101028354A - Quality controlling method of siegesbeckia orientalis tablets - Google Patents
Quality controlling method of siegesbeckia orientalis tablets Download PDFInfo
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Abstract
A quality control method for Chinese medicine 'Rheumatic Xixian' tablet prepared from 6 Chinese-medicinal materials including glandularstalk St. paulswort herb, mulberry mistletoe, clematis root, tetrandra root, etc features that the high-effect liquid-phase chromatography is used to test the content of C20H34O4 and the thin-layer chromatography is used for the determination of mulberry mistletoe, clematis root and tetrandra root.
Description
Technical field
The present invention relates to the method for quality control of Herba Siegesbeckiae tablet for rheumatism in the 2nd in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation).
Technical background
Has the quadriplegia of being used in second in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation), weakness of the waist and knees, hemiplegia, the rubella eczema, the Yao Wu Herba Siegesbeckiae tablet for rheumatism of arthralgia and rheumatic arthritis effect, this compound preparation is made up of Zhong Yao Cai Herba Siegesbeckiae 200g, Herba Taxilli 150g, Ramulus Mori 150g, Radix Clematidis 150g, Radix Stephaniae Tetrandrae 100g, Rumalus sophorae 100g, and above-mentioned raw materials is made 1000 altogether.Main flavour of a drug in the Herba Siegesbeckiae side of being, dry aerial parts for composite family Zhi Wu Herba Siegesbeckiae Siegesbeckiaorientalis L., Herba Siegesbeckiae Siegesbeckia pubescens Malino or siegesbeckia glabrescens Makino Siegesbeckia glabrescens Malino, has wind-damp dispelling, sharp joint, the effect of detoxifcation.Herba Taxilli is the dry stem and branch with leaf of Loranthaceae plant Herba Taxilli Taxiluschinensis (DC.) Danser, has invigorating the liver and kidney, bone and muscle strengthening, the effect of wind-damp dispelling; Ramulus Mori is the dry twig of moraceae plants Mulberry Morus alba L., has wind-damp dispelling, the effect in sharp joint.Radix Clematidis is the dry root and rhizome of cohosh Radix Clematidis Clematis chinensisOsbeck, Clematis hexapetala Clematis hexapetala Pall. or northeast clematis Clematis manshurica Rupr., has expelling wind and removing dampness, the effect of removing obstruction in the collateral to relieve pain; Radix Stephaniae Tetrandrae is the dry root of menispermaceous plants Radix stephaniae tetrandrae Stephania tetrandra S.Moore, has inducing diuresis to remove edema, the wind-expelling pain-stopping effect; Rumalus sophorae is the dry stem of leguminous plant Chinese scholartree Sophorajaponica L., has the effect of expelling wind and removing dampness, hemostasis heat-clearing and toxic substances removing.
Second quality control standard of issuing Herba Siegesbeckiae tablet for rheumatism of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation), but has only physicochemical identification in the Xian You Herba Siegesbeckiae tablet for rheumatism method of quality control that Ministry of Public Health is issued, limitation is very big, is difficult to the quality of accurate Kong Zhi Herba Siegesbeckiae tablet for rheumatism; The present invention is the quality control standard that overcomes the deficiencies in the prior art Ti Gao Herba Siegesbeckiae tablet for rheumatism, set up formulation content testing index and detection method thereof, increase the thin layer chromatography qualitative identification method of its Chinese crude drug Herba Taxilli, Radix Clematidis, Radix Stephaniae Tetrandrae, guaranteed this compound preparation higher quality standard level.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, formulate the method for quality control of Xin De Herba Siegesbeckiae tablet for rheumatism, utilize the content of kirenol in this compound preparation of high effective liquid chromatography for measuring; The thin layer chromatography that increases this compound preparation Chinese crude drug Herba Taxilli, Radix Clematidis, Radix Stephaniae Tetrandrae is differentiated, has guaranteed the accuracy and the advance of quality determining method, can You imitates the product quality of ground Kong Zhi Herba Siegesbeckiae tablet for rheumatism.
