CN102662027B - 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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- CN102662027B CN102662027B CN201210175097.0A CN201210175097A CN102662027B CN 102662027 B CN102662027 B CN 102662027B CN 201210175097 A CN201210175097 A CN 201210175097A CN 102662027 B CN102662027 B CN 102662027B
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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 identification method of wide muscle rattan granule, belongs to traditional Chinese medicine quality detection technique field.
Background technology
The granule of the dry rattan that wide muscle rattan granule is menispermaceous plants Tinospora sinensis through being processed into, bitter, is slightly cold, and enters 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.The advantages such as compare with traditional Chinese herbs decoction, it has exempts to decoct easy clothes, easily stores, easy to carry.< < Chinese Pharmacopoeia > > one of version in 2010 is not recorded wide muscle rattan medicinal material kind, and Chinese medicinal granule has not been had a resemblance of medicinal material after the processing of serial operation, proterties differentiates that also significant discomfort is for Chinese medicinal granule.Thin-layered chromatography is simple to operate, convenient, is applicable to the qualitative discriminating of Chinese crude drug and various Chinese medicine preparations.
Summary of the invention
The object of the invention is to set up a kind of detection method simple, the TLC Identification of the reliable wide muscle rattan granule of testing result.
Technical scheme of the present invention is such: the method comprises the steps successively, 1) get this product powder 0.5g, solubilizer 25～35ml, reflux 25～35 minutes, filter, collect filtrate, solvent evaporated, residue adds water 20ml and dissolves, add 15～25ml ethyl acetate to extract at every turn 2 times, merge extract, evaporate to dryness ethyl acetate, residue adds methyl alcohol 1ml and dissolves, as need testing solution; 2) separately get wide muscle rattan control medicinal material 5g, add water 45～55ml, boil 30 minutes, filter, filtrate water bath method, residue solubilizer 25～35ml, is made in the same way of control medicinal material solution; 3) according to thin-layered chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put on same silica gel g thin-layer plate respectively, take toluene-ethyl acetate-formic acid as developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 105 ℃ clear, puts under ultraviolet lamp and inspects; 4) in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, blueness, the green fluorescence spot of aobvious same color.
The TLC Identification of above-mentioned wide muscle rattan granule, wherein, described solvent is methyl alcohol.
The TLC Identification 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 TLC Identification 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, made up the blank that wide muscle rattan granule thin layer is differentiated, to improve wide muscle rattan granule quality control, guarantee that product quality is significant; Meanwhile, the validity of clinical application and security are had to great importance.
Accompanying drawing explanation
Fig. 1 is 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 thin-layer chromatogram E of test sample; The 5th test thin-layer chromatogram F of test sample; Point of sample 1; Blue dot 2; Green point 3.
Embodiment
Below in conjunction with embodiment; the present invention is described in further detail; but do not form any limitation of the invention, the change of any unsubstantiality that anyone makes within the scope of claim of the present invention, still in claim protection domain of the present invention.
Get this product powder 0.5g, add methyl alcohol 30ml, reflux 30 minutes, filter, filtrate water bath method, residue adds water 20ml to be made to dissolve, and adds ethyl acetate 20ml jolting to extract 2 times, combined ethyl acetate extract at every turn, water bath method ethyl acetate, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution.Separately get wide muscle rattan control medicinal material 5g, add water 50ml, boil 30 minutes, filter, filtrate water bath method, residue adds methyl alcohol 30ml, is made in the same way of control medicinal material solution.According to thin-layered chromatography, test, draw respectively each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, detecting test sample repeats five times, toluene-ethyl acetate-the formic acid (7.5:2.5:0.25) of take is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, at 105 ℃, be heated to spot colour developing clear, put under ultraviolet lamp (365nm) and inspect, testing result, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, blueness, the green fluorescence spot of aobvious 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 thin-layer chromatogram E of test sample; The 5th test thin-layer chromatogram F of test sample; Point of sample 1; Blue dot 2; Green point 3.
Method of the present invention is simple, accurate, has made up the blank that wide muscle rattan granule thin layer is differentiated, to guaranteeing and improving the quality of products, is significant; Meanwhile, the validity of clinical application and security are had to great importance.
Claims (1)
1. a TLC Identification for wide muscle rattan granule, is characterized in that, the method comprises the steps successively, 1) get this product powder 0.5g, solubilizer 25～35ml, refluxes 25～35 minutes, filter, collect filtrate solvent evaporated, in filtrate, remaining residue adds water 20ml dissolving, is adding 15～25ml ethyl acetate to extract 2 times at every turn, merge extract, evaporate to dryness ethyl acetate, residue adds methyl alcohol 1ml and dissolves, as need testing solution; 2) separately get wide muscle rattan control medicinal material 5g, add water 45～55ml, boil 30 minutes, filter, filtrate water bath method, residue adds methyl alcohol 25～35ml, is made in the same way of control medicinal material solution; 3) according to 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, take mass ratio as: toluene-ethyl acetate-formic acid of 7.5:2.5:0.25 is developping agent, launches, and takes out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 105 ℃ clear, puts under wavelength 365nm ultraviolet lamp and inspects; 4) in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, blueness, the green fluorescence spot of aobvious same color.
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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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| 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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| CN102662027B true CN102662027B (en) | 2014-03-26 |
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| CN103893440A (en) * | 2014-03-28 | 2014-07-02 | 冯佩青 | Traditional Chinese medicine granules for treating ischemic papillopathy and detection method thereof |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (6)
| Title |
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| 兰钧.藏药催汤丸的薄层色谱研究.《中国民族民间医药》.2011,(第3期), |
| 冼艳婷.宽筋藤的鉴别研究.《中药材》.2008,第31卷(第9期), |
| 利毛才让，热增才旦.藏药四味藏木香汤散的质量研究.《中成药》.2010,第32卷(第3期), * |
| 宽筋藤的鉴别研究;冼艳婷;《中药材》;20080930;第31卷(第9期);1330-1331 * |
| 湖南省食品药品监督管理局.宽筋藤.《湖南省中药材标准(2009版)》.湖南科技出版社,2010,160. * |
| 藏药催汤丸的薄层色谱研究;兰钧;《中国民族民间医药》;20110331(第3期);2-3 * |
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