CN109521137A - Menthol thin layer method in a kind of analysis cough-relieving pears soft extracts - Google Patents
Menthol thin layer method in a kind of analysis cough-relieving pears soft extracts Download PDFInfo
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- CN109521137A CN109521137A CN201811463744.1A CN201811463744A CN109521137A CN 109521137 A CN109521137 A CN 109521137A CN 201811463744 A CN201811463744 A CN 201811463744A CN 109521137 A CN109521137 A CN 109521137A
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- menthol
- solution
- thin layer
- cough
- relieving
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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
Abstract
The invention discloses menthol thin layer methods in a kind of analysis cough-relieving pears soft extracts, it is the following steps are included: step 1: taking menthol 20g, add petroleum ether 25ml, concussion is extracted 1 hour, and supernatant is taken to wave to 1ml to get test solution；Step 2: separately taking menthol reference substance, add dehydrated alcohol that solution of every 1ml containing 2mg is made, as reference substance solution.Beneficial effect is: by using petroleum ether as extracting solution, using toluene-ethyl acetate solvent, using 5% vanillin-sulfuric acid-ethanol solution as color developing agent, and using silica G plate as display board, so that the clear spot of the Chromatogram display of menthol thin layer, favorable reproducibility, eliminate colour developing deviation.
Description
Technical field
The present invention relates to Pharmaceutical Analysis method fields, and the present invention relates to menthol thin layer sides in a kind of analysis cough-relieving pears soft extracts
Method.
Background technique
Cough-relieving pears soft extracts is made of pears clear cream, dried orange peel, the tuber of pinellia (system), fritillaria thunbergii, Exocarpium Citri Rubrum, is used for xeropulmonary cough, dry cough phlegm
It is few, it coughs up phlegm not well.Cough-relieving pears soft extracts needs to carry out color during progress drug is declared for the menthol thin layer in drug
Spectrum identifies, and guarantees the ingredient and quality of drug, it is therefore desirable to correspondingly chromatographic identification method.Existing chromatographic identification method is being reflected
When other menthol thin layer, there is misalignment in chromatography colour developing, influences chromatography observation, and then influence identification quality, it is therefore desirable to
Menthol thin layer method is existing to solve the problems, such as in a kind of novel analysis cough-relieving pears soft extracts.
Summary of the invention
The object of the invention is that it is thin to provide menthol in a kind of analysis cough-relieving pears soft extracts to solve the above-mentioned problems
Layer method.
The present invention through the following technical solutions to achieve the above objectives:
Menthol thin layer method in a kind of analysis cough-relieving pears soft extracts, it the following steps are included:
Step 1: taking menthol 20g, add petroleum ether 25ml, concussion is extracted 1 hour, takes supernatant to wave to 1ml molten to get test sample
Liquid；
Step 2: separately taking menthol reference substance, add dehydrated alcohol that solution of every 1ml containing 2mg is made, as reference substance solution；
Step 3: testing, drawn in the step 1 according to thin-layered chromatography (one general rule 0502 of " Chinese Pharmacopoeia " version in 2015)
Test solution 10ul, the reference substance solution 5ul of the step 2 are put respectively on same silica GF254 lamellae, with first
Benzene-ethyl acetate is solvent, is unfolded, and takes out, dries；
Step 4: the test solution spray after being unfolded in the step 3 is heated with 5% vanillin-sulfuric acid-ethanol solution test solution at 105 DEG C
It is clear to spot development, then in ultraviolet light and observed under daylight, sample chromatogram, in position corresponding with reference substance chromatography
The spot of upper aobvious same color.
Further, the temperature of the petroleum ether in the step 1 will maintain 60 DEG C -90 DEG C.
Further, the Silica Gel Silica gel GF254 lamellae in the step 3 can also be substituted with silica G plate.
Further, the mixed proportion of toluene and ethyl acetate is 19:1 in the step 3.
Further, the mixed proportion of vanillin-sulfuric acid and ethanol solution is 1:4 in the step 4.
