CN101224259A - Quality controlling method of compound south isatis root granules - Google Patents
Quality controlling method of compound south isatis root granules Download PDFInfo
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- CN101224259A CN101224259A CNA2008100258709A CN200810025870A CN101224259A CN 101224259 A CN101224259 A CN 101224259A CN A2008100258709 A CNA2008100258709 A CN A2008100258709A CN 200810025870 A CN200810025870 A CN 200810025870A CN 101224259 A CN101224259 A CN 101224259A
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Abstract
The invention relates to a quality control method of a compound south radix isatidis granule, the method adopts: (1) thin layer chromatography is used for identifying the herba violae contained in the compound south radix isatidis granule; (2) normal butanol extract is used for detecting the content of normal butanol extract. The quality control method of the compound south radix isatidis granule of the invention overcomes the defects of the poor specialization of the existing chemical identification method and false positive result occurring when compound south radix isatidis adopts the thin layer chromatography to detect the south radix isatidis contained in the compound south radix isatidis granule, thus improving the specialization of the quality control method of the compound south radix isatidis granule and quality stability and ensuring the safety and effectiveness of application for people.
Description
Technical field
The present invention relates to the method for quality control of Chinese patent medicine, specifically, the present invention relates to the method for quality control of Chinese patent medicine compound south isatis root granules.
Background technology
Compound south isatis root granules is a kind of Chinese patent medicine (compound Chinese medicinal preparation) of eliminating inflammation and expelling toxin, has used for many years in China, and the clinical parotitis, pharyngitis, mastitis, furuncle of being used for the treatment of swells and ache, and curative effect is sure.Compound south isatis root granules is by the Chinese crude drug Rhizoma Et Radix Baphicacanthis Cusiae, and Herba Violae, Herba Taraxaci are prepared from according to the particulate common process of Chinese patent medicine.The quality standard of this product records in the 5th of ministry standard, standard numbering WS3-B-0972-91.Discrimination method in this standard includes (1) and passes through FeCl
3Make the chemical method of aldehydes matter colour developing detect phenols, Herba Taraxaci, Rhizoma Et Radix Baphicacanthis Cusiae contain phenols; (2) make the chemical method of sterol colour developing detect sterol by sulphuric acid, contain sterol in the Rhizoma Et Radix Baphicacanthis Cusiae; (3) by containing Rhizoma Et Radix Baphicacanthis Cusiae in the thin layer chromatography detection compound south isatis root granules, but the above two the obvious specificity of chemical differential method is not strong, false positive results also often appears in latter's thin layer chromatography, therefore this method is difficult to differentiate compound south isatis root granules, more can not effectively control the quality of its product.
Summary of the invention
Purpose of the present invention is exactly the shortcoming for the quality standard that overcomes present compound south isatis root granules, provides that a kind of specificity is strong, the method for quality control of compound south isatis root granules that can more accurate control product quality.
The present invention realizes like this.
The present invention adopts: (1) thin layer chromatography identifies that compound south isatis root granules contains Herba Violae; (2) the n-butyl alcohol extractum detects the n-butyl alcohol extract content.
The present invention can also further adopt the caffeic acid content in the high performance liquid chromatography detection compound south isatis root granules.
In fact, the n-butyl alcohol extractum mainly is in detecting its glycosides that contains (glycoside) class active ingredient; And contain caffeic acid in the Herba Taraxaci, by the content of the Herba Taraxaci in the caffeinic content reflection preparation.
Thin layer chromatography differentiates that the preferable condition that contains Herba Violae in the compound south isatis root granules is: get this product, porphyrize adds ethyl acetate, and supersound process is extracted, and filters, and filtrate evaporate to dryness, residue add ethyl acetate makes dissolving, as need testing solution.Other gets the Herba Violae control medicinal material, adds water boil, keeps little boiling, and filters, and filtrate evaporate to dryness, residue add ethyl acetate makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (2005 editions appendix VIB of Chinese Pharmacopoeia), draw need testing solution, control medicinal material solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (5: 3: 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 principal spot on, show the fluorescence speckle of same color.
The preferable condition that detects the content of the n-butyl alcohol extractum in the preparation is: get this product, porphyrize (crossing sieve No. two), the accurate title, decide, the accurate n-butyl alcohol that adds, measure according to the hot dipping under the determination of extractives method item (appendix xA of Chinese Pharmacopoeia version in 2005), make solvent with n-butyl alcohol.This product every bag (in dry product) contains the n-butyl alcohol extractum and must not be less than 40mg.
Caffeic acid (C in the high effective liquid chromatography for measuring compound south isatis root granules
9H
8O
4) the preferable condition of content be:
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.01% phosphoric acid solution (8: 92) is mobile phase; The detection wavelength is 323nm; 40 ℃ of column temperatures.Number of theoretical plate calculates by the caffeic acid peak should be not less than 3000.
