CN105223305A - The discrimination method of a kind of Chinese medicine alangium - Google Patents
The discrimination method of a kind of Chinese medicine alangium Download PDFInfo
- Publication number
- CN105223305A CN105223305A CN201510709923.9A CN201510709923A CN105223305A CN 105223305 A CN105223305 A CN 105223305A CN 201510709923 A CN201510709923 A CN 201510709923A CN 105223305 A CN105223305 A CN 105223305A
- Authority
- CN
- China
- Prior art keywords
- solution
- reference substance
- alangium
- need testing
- chinese medicine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses the discrimination method of a kind of Chinese medicine alangium, the preparation of reference substance solution that the method comprises the steps: (1); (2) take methylene chloride as solvent, ultrasonic method process test sample, obtained need testing solution; (3) according to thin-layered chromatography test, draw reference substance solution, need testing solution, put respectively on same silica gel g thin-layer plate, with methylene chloride-methanol-ammoniacal liquor for developping agent, launch, take out, dry, spray with bismuth potassium iodide test solution.In test sample chromatogram, on the position corresponding to reference substance chromatogram, the spot of aobvious same color.The discrimination method of medicinal material alangium provided by the invention is simple to operate, save time, and developping agent is selected suitably, good separating effect, thin layer clear spot, favorable reproducibility, blank noiseless.
Description
Technical field
The present invention relates to the discrimination method of Chinese medicine alangium, be specifically related to the TLC Identification of a kind of Chinese medicine alangium.
Background technology
Alangium is dry radicula and the fibrous root of Alangiaceae plant alangium.There is the effects such as dispelling wind and removing obstruction in the meridians, loose stasis of blood throe, anesthesia and relaxed muscle, be used for the treatment of rheumatalgia pain, paralysis and numbness, heart failure, strain pain in the back, traumatic injury etc.
Existing alangium discrimination method mainly contains two kinds: (1) is got test sample 2.5g and carry out refluxing extraction under the condition of acidic ethanol, filter, filtrate uses sodium hydroxide solution adjust pH, use methenyl choloride jolting, evaporate to dryness, residue adds 1mL methyl alcohol makes dissolving, as need testing solution, benzene-acetate-methanol-isopropyl alcohol-ammoniacal liquor (10:25:1:0.15:0.06) is adopted to be developping agent, get reference substance solution and each 20 μ L of need testing solution respectively, put respectively on same silica gel g thin-layer plate, carry out indentification by TLC, (2) get test sample 5g and add the ultrasonic process of ethanolic solution, filter, filtrate evaporate to dryness, residue adds certain density hydrochloric acid solution makes dissolving, filter, filtrate is washed with methenyl choloride, water layer strong ammonia solution adjust ph to 10, extract at twice with methenyl choloride, merge methenyl choloride liquid, with evaporate to dryness after anhydrous sodium sulfate dehydration, residue adds 1mL absolute ethyl alcohol makes dissolving, as need testing solution, with methenyl choloride-methyl alcohol-ammonia solution (90:5:1) for developping agent, get reference substance solution and each 5 μ L of need testing solution respectively, put respectively on same silica gel g thin-layer plate, carry out indentification by TLC.
But said method exists following problem: the preparation process of (1) need testing solution is complicated, and employs the larger organic solvent of toxicity " methenyl choloride " in last handling process, this is intended to be avoided in new edition pharmacopeia as far as possible; (2) developping agent kind is more, operates comparatively loaded down with trivial details; (3) need testing solution concentration is comparatively large, and point sample amount is large, is not easy to printing operation.
Summary of the invention
The object of the present invention is to provide the TLC Identification of a kind of Chinese medicine alangium, the preparation of the method need testing solution is simple, save time; Developping agent kind is few and toxicity is little, colour developing clear spot, favorable reproducibility, and result is easy to judge.
For achieving the above object, the present invention includes following steps:
A. the preparation of reference substance solution: get alangine reference substance, adds methyl alcohol and makes the solution of every 1mL containing 0.5mg, product solution in contrast;
B. the preparation of need testing solution: got this product powder after No. 4 sieves, and added the organic solvent of the ammoniacal liquor of medicinal material 0.5 ~ 1 times amount, 25 ~ 35 times amount successively, ultrasonic process 30 minutes, filter, filtrate is evaporate to dryness in 65 ~ 75 DEG C of water-baths, and residue adds methyl alcohol 1mL makes dissolving, as need testing solution;
C. thin-layered chromatography test: draw reference substance solution 10 μ L and need testing solution 5 ~ 10 μ L, put respectively on same silica gel g thin-layer plate, with methylene chloride-methanol-ammoniacal liquor for developping agent, manually contact point sample, ascending development, exhibition, apart from 8cm, is taken out, dry, spray with bismuth potassium iodide test solution, colour developing;
D. result judges: in test sample chromatogram, on the position corresponding to reference substance chromatogram, the spot of aobvious same color.
