CN102335238A - Detection method of frankincense and elecampane lithiasis-removing granular traditional Chinese preparation - Google Patents
Detection method of frankincense and elecampane lithiasis-removing granular traditional Chinese preparation Download PDFInfo
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- CN102335238A CN102335238A CN2010102340936A CN201010234093A CN102335238A CN 102335238 A CN102335238 A CN 102335238A CN 2010102340936 A CN2010102340936 A CN 2010102340936A CN 201010234093 A CN201010234093 A CN 201010234093A CN 102335238 A CN102335238 A CN 102335238A
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Abstract
The invention relates to a detection method of a frankincense and elecampane lithiasis-removing granular traditional Chinese preparation. The detection method comprises an identification process of cinnamon and a content measurement process of cynanchum paniculatum.
Description
Invention field
The present invention relates to the detection method of oral Chinese medicine preparation, particularly the detection method of two fragrant PAISHI KELIs.
Background technology
Two fragrant PAISHI KELIs record in ministry standard (WS3-B-2859-98), are made up of 13 flavor Chinese crude drug preparations such as Olibanum (system), Radix Inulae, Cortex Cinnamomi, Herba Glechomae, Radix Cynanchi Paniculati, Caulis Akebiae, and diuretic is arranged; Treating stranguria; Calculus, the effect of detoxifcation is used to treat stranguria caused by urinary stone and gets rid of urinary calculi.Existing two fragrant PAISHI KELI only detects its quality from character, exists quality control to lack limit.Main Chinese medicine Radix Cynanchi Paniculati can stimulate pendant, interrenal system and strengthen its effect in its prescription, thereby can suppress immunoreation, and the blood circulation of improvement, antiinflammation are arranged simultaneously.Therefore be necessary the content and the cinnamomic discriminating that increase its Main Ingredients and Appearance Radix Cynanchi Paniculati are carried out quality control to two fragrant PAISHI KELI preparations.
Summary of the invention
The object of the present invention is to provide a kind of method of quality control that detects the oral Chinese medicine preparation.
The object of the invention provides that a kind of Cortex Cinnamomi that detects in two fragrant PAISHI KELIs is differentiated and the new standard of the content of Radix Cynanchi Paniculati.
The Cortex Cinnamomi discrimination method:
These article of getting powder 0.5g adds ethanol 10ml, and ultrasonic 30 minutes, jolting constantly filtered, and filtrating is as need testing solution.Other gets the cinnamic aldehyde reference substance, adds ethanol and processes the solution that every 1ml contains 1 μ l, as reference substance solution.According to thin layer chromatography test, draw need testing solution 2～5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-ethyl acetate (17: 8; 17: 3; 17: 1) be to launch developing solvent, take out, to dry, spray is with dinitrophenylhydrazine ethanol test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Assay: measure according to HPLC (appendix VID of pharmacopeia in 2005)
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With methanol-water (45: 55) is mobile phase; The detection wavelength is 274nm.Number of theoretical plate calculates by the paeonol peak should be not less than 3000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the paeonol reference substance, adds methanol and process the solution that every 1ml contains 20ug, promptly gets.
The about 2g of these article is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug conical flask, the accurate methanol 50ml that adds; Claim to decide weight, supersound process (power 250W, frequency 33kHz) 20-50 minute is put cold; Claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methanol.Precision is measured subsequent filtrate 1ml, puts in the 10ml measuring bottle, adds methanol and is diluted to scale, shakes up, and promptly gets.Accurate respectively reference substance solution and each 10ul of need testing solution of drawing injects liquid phase color shop appearance, measures, and promptly gets.These article contain paeonol (C9H10O3) for every bag must not be less than 2.0mg.
Detection method of the present invention has not only increased the qualitative identification method but also has increased the Content Measurement of Effective Ingredient in Happiness method, has improved the specificity and the quality stability of the method for quality control of preparation of the present invention, has guaranteed the safety and the effectiveness of people's medications.