The present invention is achieved by following technical proposals:
The quality control detection method that Herba Siegesbeckiae tablet for rheumatism is new, this method comprises following determination step:
1. (an appendix VID of Chinese Pharmacopoeia version in 2000) Ce is Dinged kirenol (C in the Herba Siegesbeckiae tablet for rheumatism with high performance liquid chromatography
20H
34O
4) content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Acetonitrile-water (25: 75) solution is mobile phase, and the detection wavelength is 215 ± 2nm.
B. reference substance solution preparation: precision takes by weighing through the exsiccant kirenol reference substance of phosphorus pentoxide 5-12.5mg, puts in the 10-25ml measuring bottle, adds methanol and is diluted to scale, shakes up, and makes the solution that every 1ml contains 0.5mg.
C. the preparation of need testing solution: get 20 of this product, porphyrize, precision takes by weighing 5g, puts in the apparatus,Soxhlet's, add petroleum ether (60-90 ℃) 100ml, reflux, extract, 3 hours is taken out filtration paper cylinder, volatilize solvent, put in the conical flask, the accurate methanol 50ml that adds, claim to decide weight, reflux 2 hours is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter with 0.45 μ m filter membrane, get subsequent filtrate, promptly.
D. the content assaying method of kirenol: accurate respectively each the 20 μ l of reference substance solution and need testing solution that draw, inject chromatograph of liquid, the content of mensuration kirenol.
E. this film Han Herba Siegesbeckiae is with kirenol (C
20H
34O
4) meter, must not be less than 0.1mg.
2. this medicine Chinese crude drug Herba Taxilli is differentiated with thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005):
Get 5 of this product, porphyrize takes by weighing fine powder 7.5g, add methanol-water (1: 1) 60ml, reflux 1 hour, filtered while hot, after filtrate is concentrated into about 20ml, add water 10ml, add the about 0.5ml of dilute sulfuric acid again, behind the boiling reflux 1 hour, extract 2 times each 30ml, combined ethyl acetate liquid with the ethyl acetate jolting, be concentrated into about 1ml, as need testing solution.Other gets the Quercetin reference substance and adds the solution that the every 1ml of ethyl acetate contains 0.5mg, product solution in contrast.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on the silica gel g thin-layer plate of same usefulness 0.5% sodium hydroxide solution preparation, is developing solvent with toluene (water saturation)-Ethyl formate-formic acid (5: 4: 1), launch, take out, dry, spray is with 5% aluminum chloride alcoholic solution, put under the uviol lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
3. this medicine Chinese crude drug Radix Clematidis is differentiated with thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005):
Get 5 of this product, porphyrize takes by weighing fine powder 1.75g, add ethanol 50ml, reflux 2 hours filters, filtrate is concentrated into about 20ml, adds hydrochloric acid 3ml, reflux 1 hour, add water 10ml, put coldly, add petroleum ether (60～90 ℃) jolting and extract, the petroleum ether evaporate to dryness, residue is with dehydrated alcohol 10ml dissolving, as need testing solution.Other evens up pier fruit acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.45mg, in contrast product solution.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 3 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (20: 3: 0.2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 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.
4. this medicine Chinese crude drug Radix Stephaniae Tetrandrae is differentiated with thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005):
Get 5 of this product, porphyrize takes by weighing fine powder 1.5g, adds ethanol 15ml, and reflux 1 hour is put coldly, filters, and filtrate evaporate to dryness, residue add ethanol 5ml makes dissolving, as need testing solution.Other gets tetrandrine reference substance, fangchinoline reference substance, adds chloroform and makes the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (25: 5: 4: 0.20) be developing solvent, expansion was taken out with chloroform-acetone-methanol-ammonia, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
5. according to the method for quality control of the Herba Siegesbeckiae tablet for rheumatism of being stated, it is characterized in that: this medicine is the weight specification by Herba Siegesbeckiae tablet for rheumatism in the 2nd in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation), the tablet of every weight 0.2g.