In the method, the ammoniacal liquor addition described in step b is 1 times amount of medicinal material, and described organic solvent is methylene chloride, and its addition is 30 times amount of medicinal material, and described ultrasound wave treatment conditions are power 250W, frequency 40kHz; The volume ratio of the developping agent methylene chloride-methanol-ammoniacal liquor described in step c is 2:5:0.5.
A discrimination method for Chinese medicine alangium, its preferred version is as follows:
A. the preparation of reference substance solution: get alangine reference substance, adds methyl alcohol and makes the solution of every 1mL containing 0.5mg, product solution in contrast;
B. the preparation of need testing solution: got this product powder after No. 4 sieves, add the ammoniacal liquor of 1 times amount successively, the methylene chloride of 30 times amount, 30 minutes are processed under the condition of ultrasonic power 250W, frequency 40kHz, filter, filtrate is evaporate to dryness in 70 DEG C of water-baths, and residue adds methyl alcohol 1ml makes dissolving, as need testing solution;
C. thin-layered chromatography test: draw reference substance solution 10 μ L and need testing solution 5 ~ 10 μ L, put respectively on same silica gel g thin-layer plate, take volume ratio as the methylene chloride-methanol-ammoniacal liquor of 2:5:0.5 be developping agent, manual contact point sample, ascending development, exhibition is apart from 8cm, take out, dry, spray with bismuth potassium iodide test solution, colour developing;
D. result judges: in test sample chromatogram, on the position corresponding to reference substance chromatogram, the spot of aobvious same color.
Compared with prior art, tool of the present invention has the following advantages: (1) adopts ultrasonic method in test sample processing procedure, and is changed into " methylene chloride " by poisonous reagent " methenyl choloride ", and processing procedure is simple, easy to operate; (2) developping agent changes three kinds into by multiple, easy and simple to handle, save time; (3) highly sensitive, only need minute quantity reference substance namely can develop the color obviously, thin layer clear spot, favorable reproducibility, blank noiseless, result is easy to judge.
Accompanying drawing explanation
In order to make the object, technical solutions and advantages of the present invention clearly, the invention provides following accompanying drawing and being described:
Fig. 1 is the thin-layer chromatogram adopting the present invention to differentiate alangium, and wherein 1, No. 6 position is alangine reference substance, and 2, No. 3 positions are embodiment 1 design sketch, and 4, No. 5 positions are embodiment 2 design sketch.
embodiment:
In order to make those skilled in the art understand technical scheme of the present invention better, below by specific embodiment, the present invention is described in further detail.
Embodiment 1:
1, instrument and reagent
Alangine reference substance (purchased from TorontoReseardchemicalslnc, lot number: A637175); Silica G plate (100mm × 200mm, Haiyang Chemical Plant, Qingdao); It is pure that other reagent are analysis.
2, method and result
Get alangine reference substance, add methyl alcohol and make the solution of every 1mL containing 0.5mg, product solution in contrast; Get powder (the crossing No. 4 sieves) 1.0g that the raw product of alangium are produced in Yunnan, add ammoniacal liquor 1mL successively, methylene chloride 30mL, ultrasonic (power 250W, frequency 40kHz) processes 30 minutes, filters, filtrate is evaporate to dryness in 70 DEG C of water-baths, and residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Draw reference substance solution 10 μ L and need testing solution 5 μ L, 10 μ l, put respectively on same silica gel g thin-layer plate, with methylene chloride-methanol-ammoniacal liquor (2:5:0.5) for developping agent, manually contact point sample, ascending development, exhibition, apart from 8cm, is taken out, dry, spray with bismuth potassium iodide test solution, colour developing.
Testing result, in test sample chromatogram, on the position corresponding to reference substance medicinal material chromatogram, the saffron spot of aobvious same color, 2, No. 3 positions of concrete accompanying drawings 1.
Embodiment 2:
1, instrument and reagent
Alangine reference substance (purchased from TorontoReseardchemicalslnc, lot number: A637175); Silica G plate (100mm × 200mm, Haiyang Chemical Plant, Qingdao); It is pure that other reagent are analysis.