The specific embodiment
Through following specific embodiment the present invention is described further, but not as restriction of the present invention.
Experimental example 1: Cortex Cinnamomi is differentiated the research of assay method in two fragrant PAISHI KELIs
Tianjin, island book layer bed board appearance, silica gel G (Qingdao make people rich source silica gel chemical reagent work).Cinnamic aldehyde reference substance (Nat'l Pharmaceutical & Biological Products Control Institute); Water is purified water; All the other reagent are analytical pure.The sample product batch number is: 100301, and Jiangxi Jimin Kexin Drug Industry Co., Ltd provides.
The selection of developing solvent proportioning: use petroleum ether (60～90 ℃)-ethyl acetate respectively by 17: 8; 17: 3; 17: the 1 pairs of samples and contrast launch respectively, and the result launches to separate better with 17: 3 proportioning with petroleum ether (60～90 ℃)-ethyl acetate, and it is clear to develop the color.
So selecting petroleum ether (60～90 ℃)-ethyl acetate was the proportioning of developing solvent with 17: 3.
Cortex Cinnamomi is identified that selecting petroleum ether (60～90 ℃)-ethyl acetate be the proportioning of developing solvent with 17: 3 by above discrimination method, with the corresponding position of reference substance chromatograph on, the speckle of apparent same color.The result shows, this method is stable to the quality control of two fragrant PAISHI KELIs, and favorable reproducibility can better be controlled the quality of two fragrant PAISHI KELIs.
Experimental example 2: the research of Radix Cynanchi Paniculati content assaying method in two fragrant PAISHI KELIs
1, the selection of extraction conditions:
Be soluble in the characteristics of organic solvents such as methanol according to paeonol, supersound extraction is selected in experiment for use, uses methanol respectively ultrasonic 20 minutes; 30 minutes, 40 minutes, 60 minutes; The result shows with 30 minutes mensuration of methanol treatment sample ultrasonic best results, and methanol extraction impurity is few, can better protect chromatographic column.
Table 1, the selection of ultrasonic time
| Ultrasonic time | Paeonol content (mg/ bag) |
| 20 minutes | 2.56 |
| 30 minutes | 3.62 |
| 40 minutes | 3.60 |
| 60 minutes | 3.59 |
2, the investigation of chromatographic condition
Instrument and reagent: Tianjin, island LC-10ATVP high performance liquid chromatograph, the paeonol reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number :); Methanol is chromatographic grade, and water is ultra-pure water, and other reagent is analytical pure; Testing sample is that Jiangxi Jimin Kexin Drug Industry Co., Ltd provides, and lot number does
Chromatographic condition and system suitability are tested with reference to Radix Cynanchi Paniculati content detection condition (2005 editions one one of Chinese Pharmacopoeia) as a reference: with the octadecylsilane chemically bonded silica is filler; With methanol-water (45: 55) is mobile phase; Number of theoretical plate calculates by the paeonol peak should be not less than 3000.
Detect wavelength and get the paeonol reference substance solution in the interscan of wavelength 200-400nm scope, the result has absorption maximum at the 274nm place, so select 274nm as detecting wavelength.
It is an amount of that the preparation precision of reference substance solution takes by weighing the paeonol reference substance, adds methanol and process the solution that every 1ml contains 20ug, promptly gets.
The about 2g of these article is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug conical flask, the accurate methanol 50ml that adds; Claim to decide weight, supersound process (power 250W, frequency 33kHz) 20-50 minute is put cold; Claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methanol.Precision is measured subsequent filtrate 1ml, puts in the 10ml measuring bottle, adds methanol and is diluted to scale, shakes up, and promptly gets.
3, methodological study
3.1 linear relationship
Precision takes by weighing paeonol reference substance 2.02mg and puts in the measuring bottle of 100ml, adds methanol and processes the solution that every 1ml contains 20ug, promptly gets (20.02ug/ml).Draw 2,4,6,8,10ul, inject chromatograph of liquid, measure peak area, be horizontal vertical mark with the sample introduction (ug) of reference substance, be vertical coordinate with the peak area, the drawing standard curve.
