CN105866319B - The method of scutelloside in thin-layer chromatography Qualitive test throat-benefiting particle - Google Patents
The method of scutelloside in thin-layer chromatography Qualitive test throat-benefiting particle Download PDFInfo
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- CN105866319B CN105866319B CN201610248501.0A CN201610248501A CN105866319B CN 105866319 B CN105866319 B CN 105866319B CN 201610248501 A CN201610248501 A CN 201610248501A CN 105866319 B CN105866319 B CN 105866319B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/94—Development
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Abstract
The invention provides a kind of method of scutelloside in thin-layer chromatography Qualitive test, it is desirable to provide a kind of easy to operate, device simple, is advantageous to the discrimination method of scutelloside in the throat-benefiting particle of control throat-benefiting granular mass；This method comprises the steps：1) test sample is prepared；2) negative controls are prepared；3) product solution is shone；4) above-mentioned each 5 μ l of three kinds of solution are drawn, put respectively on same silica gel g thin-layer plate, using the ethyl acetate of volume ratio 80: 9: 10: 5: pyridine: water: methanol alcohol water is solvent, expansion, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear that spot development is heated at 102 DEG C, wavelength 343nm is put, is inspected under ultraviolet lamp；Belong to technical field of chemical detection.
Description
Technical field
The present invention provides a kind of discrimination method of scutelloside, is thin-layer chromatography Qualitive test throat-benefiting specifically
The method of scutelloside in grain；Belong to technical field of chemical detection.
Background technology
Throat-benefiting particle is made up of 13 kinds of Chinese medicines such as radix scutellariae, FRUCTUS TERMINALIAE IMMATURUS, balloonflower root, caulis bambusae in taenian, radix scutellariae, sterculia seed.Effect
Clearing heat, relieving sore-throat, wide chest wet one's whistle.For the pharyngeal dryness caused by affection of exogenous wind-heat, hoarseness；On acute/chronic pharyngitis, tonsillitis are shown in
Patient is stated, it is conventional to have protection vocal cords effect.Its quality standard record in：《Chinese Pharmacopoeia》Version one in 2005, only radix scutellariae
The assay index of glycosides, it is unfavorable for controlling the quality of the medicine.
The content of the invention
For above-mentioned deficiency, it is an object of the invention to provide a kind of easy to operate, device simple, is advantageous to control clear larynx profit
Swallow the discrimination method of scutelloside in the throat-benefiting particle of granular mass.
In order to solve the above technical problems, technical scheme provided by the invention is as follows：
The method of scutelloside, comprises the steps successively in a kind of thin-layer chromatography Qualitive test throat-benefiting particle：
1) this product powder 5g is taken, adds volume ratio 1：1 DMF and ethanol 30ml dissolving, centrifuging and taking supernatant
Liquid, by processed good large pore resin absorption column, first washed with 70% ethanol, collect eluent, be evaporated, then with 40% ethanol
5ml is eluted, and is collected eluent, is evaporated, with 5ml, methanol dissolving, as test sample；
2) throat-benefiting particle negative control 1g that is obtained by prescription preparation method while lacking radix scutellariae is taken, it is finely ground, add methanol 5mL,
Ultrasonic 30min, filtration, takes subsequent filtrate as negative control solution；
3) scutelloside reference substance 1g is taken, adds methanol 5ml dissolvings that reference substance solution is made；
4) above-mentioned each 5 μ l of three kinds of solution are drawn, are put respectively on same silica gel g thin-layer plate, with volume ratio 80: 9: 10: 5
Ethyl acetate: pyridine: water: methanol is solvent, deploy, take out, dry, spray with 10% ethanol solution of sulfuric acid, in 102 DEG C of heating
It is clear to spot development, wavelength 343nm is put, is inspected under ultraviolet lamp.
Further, in above-mentioned thin-layer chromatography Qualitive test throat-benefiting particle scutelloside method, described macropore
Adsorption resin column is D101 type resins.
Compared with prior art, technical scheme provided by the invention is entered using macroreticular resin absorbing method to throat-benefiting particle
Row extraction separation, then differentiated using thin-layer chromatography spectrum, it is easy, quick, be advantageous to control throat-benefiting granular mass, reappear
Property is good, can be used as the throat-benefiting particle Quality Control method of inspection.
Brief description of the drawings
Fig. 1 is throat-benefiting Particulate Extract thin layer phase chromatogram provided by the invention；
Wherein：1 reference substance tests thin-layer chromatogram；2 test samples test thin-layer chromatogram for the first time；Second of 3 test samples
Test thin-layer chromatogram；4 test samples third time experiment thin-layer chromatogram；5 negative controls test thin-layer chromatogram；Point of sample 1,
Colour developing point 2.
Embodiment
With reference to embodiment, the claim of the present invention is described in further detail, but not formed pair
Any restrictions of the present invention, the modification of any limited number of time made in the claims in the present invention protection domain, still the present invention's
Within claims.
Involved in the present invention arrives percentage composition concentration, and unless otherwise specified, solute is volumetric concentration for liquid, molten
Matter is mass concentration for fixation.
Embodiment 1
The method that the present invention provides scutelloside in a kind of thin-layer chromatography Qualitive test throat-benefiting particle, successively including following
Step：
1) need testing solution is prepared
This product powder 5g is taken, adds volume ratio 1：1 DMF and ethanol 30ml dissolving, centrifuging and taking supernatant
Liquid, by processed good D101 type resins, first washed with 70% ethanol, collect eluent, be evaporated, then washed with 40% ethanol 5ml
It is de-, eluent is collected, is evaporated, with 5ml, methanol dissolving, as test sample.