The preparation precision of reference substance solution takes by weighing the caffeic acid reference substance, adds methanol and makes the solution that every 1ml contains caffeic acid 30 μ g.
This product is got in the preparation of need testing solution, claims to decide weight, porphyrize (crossing sieve No. three), and accurate title is fixed, put in the tool plug conical flask, the accurate methanol solution that adds 5% formic acid claims to decide weight, supersound process, supply the weight that subtracts mistake with 5% formic acid methanol solution, filter, discard filtrate just, the accurate subsequent filtrate of drawing, evaporate to dryness, residue is dissolved in water, and is transferred in the separatory funnel, uses ethyl acetate extraction, combined ethyl acetate liquid, evaporate to dryness, residue with dissolve with methanol to measuring bottle, add methanol to scale, shake up, promptly.
Accurate reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
This product contains Herba Taraxaci with caffeic acid (C for every bag
9H
8O
4) meter, must not be less than 0.10mg.
This assay method is through the methodology checking, and negative sample is noiseless to measuring, and caffeic acid presents good linear relationship in 5.03～60.34 μ g/ml scopes, and the linear correlation degree is γ=1.4547 * 10
3X+3.6619 * 10
7, r=0.9999.This extracting method response rate is 96.2% (n=5), and RSD is 1.9%.Measure ten reply side's south isatis root granules with this method, the caffeic acid content results is as follows:
| Lot number | Content | Lot number | Content |
| 6030 | 0.38 | 5088 | 0.12 |
| 6029 | 0.44 | 6026 | 0.15 |
| 6028 | 0.21 | 5113 | 0.18 |
| 6027 | 0.29 | 0602 | 0.16 |
| 5065 | 0.35 | 6393 | 0.20 |
The method of quality control of compound south isatis root granules of the present invention, it is not strong to have overcome existing chemical discrimination method specificity, and the compound south isatis root thin layer chromatography detects the shortcoming that contains the false positive results of Rhizoma Et Radix Baphicacanthis Cusiae in the compound south isatis root granules, improve the specificity and the quality stability of compound south isatis root granules method of quality control, guaranteed the safety and the effectiveness of people's medications.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
The lot number of getting applicant's production is
6028Compound south isatis root granules.
[discriminating] gets this product 10g, and porphyrize adds ethyl acetate 20ml, and supersound process (power 200w, frequency 25kHz) 30 minutes filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Herba Violae control medicinal material 2g, adds water 50ml, boils, and keeps little and boils 30 minutes, filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (2005 editions appendix VIB of Chinese Pharmacopoeia), draw need testing solution 5～10 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (5: 3: 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 principal spot on, show the fluorescence speckle of same color.
[inspection] should meet every regulation relevant under the granule item (appendix IC of Chinese Pharmacopoeia version in 2005).
[n-butyl alcohol extractum] gets 10 bags of this product, and accurate the title decides, porphyrize (crossing sieve No. two), get about 20g, the accurate title, decide, the accurate n-butyl alcohol 50ml that adds, measure according to the hot dipping under the determination of extractives method item (an appendix x of Chinese Pharmacopoeia version in 2005 A), make solvent with n-butyl alcohol.It is 54.2mg that this product every bag (in dry product) contains the n-butyl alcohol extractum.
[assay] measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005)
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.01% phosphoric acid solution (8: 92) is mobile phase; The detection wavelength is 323nm; 40 ℃ of column temperatures.Number of theoretical plate calculates by the caffeic acid peak should be not less than 3000.
The preparation precision of reference substance solution takes by weighing the caffeic acid reference substance, adds methanol and makes the solution that every 1ml contains caffeic acid 30 μ g.
10 bags of this product are got in the preparation of need testing solution, claim to decide weight, porphyrize (crossing sieve No. three), precision claims to conclude a contract or treaty puts 10g in the tool plug conical flask, the accurate methanol solution 50ml that adds 5% formic acid, claim to decide weight, supersound process (power 200w, frequency 25kHz) 30 minutes, supply the weight that subtracts mistake with 5% formic acid methanol solution, filter, discard filtrate just, the accurate subsequent filtrate 25ml that draws, evaporate to dryness, residue add water 30ml dissolving, are transferred in the separatory funnel, with ethyl acetate extraction 4 times, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue with dissolve with methanol to the 5ml measuring bottle, add methanol to scale, shake up, promptly.
Accurate reference substance solution and the need testing solution 5 μ l of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
This product contains Herba Taraxaci with caffeic acid (C for every bag
9H
8O
4) meter, be 0.21mg.
Claims (4)
1. the method for quality control of a compound south isatis root granules comprises employing: (1) thin layer chromatography identifies that compound south isatis root granules contains Herba Violae; (2) the n-butyl alcohol extractum detects the n-butyl alcohol extract content.