Table 2: linear relationship experimental data (n=5)
Y＝600000X-10064
R＝0.9993
The result shows: in 0.04004～0.20020ug scope, be good linear relationship.
3.2 negative control experiment:
In the ratio (removal Radix Cynanchi Paniculati) of prescription taste of Chinese medicine, the blank preparation of the two fragrant PAISHI KELIs of preparation is pressed " assay " operation down with the sample of preparation, and the result shows: other component is surveyed content detection of paeonol to this method in the sample does not have interference.
3.3 stability test
The accurate reference substance solution 10ul that draws, interval certain hour sample introduction, the peak area of mensuration paeonol, RSD is: 1.11%, the result shows that the mensuration result is stable in 24 hours, the result sees table 5.
Table 3 stability test data (n=5)
3.4 precision test
The accurate need testing solution 10ul that draws injects chromatograph of liquid, measures the peak area of paeonol, repeats sample introduction 5 times, and RSD is 1.43% as a result, sees table 6
Table 4 precision test data (n=5)
3.5 repeatability test
According to the operation down of assay item, (lot number: 090101) sample is measured for 5 parts, and trying to achieve relative standard deviation RSD is 0.43%, and the result sees table 7 to same lot number
Table 5 repeatability test data
3.6 recovery test
Reclaim with application of sample; Precision take by weighing known paeonol content same lot number (lot number: the about 1g of test sample 090101 0.038mg/ sheet), it is a certain amount of that precision adds paeonol reference substance solution (0.1021mg/ml) respectively, according to the operation down of assay item; Be calculated as follows the response rate, the result sees table 8
Average recovery rate is: 99.81%RSD is 0.03%
The method that embodiment 3, two fragrant PAISHI KELI quality of the pharmaceutical preparations detect
Differentiate detection method
These article of getting powder 0.5g adds ethanol 10ml, and ultrasonic 30 minutes, jolting constantly filtered, and filtrating is as need testing solution.Other gets the cinnamic aldehyde reference substance, adds ethanol and processes the solution that every 1ml contains 1 μ l, as reference substance solution.According to the thin layer chromatography test, draw need testing solution 2～5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate; With petroleum ether (60～90 ℃)-ethyl acetate (17: 3) is developing solvent, launches, and takes out; Dry, spray is with dinitrophenylhydrazine ethanol test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
The paeonol content detection method
Assay: measure according to HPLC (appendix VID of pharmacopeia in 2005)
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With methanol-water (45: 55) is mobile phase; The detection wavelength is 274nm.Number of theoretical plate calculates by the paeonol peak should be not less than 3000.It is an amount of that the preparation precision of reference substance solution takes by weighing the paeonol reference substance, adds methanol and process the solution that every 1ml contains 20ug, promptly gets.The about 2g of these article is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug conical flask, the accurate methanol 50ml that adds; Claim to decide weight, supersound process (power 250W, frequency 33kHz) 30 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 1ml, puts in the 10ml measuring bottle, adds methanol and is diluted to scale, shakes up, and promptly gets.Accurate respectively reference substance solution and each 10ul of need testing solution of drawing injects liquid phase color shop appearance, measures, and promptly gets.These article contain paeonol (C9H10O3) for every bag must not be less than 2.0mg.
Claims (4)
1. the detection method of two fragrant PAISHI KELI Chinese medicine preparation is characterized in that, comprises the assay of cinnamomic discrimination method and Radix Cynanchi Paniculati.