It analyzes the specific implementation step of menthol thin layer method in cough-relieving pears soft extracts: when identifying, first taking menthol 20g,
Petroleum ether (60-90 DEG C) or ether 25ml, soaked overnight after concussion is extracted 1 hour, take supernatant to be placed in evaporating dish, and solution is certainly
So+wave to about 1ml, as test solution, menthol reference substance is separately taken, adds dehydrated alcohol that solution of every 1ml containing 2mg is made,
It as reference substance solution, is tested according to thin-layered chromatography (one general rule 0502 of " Chinese Pharmacopoeia " version in 2015), it is molten to draw test sample
Liquid 10ul, reference substance solution 5ul put respectively on same silica GF254 lamellae, are with toluene-ethyl acetate (19:1)
Solvent is unfolded, and takes out, dries, and it is aobvious to be heated to spot at 105 DEG C with 5% vanillin-sulfuric acid-ethanol solution (1:4) test solution for spray
Color is clear, in sample chromatogram, shows the spot of same color at the position corresponding to the chromatogram of the reference substance.
The beneficial effects of the present invention are:
By using petroleum ether as extracting solution, with toluene-ethyl acetate solvent, be aobvious with 5% vanillin-sulfuric acid-ethanol solution
Toner, and using silica G plate as display board, so that the clear spot of the Chromatogram display of menthol thin layer, favorable reproducibility eliminate
Develop the color deviation.
Specific embodiment
The invention will be further described below:
Menthol thin layer method in a kind of analysis cough-relieving pears soft extracts, it the following steps are included:
Step 1: taking menthol 20g, add petroleum ether 25ml, concussion is extracted 1 hour, takes supernatant to wave to 1ml molten to get test sample
Liquid；
Step 2: separately taking menthol reference substance, add dehydrated alcohol that solution of every 1ml containing 2mg is made, as reference substance solution；
Step 3: testing, drawn in the step 1 according to thin-layered chromatography (one general rule 0502 of " Chinese Pharmacopoeia " version in 2015)
Test solution 10ul, the reference substance solution 5ul of the step 2 are put respectively on same silica GF254 lamellae, with first
Benzene-ethyl acetate is solvent, is unfolded, and takes out, dries；
Step 4: the test solution spray after being unfolded in the step 3 is heated with 5% vanillin-sulfuric acid-ethanol solution test solution at 105 DEG C
It is clear to spot development, then in ultraviolet light and observed under daylight, sample chromatogram, in position corresponding with reference substance chromatography
The spot of upper aobvious same color.
In the present embodiment, the temperature of the petroleum ether in the step 1 will maintain 60 DEG C -90 DEG C.
In the present embodiment, the Silica Gel Silica gel GF254 lamellae in the step 3 can also be substituted with silica G plate.
In the present embodiment, the mixed proportion of toluene and ethyl acetate is 19:1 in the step 3.
In the present embodiment, the mixed proportion of vanillin-sulfuric acid and ethanol solution is 1:4 in the step 4.
It analyzes the specific implementation step of menthol thin layer method in cough-relieving pears soft extracts: when identifying, first taking menthol 20g,
Petroleum ether (60-90 DEG C) or ether 25ml, soaked overnight after concussion is extracted 1 hour, take supernatant to be placed in evaporating dish, and solution is certainly
So+wave to about 1ml, as test solution, menthol reference substance is separately taken, adds dehydrated alcohol that solution of every 1ml containing 2mg is made,
It as reference substance solution, is tested according to thin-layered chromatography (one general rule 0502 of " Chinese Pharmacopoeia " version in 2015), it is molten to draw test sample
Liquid 10ul, reference substance solution 5ul put respectively on same silica GF254 lamellae, are with toluene-ethyl acetate (19:1)
Solvent is unfolded, and takes out, dries, and it is aobvious to be heated to spot at 105 DEG C with 5% vanillin-sulfuric acid-ethanol solution (1:4) test solution for spray
Color is clear, in sample chromatogram, shows the spot of same color at the position corresponding to the chromatogram of the reference substance.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. menthol thin layer method in a kind of analysis cough-relieving pears soft extracts, it is characterised in that: it the following steps are included:
Step 1: taking menthol 20g, add petroleum ether 25ml, concussion is extracted 1 hour, takes supernatant to wave to 1ml molten to get test sample
Liquid；
Step 2: separately taking menthol reference substance, add dehydrated alcohol that solution of every 1ml containing 2mg is made, as reference substance solution；
Step 3: testing, drawn in the step 1 according to thin-layered chromatography (one general rule 0502 of " Chinese Pharmacopoeia " version in 2015)
Test solution 10ul, the reference substance solution 5ul of the step 2 are put respectively on same silica GF254 lamellae, with first
Benzene-ethyl acetate is solvent, is unfolded, and takes out, dries；
Step 4: the test solution spray after being unfolded in the step 3 is heated with 5% vanillin-sulfuric acid-ethanol solution test solution at 105 DEG C
It is clear to spot development, then in ultraviolet light and observed under daylight, sample chromatogram, in position corresponding with reference substance chromatography
The spot of upper aobvious same color.