2, method and result
Get alangine reference substance, add methyl alcohol and make the solution of every 1mL containing 0.5mg, product solution in contrast; Get powder (the crossing No. 4 sieves) 1.0g that the raw product of alangium are produced in Guizhou, add ammoniacal liquor 1mL successively, methylene chloride 30ml, ultrasonic (power 250W, frequency 40kHz) processes 30 minutes, filters, filtrate is evaporate to dryness in 70 DEG C of water-baths, and residue adds methyl alcohol 1mL makes dissolving, as need testing solution; Draw reference substance solution 10 μ L and need testing solution 5 μ L, 10 μ L, put respectively on same silica gel g thin-layer plate, with methylene chloride-methanol-ammoniacal liquor (2:5:0.5) for developping agent, manually contact point sample, ascending development, exhibition, apart from 8cm, is taken out, dry, spray with bismuth potassium iodide test solution, colour developing.
Testing result, in test sample chromatogram, on the position corresponding to reference substance medicinal material chromatogram, the saffron spot of aobvious same color, 4, No. 5 positions of concrete accompanying drawings 1.
Specific description of embodiments of the present invention does not above limit the present invention, and those skilled in the art can make various change or distortion according to the present invention, only otherwise depart from spirit of the present invention, all should belong to the scope of claims of the present invention.
Claims (6)
1. a discrimination method for Chinese medicine alangium, is characterized in that, comprises the following steps:
A. the preparation of reference substance solution: get alangine reference substance, adds methyl alcohol and makes the solution of every 1mL containing 0.5mg, product solution in contrast;
The preparation of b need testing solution: got this product powder after No. 4 sieves, and added the organic solvent of the ammoniacal liquor of medicinal material 0.5 ~ 1 times amount, 25 ~ 35 times amount successively, ultrasonic process 30 minutes, filter, filtrate is evaporate to dryness in 65 ~ 75 DEG C of water-baths, and residue adds methyl alcohol 1mL makes dissolving, as need testing solution;
C. thin-layered chromatography test: draw reference substance solution 10 μ L and need testing solution 5 ~ 10 μ L, put respectively on same silica gel g thin-layer plate, with methylene chloride-methanol-ammoniacal liquor for developping agent, manually contact point sample, ascending development, exhibition, apart from 8cm, is taken out, dry, spray with bismuth potassium iodide test solution, colour developing;
D. result judges: in test sample chromatogram, on the position corresponding to reference substance chromatogram, the spot of aobvious same color.
2. the discrimination method of a kind of Chinese medicine alangium according to claim 1, is characterized in that, the ammoniacal liquor addition described in step b is 1 times amount of medicinal material.
3. the discrimination method of a kind of Chinese medicine alangium according to claim 1, is characterized in that, the organic solvent described in step b is methylene chloride, and its addition is 30 times amount of medicinal material.
4. the discrimination method of a kind of Chinese medicine alangium according to claim 1, is characterized in that, the ultrasound wave treatment conditions described in step b are power 250W, frequency 40kHz.
5. the discrimination method of a kind of Chinese medicine alangium according to claim 1, is characterized in that, the volume ratio of the developping agent methylene chloride-methanol-ammoniacal liquor described in step c is 2:5:0.5.
6. the discrimination method of a kind of Chinese medicine alangium according to claim 1, it is characterized in that, its method for optimizing comprises the steps:
A. the preparation of reference substance solution: get alangine reference substance, adds methyl alcohol and makes the solution of every 1mL containing 0.5mg, product solution in contrast;
B. the preparation of need testing solution: got this product powder after No. 4 sieves, add the ammoniacal liquor of medicinal material 1 times amount successively, the methylene chloride of 30 times amount, 30 minutes are processed under the condition of ultrasonic power 250W, frequency 40kHz, filter, filtrate is evaporate to dryness in 70 DEG C of water-baths, and residue adds methyl alcohol 1mL makes dissolving, as need testing solution;
C. thin-layered chromatography test: draw reference substance solution 10 μ L and need testing solution 5 ~ 10 μ L, put respectively on same silica gel g thin-layer plate, take volume ratio as the methylene chloride-methanol-ammoniacal liquor of 2:5:0.5 be developping agent, manual contact point sample, ascending development, exhibition is apart from 8cm, take out, dry, spray with bismuth potassium iodide test solution, colour developing;
