CN101224259B - Detection method of compound south isatis root granules - Google Patents
Detection method of compound south isatis root granules Download PDFInfo
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- CN101224259B CN101224259B CN2008100258709A CN200810025870A CN101224259B CN 101224259 B CN101224259 B CN 101224259B CN 2008100258709 A CN2008100258709 A CN 2008100258709A CN 200810025870 A CN200810025870 A CN 200810025870A CN 101224259 B CN101224259 B CN 101224259B
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- isatis root
- compound south
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Abstract
The invention relates to a detection 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 detection 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 detection 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 detection method of Chinese patent drug, specifically, the present invention relates to the detection method of Chinese patent drug compound south isatis root granules.
Background technology
Compound south isatis root granules is a kind of Chinese patent drug (compound Chinese medicinal preparation) of eliminating inflammation and expelling toxin, has used for many years in China, clinical mumps, pharyngitis, mastitis, the sore furuncle pain of being used for the treatment of, and curative effect is sure.Compound south isatis root granules is by the Chinese crude drug rhizoma et Radix Baphicacanthis Cusiae, and Chinese violet, dandelion are prepared from according to the common process of Chinese patent drug particle.The quality standard of this product is recorded in the 5th of ministerial 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, dandelion, rhizoma et Radix Baphicacanthis Cusiae contain phenols; (2) make the chemical method of sterol colour developing detect sterol by sulfuric acid, contain sterol in the rhizoma et Radix Baphicacanthis Cusiae; (3) by containing rhizoma et Radix Baphicacanthis Cusiae in the thin-layered 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-layered 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 detection method 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-layered chromatography identifies that compound south isatis root granules contains Chinese violet; (2) the normal butyl alcohol extract detects the normal 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 normal butyl alcohol extract mainly is in detecting its glycosides that contains (glucoside) class effective ingredient; And contain caffeic acid in the dandelion, by the content of the dandelion in the caffeinic content reflection preparation.
Thin-layered chromatography differentiates that the preferable condition that contains Chinese violet in the compound south isatis root granules is: get this product, porphyrize adds ethyl acetate, and sonicated is extracted, and filters, and filtrate evaporate to dryness, residue add ethyl acetate makes dissolving, as need testing solution.Other gets the Chinese violet control medicinal material, adds water boil, keeps little boiling, and filters, and filtrate evaporate to dryness, residue add ethyl acetate makes dissolving, in contrast medicinal material solution.Test according to thin-layered 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 developping agent, launch, take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the fluorescence spot of same color.
The preferable condition that detects the content of the normal butyl alcohol extract in the preparation is: get this product, porphyrize (crossing sieve No. two), the accurate title, decide, the accurate normal 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 normal butyl alcohol.This product every bag (in dry product) contains the normal butyl alcohol extract 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 filling agent with the octadecylsilane chemically bonded silica; With acetonitrile-0.01% phosphoric acid solution (8: 92) is moving 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 methyl alcohol 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, sonicated, 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 separating funnel, uses ethyl acetate extraction, combined ethyl acetate liquid, evaporate to dryness, residue with dissolve with methanol to measuring bottle, add methyl alcohol to scale, shake up, promptly.
Accurate reference substance solution and the need testing solution drawn of determination method injects liquid chromatograph, measures, promptly.
This product contains dandelion 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 dependence degree is γ=1.4547 * 10
3X+3.6619 * 10
7, r=0.9999.This extracting method recovery 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-layered 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 security and the validity of people's medications.
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 sonicated (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 Chinese violet 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 medicinal material solution.Test according to thin-layered 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 developping agent, launch, take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the fluorescence spot of same color.
[inspection] should meet every regulation relevant under the granule item (appendix IC of Chinese Pharmacopoeia version in 2005).
[normal butyl alcohol extract] 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 normal 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 normal butyl alcohol.It is 54.2mg that this product every bag (in dry product) contains the normal butyl alcohol extract.
[assay] measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005)
Chromatographic condition and system suitability test are filling agent with the octadecylsilane chemically bonded silica; With acetonitrile-0.01% phosphoric acid solution (8: 92) is moving 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 methyl alcohol 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, sonicated (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 separating 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 methyl alcohol to scale, shake up, promptly.
Accurate reference substance solution and the need testing solution 5 μ l of drawing of determination method inject liquid chromatograph, measure, promptly.
This product contains dandelion with caffeic acid (C for every bag
9H
8O
4) meter, be 0.21mg.
Claims (4)
1. the detection method of a compound south isatis root granules comprises employing: (1) thin-layered chromatography identifies that compound south isatis root granules contains Chinese violet; (2) the normal butyl alcohol extract detects the normal butyl alcohol extract content.
2. the detection method of a kind of compound south isatis root granules according to claim 1, it is characterized in that the condition that contains Chinese violet in the thin-layered chromatography discriminating compound south isatis root granules is: get this product, porphyrize, add ethyl acetate, sonicated is extracted, and filters the filtrate evaporate to dryness, residue adds ethyl acetate makes dissolving, as need testing solution; Other gets the Chinese violet 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 medicinal material solution; Draw need testing solution, control medicinal material solution, put respectively on same silica gel g thin-layer plate, be developping agent with toluene-ethyl acetate-formic acid at 5: 3: 1, launches, and takes out, and dries, and puts under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram principal spot on, show the fluorescence spot of same color.
3. the detection method 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 normal butyl alcohol extract content, porphyrize is crossed sieve No. two, the accurate title, decide, the accurate normal butyl alcohol that adds is measured according to hot dipping, makes solvent with normal butyl alcohol; This product contains the normal butyl alcohol extract in dry product for every bag must not be less than 40mg.
4. a kind of compound south isatis root granules detection method 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 filling agent with the octadecylsilane chemically bonded silica; With acetonitrile-0.01% phosphoric acid solution is moving 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 methyl alcohol 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, sonicated, 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 separating funnel, uses ethyl acetate extraction, combined ethyl acetate liquid, evaporate to dryness, residue with dissolve with methanol to measuring bottle, add methyl alcohol to scale, shake up, promptly;
Accurate reference substance solution and the need testing solution drawn of determination method injects liquid chromatograph, measures, promptly; This product contains dandelion with caffeic acid C for every bag
9H
8O
4Meter must not be less than 0.10mg.
Priority Applications (1)
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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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| CN101224259B true CN101224259B (en) | 2011-04-20 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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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- 2008-01-17 CN CN2008100258709A patent/CN101224259B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 李钦等.复方南板蓝根冲剂质量标准研究.中国药学杂志.2004,39(12),938-940. * |
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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 |