2) negative control solution is prepared
Throat-benefiting particle negative control 1g that is obtained by prescription preparation method while lacking radix scutellariae is taken, it is finely ground, add methanol 5mL, surpass
Sound 30min, filtration, takes subsequent filtrate as negative control solution；
3) reference substance is prepared
Scutelloside reference substance 1g is taken, adds methanol 5ml dissolvings that reference substance solution is made；
4) above-mentioned each 5 μ l of three kinds of solution are drawn, are put respectively on same silica gel g thin-layer plate, with the ethyl acetate of volume ratio-
Pyridine-water-methanol (80: 9: 10: 5) is solvent, is deployed, and takes out, dries, spray with 10% ethanol solution of sulfuric acid, is added at 102 DEG C
Heat is clear to spot development, puts and is inspected under ultraviolet lamp in wavelength 343nm；Referring particularly to Fig. 1, wherein：1 reference substance tests thin layer
Chromatogram；2 test samples test thin-layer chromatogram for the first time；3 test samples test thin-layer chromatogram for the second time；4 test samples third time
Test thin-layer chromatogram, 5 negative controls experiment thin-layer chromatogram；Point of sample A, colour developing point B.
Compared with prior art, the advantage of the invention is that method is simply accurate, to improving product quality and clinical application
Validity and security be respectively provided with significance.
Claims (2)
1. a kind of method of scutelloside in thin-layer chromatography Qualitive test throat-benefiting particle, it is characterised in that successively including following
Step：
1) this product powder 5g is taken, adds volume ratio 1：1 DMF and ethanol 30ml dissolving, centrifuging and taking supernatant,
By processed good large pore resin absorption column, first washed with 70% ethanol, collect eluent, be evaporated, then washed with 40% ethanol 5ml
It is de-, eluent is collected, is evaporated, the eluent after being evaporated twice with the dissolving of 5ml methanol, as test sample；
2) throat-benefiting particle negative control 1g that is obtained by prescription preparation method while lacking radix scutellariae is taken, it is finely ground, add methanol 5mL, ultrasound
30min, filtration, takes subsequent filtrate as negative control solution；
3) scutelloside reference substance 1g is taken, adds methanol 5ml dissolvings that reference substance solution is made；
4) above-mentioned each 5 μ l of three kinds of solution are drawn, are put respectively on same silica gel g thin-layer plate, with the acetic acid of volume ratio 80: 9: 10: 5
Ethyl ester: pyridine: water: methanol is solvent, deploy, take out, dry, spray with 10% ethanol solution of sulfuric acid, spot is heated at 102 DEG C
Point colour developing is clear, puts wavelength 343nm, is inspected under ultraviolet lamp.
2. the method for scutelloside, its feature exist in thin-layer chromatography Qualitive test throat-benefiting particle according to claim 1
In described large pore resin absorption column is D101 type resins.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610248501.0A CN105866319B (en) | 2016-04-20 | 2016-04-20 | The method of scutelloside in thin-layer chromatography Qualitive test throat-benefiting particle |
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|---|---|---|---|
| CN201610248501.0A CN105866319B (en) | 2016-04-20 | 2016-04-20 | The method of scutelloside in thin-layer chromatography Qualitive test throat-benefiting particle |
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| CN105866319A CN105866319A (en) | 2016-08-17 |
| CN105866319B true CN105866319B (en) | 2017-12-05 |
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Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100522138C (en) * | 2004-06-05 | 2009-08-05 | 余世春 | Preparation process and quality control technology of decoction of bupleurum root for regulating Shaoyang |
| CN1911396A (en) * | 2005-08-12 | 2007-02-14 | 北京联合西创药物科技有限公司 | Method for controlling quality injection contg. traditional Chinese medicine |
| CN1739614A (en) * | 2005-09-16 | 2006-03-01 | 中国科学院长春应用化学研究所 | The component detection method of WEITELING JIAONANG |
| CN1973866A (en) * | 2006-12-21 | 2007-06-06 | 贵州益佰制药股份有限公司 | Quality control method for cold treating and cough relieving syrup |
| GB2463530B (en) * | 2008-09-23 | 2012-08-08 | Gary William Wheatley | The sub-critical water extraction of German Chamomile flowers |
| CN101564514B (en) * | 2009-06-12 | 2013-06-05 | 杨文龙 | Method for analyzing children Fengreqing particle |
| CN101670041A (en) * | 2009-07-17 | 2010-03-17 | 贵州信邦制药股份有限公司 | Method for controlling quality of astragalus in Chinese medicine preparation |
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Address after: 543000 198 West Ring Road, Wuzhou, the Guangxi Zhuang Autonomous Region Patentee after: WUZHOU FOOD AND DRUG INSPECTION INSTITUTE Address before: 543000 198 West Ring Road, Wuzhou, the Guangxi Zhuang Autonomous Region Patentee before: WUZHOU INSTITUTE FOR FOOD AND DRUG CONTROL, GUANGXI ZHUANG AUTONOMOUS REGION |
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Application publication date: 20160817 Assignee: GUANGXI GUILIN RUIDE DETECTION AUTHENTICATION TECHNOLOGY Co.,Ltd. Assignor: WUZHOU FOOD AND DRUG INSPECTION INSTITUTE Contract record no.: X2022450000291 Denomination of invention: Qualitative Identification of Baicalin in Qinghou Liyan Granules by TLC Granted publication date: 20171205 License type: Common License Record date: 20221214 |