2. detection method according to claim 1 is characterized in that, said discrimination method comprises:
These article of getting powder 0.5g adds ethanol 10ml, and ultrasonic 30 minutes, jolting constantly filtered, and filtrating is as need testing solution.Other gets the cinnamic aldehyde reference substance, adds ethanol and processes the solution that every 1ml contains 1 μ l, as reference substance solution.According to thin layer chromatography test, draw need testing solution 2～5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-ethyl acetate (17: 8; 17: 3; 17: 1) be to launch developing solvent, take out, to dry, spray is with dinitrophenylhydrazine ethanol test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
3. detection method according to claim 1 is characterized in that, said assay comprises:
Measure according to HPLC (appendix VID of pharmacopeia in 2005)
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With methanol-water (45: 55) is mobile phase; The detection wavelength is 274nm.Number of theoretical plate calculates by the paeonol peak should be not less than 3000,
It is an amount of that the preparation precision of reference substance solution takes by weighing the paeonol reference substance, adds methanol and process the solution that every 1ml contains 20ug, promptly get,
The about 2g of these article is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug conical flask, the accurate methanol 50ml that adds; Claim to decide weight, supersound process (power 250W, frequency 33kHz) 20-50 minute is put cold; Claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methanol.Precision is measured subsequent filtrate 1ml, puts in the 10ml measuring bottle, adds methanol and is diluted to scale, shakes up, and promptly gets.Accurate respectively reference substance solution and each 10ul of need testing solution of drawing injects liquid phase color shop appearance, measures, and promptly gets.
These article contain paeonol (C9H10O3) for every bag must not be less than 2.0mg.
4. the detection method of two fragrant PAISHI KELI Chinese medicine preparation is characterized in that, may further comprise the steps:
Discrimination method
These article of getting powder 0.5g adds ethanol 10ml, and ultrasonic 30 minutes, jolting constantly filtered, and filtrating is as need testing solution.Other gets the cinnamic aldehyde reference substance, adds ethanol and processes the solution that every 1ml contains 1 μ l, as reference substance solution.According to the thin layer chromatography test, draw need testing solution 2～5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate; With petroleum ether (60～90 ℃)-ethyl acetate (17: 3) is developing solvent, launches, and takes out; Dry, spray is with dinitrophenylhydrazine ethanol test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color,
The paeonol content detection method
Assay: measure according to HPLC (appendix VID of pharmacopeia in 2005)
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With methanol-water (45: 55) is mobile phase; The detection wavelength is 274nm.Number of theoretical plate calculates by the paeonol peak should be not less than 3000,
It is an amount of that the preparation precision of reference substance solution takes by weighing the paeonol reference substance, adds methanol and process the solution that every 1ml contains 20ug, promptly get,
The about 2g of these article is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug conical flask, the accurate methanol 50ml that adds; Claim to decide weight, supersound process (power 250W, frequency 33kHz) 30 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 1ml, puts in the 10ml measuring bottle, adds methanol and is diluted to scale, shakes up, and promptly gets, and accurate respectively reference substance solution and each 10ul of need testing solution of drawing injects liquid phase color shop appearance, measures, promptly get,
These article contain paeonol (C9H10O3) for every bag must not be less than 2.0mg.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102340936A CN102335238A (en) | 2010-07-22 | 2010-07-22 | Detection method of frankincense and elecampane lithiasis-removing granular traditional Chinese preparation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203687A (en) * | 2015-09-18 | 2015-12-30 | 西安科技大学 | Paeonol quick detection method |
| CN106692316A (en) * | 2016-12-22 | 2017-05-24 | 江西济民可信药业有限公司 | Preparation method of frankincense and elecampane urinary calculus-removing granules |
-
2010
- 2010-07-22 CN CN2010102340936A patent/CN102335238A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203687A (en) * | 2015-09-18 | 2015-12-30 | 西安科技大学 | Paeonol quick detection method |
| CN106692316A (en) * | 2016-12-22 | 2017-05-24 | 江西济民可信药业有限公司 | Preparation method of frankincense and elecampane urinary calculus-removing granules |
| CN106692316B (en) * | 2016-12-22 | 2018-11-20 | 江西济民可信药业有限公司 | A kind of preparation method of double fragrant PAISHI KELIs |
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