Claims (1)
- The method of quality control of Yi Zhong Herba Siegesbeckiae tablet for rheumatism, wherein said pharmaceutical formulation is made up of Zhong Yao Cai Herba Siegesbeckiae 200g, Herba Taxilli 150g, Ramulus Mori 150g, Radix Clematidis 150g, Radix Stephaniae Tetrandrae 100g, Rumalus sophorae 100g, above-mentioned raw materials is made 1000 altogether, it is characterized in that this method comprises the following steps:(1) measures kirenol (C in this medicine with high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005) 20H 34O 4) content:A. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Acetonitrile-water (25: 75) solution is mobile phase, and the detection wavelength is 215 ± 2nm.B. reference substance solution preparation: precision takes by weighing through the exsiccant kirenol reference substance of phosphorus pentoxide 5-12.5mg, puts in the 10-25ml measuring bottle, adds methanol and is diluted to scale, shakes up, and makes the solution that every 1ml contains 0.5mg.C. the preparation of need testing solution: get 20 of this product, porphyrize, precision takes by weighing 5g, puts in the apparatus,Soxhlet's, add petroleum ether (60-90 ℃) 100ml, reflux, extract, 3 hours is taken out filtration paper cylinder, volatilize solvent, put in the conical flask, the accurate methanol 50ml that adds, claim to decide weight, reflux 2 hours is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter with 0.45 μ m filter membrane, get subsequent filtrate, promptly.D. the content assaying method of kirenol: accurate respectively each the 20 μ l of reference substance solution and need testing solution that draw, inject chromatograph of liquid, the content of mensuration kirenol.E. this film Han Herba Siegesbeckiae is with kirenol (C 20H 34O 4) meter, must not be less than 0.1mg.(2) this medicine Chinese crude drug Herba Taxilli is differentiated with thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005):Get 5 of this product, porphyrize takes by weighing fine powder 7.5g, add methanol-water (1: 1) 60ml, reflux 1 hour, filtered while hot, after filtrate is concentrated into about 20ml, add water 10ml, add the about 0.5ml of dilute sulfuric acid again, behind the boiling reflux 1 hour, extract 2 times each 30ml, combined ethyl acetate liquid with the ethyl acetate jolting, be concentrated into about 1ml, as need testing solution.Other gets the Quercetin reference substance and adds ethyl acetate and make the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on the silica gel g thin-layer plate of same usefulness 0.5% sodium hydroxide solution preparation, is developing solvent with toluene (water saturation)-Ethyl formate-formic acid (5: 4: 1), launch, take out, dry, spray is with 5% aluminum chloride alcoholic solution, put under the uviol lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.(3). this medicine Chinese crude drug Radix Clematidis is differentiated with thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005):Get 5 of this product, porphyrize takes by weighing fine powder 1.75g, add ethanol 50ml, reflux 2 hours filters, filtrate is concentrated into about 20ml, adds hydrochloric acid 3ml, reflux 1 hour, add water 10ml, put coldly, add petroleum ether (60～90 ℃) jolting and extract, the petroleum ether evaporate to dryness, residue is with dehydrated alcohol 10ml dissolving, as need testing solution.Other evens up pier fruit acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.45mg, in contrast product solution.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 3 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (20: 3: 0.2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 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.(4). this medicine Chinese crude drug Radix Stephaniae Tetrandrae is differentiated with thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005):Get 5 of this product, porphyrize takes by weighing fine powder 1.5g, adds ethanol 15ml, and reflux 1 hour is put coldly, filters, and filtrate evaporate to dryness, residue add ethanol 5ml makes dissolving, as need testing solution.Other gets tetrandrine reference substance, fangchinoline reference substance, adds chloroform and makes the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (25: 5: 4: 0.20) be developing solvent, expansion was taken out with chloroform-acetone-methanol-ammonia, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.(5). the method for quality control of the Herba Siegesbeckiae tablet for rheumatism of stating according to claim, this medicine are the weight specifications by Herba Siegesbeckiae tablet for rheumatism in the 2nd in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation), the tablet of every weight 0.2g.