2. the method for quality control of a kind of compound south isatis root granules according to claim 1, it is characterized in that the condition that contains Herba Violae in the thin layer chromatography discriminating compound south isatis root granules is: get this product, porphyrize, add ethyl acetate, supersound process is extracted, and filters the filtrate evaporate to dryness, residue adds ethyl acetate makes dissolving, as need testing solution; Other gets the Herba Violae control medicinal material and adds water, boils, and keeps little boiling, and filters, and filtrate evaporate to dryness, residue add ethyl acetate makes dissolving, in contrast medical material solution; Draw need testing solution, control medicinal material solution, put respectively on same silica gel g thin-layer plate, be developing solvent with toluene-ethyl acetate-formic acid at 5: 3: 1, launches, and takes out, and dries, and puts under the ultra-violet lamp 365nm and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph principal spot on, show the fluorescence speckle of same color.
3. the method for quality control of a kind of compound south isatis root granules according to claim 1, its feature is to get this product in the condition that detects the n-butyl alcohol extract content, porphyrize is crossed sieve No. two, the accurate title, decide, the accurate n-butyl alcohol that adds is measured according to hot dipping, makes solvent with n-butyl alcohol; This product contains the n-butyl alcohol extractum in dry product for every bag must not be less than 40mg.
4. a kind of compound south isatis root granules method of quality control according to claim 1 is characterized in that also comprising the caffeinic content of high effective liquid chromatography for measuring, and its condition is:
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.01% phosphoric acid solution is mobile phase at 8: 92; The detection wavelength is 323nm; 40 ℃ of column temperatures; Number of theoretical plate calculates by the caffeic acid peak should be not less than 3000;
The preparation precision of reference substance solution takes by weighing the caffeic acid reference substance, adds methanol and makes the solution that every 1ml contains caffeic acid 30 μ g;
This product is got in the preparation of need testing solution, claims to decide weight, and porphyrize is crossed sieve No. three, and accurate the title decides, put in the tool plug conical flask, the accurate methanol solution that adds 5% formic acid claims to decide weight, supersound process, supply the weight that subtracts mistake with 5% formic acid methanol solution, filter, discard filtrate just, the accurate subsequent filtrate of drawing, evaporate to dryness, residue is dissolved in water, and is transferred in the separatory funnel, uses ethyl acetate extraction, combined ethyl acetate liquid, evaporate to dryness, residue with dissolve with methanol to measuring bottle, add methanol to scale, shake up, promptly;
Accurate reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly; This product contains Herba Taraxaci with caffeic acid C for every bag
9H
8O
4Meter must not be less than 0.10mg.
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|---|---|---|---|
| CN2008100258709A CN101224259B (en) | 2008-01-17 | 2008-01-17 | Detection method of compound south isatis root granules |
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|---|---|---|---|
| CN2008100258709A CN101224259B (en) | 2008-01-17 | 2008-01-17 | Detection method of compound south isatis root granules |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104666688A (en) * | 2015-03-16 | 2015-06-03 | 黄芳 | Traditional Chinese medicine composition and acupuncture point combination acupuncture application for treating mastitis |
| CN106226450A (en) * | 2016-08-25 | 2016-12-14 | 广州白云山奇星药业有限公司 | The qualitative checking method of indirubin in a kind of compound south isatis root granules |
| CN109521119A (en) * | 2018-12-24 | 2019-03-26 | 广州白云山奇星药业有限公司 | A kind of measuring method of compound south isatis root granules finger-print |
-
2008
- 2008-01-17 CN CN2008100258709A patent/CN101224259B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104666688A (en) * | 2015-03-16 | 2015-06-03 | 黄芳 | Traditional Chinese medicine composition and acupuncture point combination acupuncture application for treating mastitis |
| CN106226450A (en) * | 2016-08-25 | 2016-12-14 | 广州白云山奇星药业有限公司 | The qualitative checking method of indirubin in a kind of compound south isatis root granules |
| CN109521119A (en) * | 2018-12-24 | 2019-03-26 | 广州白云山奇星药业有限公司 | A kind of measuring method of compound south isatis root granules finger-print |
| CN109521119B (en) * | 2018-12-24 | 2021-07-20 | 广州白云山奇星药业有限公司 | Method for determining fingerprint spectrum of compound rhizoma et radix baphicacanthis cusiae granules |
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| Publication number | Publication date |
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| CN101224259B (en) | 2011-04-20 |
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Owner name: GUANGZHOU BAIYUNSHAN QIXING PHARMACEUTICAL CO., LT Free format text: FORMER NAME: QIXING PHARMACEUTICAL CO., LTD., GUANGZHOU |
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Address after: Guangzhou City, Haizhuqu District Xingang road Chigang Road No. 33 Patentee after: GUANGZHOU BAIYUNSHAN QIXING PHARMACEUTICAL CO., LTD. Address before: 510310 Guangdong Province, Guangzhou city Xingang road Chigang Road No. 33 Patentee before: Qixing Pharmaceutical Co., Ltd., Guangzhou |