CN102662027A - Thin-layer chromatography identification method of caulis tinosporae sinensis formula granules - Google Patents
Thin-layer chromatography identification method of caulis tinosporae sinensis formula granules Download PDFInfo
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- CN102662027A CN102662027A CN2012101750970A CN201210175097A CN102662027A CN 102662027 A CN102662027 A CN 102662027A CN 2012101750970 A CN2012101750970 A CN 2012101750970A CN 201210175097 A CN201210175097 A CN 201210175097A CN 102662027 A CN102662027 A CN 102662027A
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Abstract
The invention discloses a thin-layer chromatography identification method of caulis tinosporae sinensis formula granules and belongs to the technical field of traditional Chinese medicine quality detection. The method is simple in detection and reliable in detection result, and is technically characterized in that the method sequentially includes the steps: taking 0.5g of caulis tinosporae sinensis formula granule powder, adding solvent for reflux, filtering, collecting filtrate, drying the solvent by distillation, adding water into residue for dissolution, then adding ethyl acetate for extraction, combining ethyl acetate extracting solution, drying the ethyl acetate by distillation, adding 1ml of methanol into residue for dissolution, and using the dissolved residue as test sample solution; separately taking 5g of caulis tinosporae sinensis comparison medicinal materials, adding water, boiling for 30 minutes, filtering, drying filtrate by distillation by means of water bath and adding solvent into residue so that comparison medicinal material solution is prepared by the same method; and testing according to thin-layer chromatography by absorbing 5-microliter of each of the two solutions, developing by the aid of methylbenzene-ethyl acetate-methanoic acid serving as developer, taking out, drying, spraying sulfuric acid and ethanol solution with the concentration of 10%, heating at 105 DEG C until spot color is distinct, and inspecting below an ultraviolet lamp.
Description
Technical field
The present invention relates to a kind of detection method, specifically, is a kind of thin layer discrimination method of wide muscle rattan granule, belongs to traditional Chinese medicine quality detection technique field.
Background technology
Wide muscle rattan granule is the granule of dry rattan through being processed into of menispermaceous plants China limacia sagittata, and bitter is slightly cold, and goes into Liver Channel, has and stimulates the circulation of the blood and cause the muscles and joints to relax, and the effect of wind-expelling pain-stopping is mainly used in arthralgia due to wind-dampness, the contraction of muscle arteries and veins, joint stuffiness, traumatic injury.Compare advantage such as it has to exempt to fry in shallow oil and is prone to clothes, is prone to store, and is easy to carry with the traditional Chinese medicines decoction." Chinese pharmacopoeia one one of version in 2010 is not recorded wide muscle rattan medicinal material kind, and Chinese medicinal granule has not been through had the resemblance of medicinal material after the processing of serial operation, and character identification also significant discomfort is used for Chinese medicinal granule.Thin-layered chromatography is simple to operate, and is convenient, is applicable to the qualitative identification of Chinese crude drug and various Chinese medicine preparations.
Summary of the invention
It is simple to the objective of the invention is to set up a kind of detection method, the thin-layer chromatography discrimination method of the reliable wide muscle rattan granule of testing result.
Technical scheme of the present invention is such: this method comprises the steps 1 successively) get these article powder 0.5g, solubilizer 25～35ml refluxed 25～35 minutes; Filter, collect filtrating, solvent evaporated; Residue adds water 20ml dissolving, adds 15～25ml ethyl acetate extraction 2 times at every turn, merges extract; Evaporate to dryness ethyl acetate, residue add methyl alcohol 1ml dissolving, as need testing solution; 2) get wide muscle rattan control medicinal material 5g in addition, add water 45～55ml, boiled 30 minutes, filter, the filtrating water bath method, residue solubilizer 25～35ml shines medicinal material solution in pairs with legal system; 3) according to the thin-layered chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with toluene-ethyl acetate-formic acid; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing at 105 ℃, puts under the ultraviolet lamp and inspects; 4) in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show blueness, the green fluorescence spot of same color.
The thin-layer chromatography discrimination method of above-mentioned wide muscle rattan granule, wherein, described solvent is a methyl alcohol.
The thin-layer chromatography discrimination method of above-mentioned wide muscle rattan granule, wherein, the mass ratio of described toluene and ethyl acetate and formic acid is: 7.5:2.5:0.25.
The thin-layer chromatography discrimination method of above-mentioned wide muscle rattan granule, wherein, the wavelength of described ultraviolet lamp is 365nm.
Compared with prior art, the method that the invention has the advantages that is simple, accurately, remedied the blank that wide muscle rattan granule thin layer is differentiated, to the quality control that improves wide muscle rattan granule, guarantee that product quality is significant; Simultaneously, validity and the security to clinical application has great importance.
Description of drawings
Fig. 1 is a wide muscle rattan granule thin-layer chromatogram of the present invention;
Wherein: control medicinal material test thin-layer chromatogram A; Test sample is tested thin-layer chromatography B figure for the first time; Test sample is tested thin-layer chromatogram C for the second time; Test sample is tested thin-layer chromatogram D for the third time; The 4th test of test sample thin-layer chromatogram E; The 5th test of test sample thin-layer chromatogram F; Point of sample 1; Blue dot 2; Green point 3.