2. menthol thin layer method in a kind of analysis cough-relieving pears soft extracts according to claim 1, it is characterised in that: the step
The temperature of petroleum ether in rapid 1 will maintain 60 DEG C -90 DEG C.
3. menthol thin layer method in a kind of analysis cough-relieving pears soft extracts according to claim 1, it is characterised in that: the step
Silica Gel Silica gel GF254 lamellae in rapid 3 can also be substituted with silica G plate.
4. menthol thin layer method in a kind of analysis cough-relieving pears soft extracts according to claim 1, it is characterised in that: the step
The mixed proportion of toluene and ethyl acetate is 19:1 in rapid 3.
5. menthol thin layer method in a kind of analysis cough-relieving pears soft extracts according to claim 1, it is characterised in that: the step
The mixed proportion of vanillin-sulfuric acid and ethanol solution is 1:4 in rapid 4.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811463744.1A CN109521137A (en) | 2018-12-03 | 2018-12-03 | Menthol thin layer method in a kind of analysis cough-relieving pears soft extracts |
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| CN201811463744.1A CN109521137A (en) | 2018-12-03 | 2018-12-03 | Menthol thin layer method in a kind of analysis cough-relieving pears soft extracts |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020182260A1 (en) * | 1998-05-29 | 2002-12-05 | Cellegy Pharmaceuticals, Inc. | Anti-inflammatory agents and methods for their preparation and use |
| CN101138594A (en) * | 2006-09-04 | 2008-03-12 | 广西壮族自治区花红药业股份有限公司 | Quality control method of traditional chinese medicine preparation for treating traumatic injury and rheumatism ostealgia |
| CN101485762A (en) * | 2008-01-16 | 2009-07-22 | 韩勇 | Quality control method of Chinese medicine preparation |
| CN101744946A (en) * | 2010-01-15 | 2010-06-23 | 北京同仁堂科技发展股份有限公司 | Chinese medicinal composition and detection method for Chinese medicinal composition preparation |
| CN104897789A (en) * | 2015-03-17 | 2015-09-09 | 广西昌弘制药有限公司 | Quality control method for sore-throat-relieving and pain-relieving preparation |
| CN105616946A (en) * | 2015-10-29 | 2016-06-01 | 广东一力罗定制药有限公司 | Preparation for treating cough, preparation method and quality control method thereof |
-
2018
- 2018-12-03 CN CN201811463744.1A patent/CN109521137A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020182260A1 (en) * | 1998-05-29 | 2002-12-05 | Cellegy Pharmaceuticals, Inc. | Anti-inflammatory agents and methods for their preparation and use |
| CN101138594A (en) * | 2006-09-04 | 2008-03-12 | 广西壮族自治区花红药业股份有限公司 | Quality control method of traditional chinese medicine preparation for treating traumatic injury and rheumatism ostealgia |
| CN101485762A (en) * | 2008-01-16 | 2009-07-22 | 韩勇 | Quality control method of Chinese medicine preparation |
| CN101744946A (en) * | 2010-01-15 | 2010-06-23 | 北京同仁堂科技发展股份有限公司 | Chinese medicinal composition and detection method for Chinese medicinal composition preparation |
| CN104897789A (en) * | 2015-03-17 | 2015-09-09 | 广西昌弘制药有限公司 | Quality control method for sore-throat-relieving and pain-relieving preparation |
| CN105616946A (en) * | 2015-10-29 | 2016-06-01 | 广东一力罗定制药有限公司 | Preparation for treating cough, preparation method and quality control method thereof |
Non-Patent Citations (5)
| Title |
|---|
| ALINA PYKA 等: "Application of topological indexes for evaluation of the TLC separation of selected essential oil components", 《ACTA POLONIAC PHARMACCUTICA-DRUG RESEARCH》 * |
| 伍小勇等: "TLC法鉴别复方鱼肝油滴鼻液中薄荷脑成分 ", 《解放军药学学报》 * |
| 刘文志 等: "蜜炼强力枇杷膏质量标准研究", 《中药材》 * |
| 李嘉华 等: "活络止痛膏的质量标准研究", 《中医药导报》 * |
| 马俊奇等: "薄荷桉油片(Ⅰ)中薄荷脑薄层色谱鉴别方法的改进", 《北方药学》 * |
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