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| CN103149320A (en) * | 2013-04-01 | 2013-06-12 | 山西振东开元制药有限公司 | Quality control method of loins-strengthening and kidney-invigorating medicine |
| CN103926330A (en) * | 2013-01-11 | 2014-07-16 | 中国医学科学院药用植物研究所 | Wine fried herba siegesbeckiae detection method |
| CN105004833A (en) * | 2015-05-25 | 2015-10-28 | 贵州百灵企业集团制药股份有限公司 | Detection method for traditional Chinese medicine preparation for treating acute gouty arthritis and gout |
| CN105343209A (en) * | 2015-12-07 | 2016-02-24 | 黑龙江省智诚医药科技有限公司 | Herba siegesbeckiae rheumatism dispersible tablet and preparation method thereof |
| CN108459129A (en) * | 2017-02-17 | 2018-08-28 | 华润三九医药股份有限公司 | A kind of method of quality control of Tetrandra and Poria Decoction composition |
| CN108704014A (en) * | 2018-08-10 | 2018-10-26 | 刘亚飞 | It is a kind of to treat numb in every limb Tea containing traditional Chinese medicine |
| CN109030701A (en) * | 2018-08-20 | 2018-12-18 | 四川新绿色药业科技发展有限公司 | A kind of thin-layer identification method for the control of root of fangji medicinal material, medicine materical crude slice and granule quality |
| CN114053340A (en) * | 2021-12-27 | 2022-02-18 | 吉林吉春制药股份有限公司 | A Chinese medicinal composition for treating rheumatism, and its preparation method |
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| CN103926330A (en) * | 2013-01-11 | 2014-07-16 | 中国医学科学院药用植物研究所 | Wine fried herba siegesbeckiae detection method |
| CN103926330B (en) * | 2013-01-11 | 2015-11-11 | 中国医学科学院药用植物研究所 | A kind of detection method of Jiu Zhi Common St.Paulswort Herb |
| CN103149320A (en) * | 2013-04-01 | 2013-06-12 | 山西振东开元制药有限公司 | Quality control method of loins-strengthening and kidney-invigorating medicine |
| CN105004833A (en) * | 2015-05-25 | 2015-10-28 | 贵州百灵企业集团制药股份有限公司 | Detection method for traditional Chinese medicine preparation for treating acute gouty arthritis and gout |
| CN105004833B (en) * | 2015-05-25 | 2018-07-03 | 贵州百灵企业集团制药股份有限公司 | It is a kind of treat acute gouty arthritis, gout Chinese medicine preparation detection method |
| CN105343209A (en) * | 2015-12-07 | 2016-02-24 | 黑龙江省智诚医药科技有限公司 | Herba siegesbeckiae rheumatism dispersible tablet and preparation method thereof |
| CN108459129A (en) * | 2017-02-17 | 2018-08-28 | 华润三九医药股份有限公司 | A kind of method of quality control of Tetrandra and Poria Decoction composition |
| CN108459129B (en) * | 2017-02-17 | 2020-06-05 | 华润三九医药股份有限公司 | Quality control method of radix Stephaniae Tetrandrae and Poria decoction composition |
| CN108704014A (en) * | 2018-08-10 | 2018-10-26 | 刘亚飞 | It is a kind of to treat numb in every limb Tea containing traditional Chinese medicine |
| CN109030701A (en) * | 2018-08-20 | 2018-12-18 | 四川新绿色药业科技发展有限公司 | A kind of thin-layer identification method for the control of root of fangji medicinal material, medicine materical crude slice and granule quality |
| CN114053340A (en) * | 2021-12-27 | 2022-02-18 | 吉林吉春制药股份有限公司 | A Chinese medicinal composition for treating rheumatism, and its preparation method |
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