Embodiment
Below in conjunction with embodiment; The present invention is done further detailed description; But do not constitute any restriction of the present invention, the change of any unsubstantiality that anyone makes in claim scope of the present invention is still in claim protection domain of the present invention.
These article of getting powder 0.5g adds methyl alcohol 30ml, refluxes 30 minutes, filters; The filtrating water bath method, residue adds water 20ml makes dissolving, adds ethyl acetate 20ml jolting at every turn and extracts the combined ethyl acetate extract 2 times; Water bath method ethyl acetate, residue add methyl alcohol 1ml makes dissolving, as need testing solution.Other gets wide muscle rattan control medicinal material 5g, adds water 50ml, boils 30 minutes, filter, and the filtrating water bath method, residue adds methyl alcohol 30ml, shines medicinal material solution in pairs with legal system.According to the thin-layered chromatography test, draw each 5 μ l of above-mentioned two kinds of solution respectively, put respectively on same silica gel g thin-layer plate; Detecting test sample and repeat five times, is developping agent with toluene-ethyl acetate-formic acid (7.5:2.5:0.25), launches; Take out, dry, spray is with 10% ethanol solution of sulfuric acid; It is clear to be heated to spot colour developing at 105 ℃, puts under the ultraviolet lamp (365nm) and inspects testing result; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show blueness, the green fluorescence spot of same color; Specifically consult Fig. 1, control medicinal material test thin-layer chromatogram A; Test sample is tested thin-layer chromatogram B for the first time; Test sample is tested thin-layer chromatogram C for the second time; Test sample is tested thin-layer chromatogram D for the third time; The 4th test of test sample thin-layer chromatogram E; The 5th test of test sample thin-layer chromatogram F; Point of sample 1; Blue dot 2; Green point 3.
Method of the present invention is simple, accurate, has remedied the blank that wide muscle rattan granule thin layer is differentiated, is significant to guaranteeing and improving the quality of products; Simultaneously, validity and the security to clinical application has great importance.
Claims (4)
1. the thin-layer chromatography discrimination method of one kind wide muscle rattan granule is characterized in that, this method comprises the steps 1 successively) get these article powder 0.5g; Solubilizer 25～35ml refluxed 25～35 minutes, filtered, and collected the filtrating solvent evaporated; Residue adds water 20ml dissolving, adds 15～25ml ethyl acetate extraction 2 times each, merges extract; Evaporate to dryness ethyl acetate, residue add methyl alcohol 1ml dissolving, as need testing solution; 2) get wide muscle rattan control medicinal material 5g in addition, add water 45～55ml, boiled 30 minutes, filter, the filtrating water bath method, residue solubilizer 25～35ml shines medicinal material solution in pairs with legal system; 3) according to the thin-layered chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with toluene-ethyl acetate-formic acid; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing at 105 ℃, puts under the ultraviolet lamp and inspects; 4) in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show blueness, the green fluorescence spot of same color.
2. the thin-layer chromatography discrimination method of wide muscle rattan granule according to claim 1 is characterized in that, described solvent is a methyl alcohol.
3. the thin-layer chromatography discrimination method of wide muscle rattan granule according to claim 1 is characterized in that, described toluene-be with the mass ratio of ethyl acetate and-formic acid: 7.5:2.5:0.25.
4. the thin-layer chromatography discrimination method of wide muscle rattan granule according to claim 1 is characterized in that, the wavelength 365nm of described ultraviolet lamp.
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| CN201210175097.0A CN102662027B (en) | 2012-05-30 | 2012-05-30 | Thin-layer chromatography identification method of caulis tinosporae sinensis formula granules |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103893440A (en) * | 2014-03-28 | 2014-07-02 | 冯佩青 | Traditional Chinese medicine granules for treating ischemic papillopathy and detection method thereof |
| CN106236842A (en) * | 2016-08-30 | 2016-12-21 | 青海民族大学 | Herba Lycopodii suppresses HDAC1 enzyme effective site and preparation method and application |
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| CN101336972A (en) * | 2008-08-13 | 2009-01-07 | 甘肃奇正藏药有限公司 | Qingpeng paste and quality standard and detection method thereof |
| CN102419357A (en) * | 2011-12-26 | 2012-04-18 | 西藏奇正藏药股份有限公司 | Method for detecting eighteen-component codonopsis pilosula preparation |
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| CN101336972A (en) * | 2008-08-13 | 2009-01-07 | 甘肃奇正藏药有限公司 | Qingpeng paste and quality standard and detection method thereof |
| CN102419357A (en) * | 2011-12-26 | 2012-04-18 | 西藏奇正藏药股份有限公司 | Method for detecting eighteen-component codonopsis pilosula preparation |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103893440A (en) * | 2014-03-28 | 2014-07-02 | 冯佩青 | Traditional Chinese medicine granules for treating ischemic papillopathy and detection method thereof |
| CN106236842A (en) * | 2016-08-30 | 2016-12-21 | 青海民族大学 | Herba Lycopodii suppresses HDAC1 enzyme effective site and preparation method and application |
| CN106236842B (en) * | 2016-08-30 | 2019-12-10 | 青海民族大学 | Effective part of tinospora sinensis for inhibiting HDAC1 enzyme, preparation method and application |
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