D. result judges: in test sample chromatogram, on the position corresponding to reference substance chromatogram, the spot of aobvious same color.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510709923.9A CN105223305B (en) | 2015-10-28 | 2015-10-28 | A kind of discrimination method of Chinese medicine Radix Alangii |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510709923.9A CN105223305B (en) | 2015-10-28 | 2015-10-28 | A kind of discrimination method of Chinese medicine Radix Alangii |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105223305A true CN105223305A (en) | 2016-01-06 |
| CN105223305B CN105223305B (en) | 2016-10-12 |
Family
ID=54992375
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510709923.9A Active CN105223305B (en) | 2015-10-28 | 2015-10-28 | A kind of discrimination method of Chinese medicine Radix Alangii |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105223305B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102370691A (en) * | 2010-08-26 | 2012-03-14 | 江西济民可信集团有限公司 | Ibufenac traditional Chinese preparation detection method |
| CN104880531A (en) * | 2014-02-27 | 2015-09-02 | 贵州益佰制药股份有限公司 | Detection method of medicinal preparation for treating arthralgia |
-
2015
- 2015-10-28 CN CN201510709923.9A patent/CN105223305B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102370691A (en) * | 2010-08-26 | 2012-03-14 | 江西济民可信集团有限公司 | Ibufenac traditional Chinese preparation detection method |
| CN104880531A (en) * | 2014-02-27 | 2015-09-02 | 贵州益佰制药股份有限公司 | Detection method of medicinal preparation for treating arthralgia |
Non-Patent Citations (3)
| Title |
|---|
| SARASWATHY A等: "Pharmacognostic studies on Alangium salvifolium (Linn.f.) Wang. root bark", 《PHARMACOGNOSY JOURNAL》 * |
| 湖南省食品药品监督管理局: "《湖南省中药材标准 2009年版》", 28 February 2010, 湖南科学技术出版社 * |
| 蒋媛媛等: "针椒巴布剂中两面针和八角枫的薄层色谱实验研究", 《时珍国医国药》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105223305B (en) | 2016-10-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102735784B (en) | Method for simultaneously determining one hundred pesticide residuals in traditional Chinese medicine through ultrahigh performance liquid chromatography-tandem quadrupole mass spectrum | |
| CN105259288B (en) | It is a kind of at the same detect poultry tissues in multi-medicament residual quantity method | |
| CN109270190A (en) | A method of 101 kinds of persticide residues in measurement fructus lycii | |
| CN104698107B (en) | The pre-treating method of residual Multiple Classes of Antibiotics in a kind of quick solvent extraction soil | |
| CN102297926B (en) | Rapid TLC identification and three-component simultaneous quantitative determination method for antitussive tablets | |
| CN103134871B (en) | Preparation method of test solution for detecting aconitine-type alkaloids through high-efficiency liquid phase chromatography | |
| CN106501442B (en) | A kind of quality determining method of a kind of reed mentioned in ancient books Huang powder for clearing lung-heat | |
| CN103091422B (en) | Method for detecting residual quantity of sodium nitrophenol in aquatic product | |
| CN105203654A (en) | Method for measuring content of 11 illegally added medicaments in veterinary drug powder | |
| CN104306745A (en) | Quality control method for rhizoma gastrodiae capsule | |
| CN103880721A (en) | Method of separating chiral drug penicillamine enantiomer based on functional gold nanochannel | |
| CN105021762B (en) | A kind of quick multi information thin-layer identification method of spina date seed water extract | |
| JP2012107954A5 (en) | ||
| CN103983703A (en) | High-performance-liquid-chromatography detection method for methylene blue in aquaculture water | |
| CN101869630A (en) | Measurement method for content of atropine sulfate in traditional Chinese medicine suppository containing belladonna liquid extract | |
| CN105223305A (en) | The discrimination method of a kind of Chinese medicine alangium | |
| CN109884199A (en) | Method for measuring content of flavonoid components in honey | |
| CN108828082A (en) | A kind of detection method for extracting albendazole class compound from the flesh of fish | |
| CN103901143A (en) | Pretreatment method for analyzing tetrabromobisphenol A in small amount of biologic serum | |
| CN104807944A (en) | Preparing method of scorzonera general flavone and finger-print map thereof | |
| CN103728399A (en) | Single-walled carbon nanohorn dispersion liquid-based dispersive micro solid phase extraction method | |
| CN112858550B (en) | Method for analyzing similarity of ginkgo leaf medicines of different manufacturers and/or different batches of same manufacturers | |
| CN112526057A (en) | Thin-layer chromatography identification method of Fuyanjing capsule | |
| CN107782840B (en) | Detection method of Shanmei summer-heat clearing granules | |
| CN109959737A (en) | The detection method of paraquat in traditional Chinese medicinal material raw materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |