CN102023193A - Ephedra medicinal material identification method - Google Patents
Ephedra medicinal material identification method Download PDFInfo
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- CN102023193A CN102023193A CN2010105044864A CN201010504486A CN102023193A CN 102023193 A CN102023193 A CN 102023193A CN 2010105044864 A CN2010105044864 A CN 2010105044864A CN 201010504486 A CN201010504486 A CN 201010504486A CN 102023193 A CN102023193 A CN 102023193A
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- chinese ephedra
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- methyl alcohol
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Abstract
The invention discloses an ephedra medicinal material identification method, comprising the following steps: preparing a reference substance solution and a test solution; and carrying out the steps such as sample application, stretching, viewing or inspection and the like. In the invention, the ultrasonic cavatition is utilized to damage the cells of plant medicinal materials, so as to enable the solvent to permeate into the cells easily, and meanwhile, the ultrasonic mechanical movement, emulsification, diffusion, crushing, chemical effect and the like can accelerate the diffusion, releasing and dissolving of the effective components in the cells, thus promoting the speed of the extraction. In the invention, only one organic solvent, namely methyl alcohol is used, ultrasonic processing is utilized to replace the operations such as heating, backflow, drying by distillation and the like in the prior art, thus the categories of the used organic solvents are greatly reduced, a large quantity of organic solvents are prevented from being evaporated to air to pollute the environment and harm the health, and the identification time is ensured to be greatly shortened, and the cost is lowered. The identification method is suitable for identifying the effective components of the traditional Chinese medicine raw material ephedra.
Description
Technical field
The invention belongs to the drug ingedient detection range, specifically a kind of discrimination method of Chinese ephedra medicinal material.
Background technology
Chinese ephedra is the dry herbaceous stem stem of Ephedraceae plant plait Chinese ephedra (Ephedra sinica Stapf), epheday intermedia (Ephedra intermedia Schrenk et C.A.Mey.) or ephedra equisetina (Ephedra equisetina Bge.), it is warm in nature, flavor is hot, be important simply diaphoretic medicine, have effects such as Pulvis Diaphoreticus is trembled with fear, freeinged lung and relieving asthma, inducing diuresis for removing edema.
Chinese ephedra is medicinal herbs most in use simply, dragons and fishes jumbled together for the Chinese ephedra medicinal material that circulates on the market, pseudo-product ephedra likiangensis Florin, Ephedra przewalskii are for example arranged, even some illegal businessman serves as the Chinese ephedra sale with the woody stems of Chinese ephedra, therefore be the true and false of determining Chinese ephedra, the quality that guarantees Chinese ephedra, discrimination method is vital accurately and efficiently.Present stage, thin-layer chromatography commonly used was tentatively differentiated Chinese ephedra, and employing adds the organic solvent reflux after adding alkali in this method, filters, with the filtrate evaporate to dryness, use a certain amount of dissolution with solvents as need testing solution again, for example 05 edition pharmacopeia sample treatment is: sample thief 1g, add strong ammonia solution number droplet, add methenyl choloride 10ml, reflux 1 hour filters, the filtrate evaporate to dryness, residue adds methyl alcohol 2ml shake well, filters, and filtrate is operated as need testing solution again.This discrimination method is not only lost time, the waste resource, and the cost height, and also a large amount of organic solvent evaporate into and causes environmental pollution in the air, and human body is produced harm.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of discrimination method of Chinese ephedra medicinal material, can overcome the above-mentioned defective of existing in prior technology, have accurately, efficient, saving of labor, save time, the characteristics of safety and environmentally safe.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
A kind of discrimination method of Chinese ephedra medicinal material, it carries out according to the following steps order:
A. prepare need testing solution: get Chinese ephedra medicinal material sample and add methyl alcohol in right amount, wherein the volume of methyl alcohol is 1～6ml: 1g with the ratio of Chinese ephedra medicinal material sample quality; Sonicated 5～30min filters, and gets filtrate and promptly gets need testing solution, and is standby;
B. prepare reference substance solution: get the Chinese ephedra control medicinal material of having identified and add methyl alcohol in right amount, wherein the volume of methyl alcohol is 1～6ml: 1g with the ratio of Chinese ephedra medicinal material sample quality; Sonicated 5～30min filters, and gets filtrate and promptly gets reference substance solution, and is standby;
C. point sample: draw above-mentioned need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate;
D. launch: with methenyl choloride-methyl alcohol-strong ammonia solution volume ratio be 20: 5: 0.5 mixed liquor as developping agent, launch;
E. inspect: take out silica gel g thin-layer plate, dry, spray is with ninhydrin solution, it is clear to be heated to spot colour developing at 105 ℃, in the test sample chromatogram, with the corresponding position of reference substance medicinal material chromatogram on, observe and whether manifest identical punctation, and judgement sample genuine piece Chinese ephedra whether according to this, if that is: manifest identical punctation, then sample is the genuine piece Chinese ephedra; If it is not identical manifesting the result, then sample is pseudo-product Chinese ephedra.
So far, the quality of having finished the medicinal material sample is differentiated.
Illustrate:, medicinal material can't be immersed fully make extraction not exclusively in the solvent 1. because the consumption of methyl alcohol is few; And methanol usage is excessive, and the concentration of the composition of examining is too low, may be speckless, and can't realize authentication purposes.Therefore the effective range with the volume of methyl alcohol and the ratio of Chinese ephedra medicinal material sample quality is defined as 1～6ml: 1g.2. sonicated is time qualified is 5～30min, short again can the extraction not exclusively of time, and the time has oversizely been run counter to original intention of the present invention.3. developping agent is preferably the mixed liquor of methenyl choloride-methyl alcohol-strong ammonia solution, and reason is that the composition of examining is an alkaloids in the Chinese ephedra, and adding dense ammonia test is to examine composition to exist with single form in order to guarantee; The foundation that three's ratio is selected is to adjust the polarity of developping agent, guarantees to launch the best as a result.Be heated to spot at 105 ℃ when 4. inspecting, this temperature is such testing routine temperature.5. inspecting " identical " described in the step, to mean the color that manifests spot identical.
As qualification of the present invention,
Described sonicated can be to carry out under frequency 42KHz, power 120W condition.
Described sonicated also can be to carry out under frequency 40KHz, power 100 conditions.
Last said conditions is the performance parameter of laboratory common equipment.
As optimization of the present invention, the volume of methyl alcohol is 6: 1 with the ratio of the quality of Chinese ephedra medicinal material sample among the described step a.
This proportioning is an optimal proportion, and the extracts active ingredients effect of medicinal material is best, and identification result is the most accurate.
The present invention utilizes cavitation effect of ultrasonic waves, destroy the cell of vegetable drug, make solvent be easy to infiltrate in the cell, hyperacoustic mechanical motion, emulsification simultaneously, spread, smash, diffusion, release and dissolving that chemical effect etc. can be quickened effective constituent cell in, promote carrying out fast of extraction.The present invention only uses a kind of organic solvent---and methyl alcohol and use sonicated replace operations such as reflux of the prior art, evaporate to dryness, make that not only the organic solvent kind of using greatly reduces, avoided a large amount of organic solvents to be evaporated to contaminated environment in the air, health risk, and making the used time of discriminating also shorten dramatically, cost reduces.
To sum up, compared with prior art, the obtained technical progress of the present invention is:
(1) save time: sonicated fast, efficiently;
(2) save resource: only use a kind of organic solvent, and without reflux and evaporate to dryness, save solvent, save the power and water equal energy source, cost is low;
(3) reduce pollution: almost do not have organic solvent emission in air, environmental pollution is little, is not detrimental to health.
The present invention is suitable for the effective constituent of Chinese medicine bulk drug Chinese ephedra is differentiated.
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment
The discrimination method of 1 one kinds of Chinese ephedra medicinal materials of embodiment
This discrimination method carries out according to the following steps order:
A1. prepare need testing solution: get Chinese ephedra medicinal material sample 0.5g, add methyl alcohol 3ml, sonicated 10min (frequency 40KHz, power 100W) filters, and gets filtrate and promptly gets need testing solution, and is standby;
B1. prepare reference substance solution: get Chinese ephedra control medicinal material 0.5g, add methyl alcohol 3ml, sonicated 10min (frequency 40KHz, power 100W) filters, and gets filtrate and promptly gets reference substance solution, and is standby;
C1. point sample: draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate;
D1. launch: with methenyl choloride-methyl alcohol-strong ammonia solution volume ratio is developping agent at 20: 5: 0.5, launches;
E1. inspect: take out silica gel g thin-layer plate, dry, spray is with ninhydrin solution, it is clear to be heated to spot colour developing at 105 ℃, in the test sample chromatogram, with the corresponding position of reference substance medicinal material chromatogram on, observe and whether manifest identical punctation, and judgement sample genuine piece Chinese ephedra whether according to this, if that is: manifest identical punctation, then sample is the genuine piece Chinese ephedra; If it is not identical manifesting the result, then sample is pseudo-product Chinese ephedra.
2 one kinds of embodiment
The discrimination method of Chinese ephedra medicinal material
This discrimination method carries out according to the following steps order:
A2. prepare need testing solution: get Chinese ephedra control medicinal material 1g, add methyl alcohol 5ml, sonicated 5min (frequency 42KHz, power 120W) filters, and gets filtrate and promptly gets reference substance solution, and is standby;
B2. prepare reference substance solution: get the Chinese ephedra control medicinal material, add methyl alcohol 5ml; Sonicated 5min (frequency 42KHz, power 120W) filters, and gets filtrate and promptly gets reference substance solution, and is standby;
C2. point sample: draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate;
D2. launch: with methenyl choloride-methyl alcohol-strong ammonia solution volume ratio is developping agent at 20: 5: 0.5, launches;
E2. inspect: take out silica gel g thin-layer plate, dry, spray is with ninhydrin solution, it is clear to be heated to spot colour developing at 105 ℃, in the test sample chromatogram, with the corresponding position of reference substance medicinal material chromatogram on, observe and whether manifest identical punctation, and judgement sample genuine piece Chinese ephedra whether according to this, if that is: manifest identical punctation, then sample is the genuine piece Chinese ephedra; If it is not identical manifesting the result, then sample is pseudo-product Chinese ephedra.
The discrimination method of 3 one kinds of Chinese ephedra medicinal materials of embodiment
This discrimination method carries out according to the following steps order:
A3. prepare need testing solution: get Chinese ephedra medicinal material sample 1g, add methyl alcohol 1ml, sonicated 20min (frequency 40KHz, power 100W) filters, and gets filtrate and promptly gets need testing solution, and is standby;
B3. prepare reference substance solution: get Chinese ephedra control medicinal material 1g, add methyl alcohol 1ml, sonicated 20min (frequency 40KHz, power 100W) filters, and gets filtrate and promptly gets reference substance solution, and is standby;
C3. point sample: draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate;
D3. launch: with methenyl choloride-methyl alcohol-strong ammonia solution volume ratio is developping agent at 20: 5: 0.5, launches;
E3. inspect: take out silica gel g thin-layer plate, dry, spray is with ninhydrin solution, it is clear to be heated to spot colour developing at 105 ℃, in the test sample chromatogram, with the corresponding position of reference substance medicinal material chromatogram on, observe and whether manifest identical punctation, and judgement sample genuine piece Chinese ephedra whether according to this, if that is: manifest identical punctation, then sample is the genuine piece Chinese ephedra; If it is not identical manifesting the result, then sample is pseudo-product Chinese ephedra.
The discrimination method of 4 one kinds of Chinese ephedra medicinal materials of embodiment
This discrimination method carries out according to the following steps order:
A4. prepare need testing solution: get Chinese ephedra medicinal material sample 0.5g, add methyl alcohol 2ml, sonicated 25min (frequency 42KHz, power 120W) filters, and gets filtrate and promptly gets need testing solution, and is standby;
B4. prepare reference substance solution: get Chinese ephedra control medicinal material 0.5g, add methyl alcohol 2ml, sonicated 25min (frequency 42KHz, power 120W) filters, and gets filtrate and promptly gets reference substance solution, and is standby;
C4. point sample: draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate;
D4. launch: with methenyl choloride-methyl alcohol-strong ammonia solution volume ratio is developping agent at 20: 5: 0.5, launches;
E4. inspect: take out silica gel g thin-layer plate, dry, spray is with ninhydrin solution, it is clear to be heated to spot colour developing at 105 ℃, in the test sample chromatogram, with the corresponding position of reference substance medicinal material chromatogram on, observe and whether manifest identical punctation, and judgement sample genuine piece Chinese ephedra whether according to this, if that is: manifest identical punctation, then sample is the genuine piece Chinese ephedra; If it is not identical manifesting the result, then sample is pseudo-product Chinese ephedra.
The discrimination method of 5 one kinds of Chinese ephedra medicinal materials of embodiment
This discrimination method carries out according to the following steps order:
A5. prepare need testing solution: get Chinese ephedra medicinal material sample 0.3g, add methyl alcohol 1ml, sonicated 30min (frequency 40KHz, power 100W) filters, and gets filtrate and promptly gets need testing solution, and is standby;
B5. prepare reference substance solution: get Chinese ephedra control medicinal material 0.3g, add methyl alcohol 1ml, sonicated 30min (frequency 40KHz, power 100W) filters, and gets filtrate and promptly gets reference substance solution, and is standby;
C5. point sample: draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate;
D5. launch: with methenyl choloride-methyl alcohol-strong ammonia solution volume ratio is developping agent at 20: 5: 0.5, launches;
E5. inspect: take out silica gel g thin-layer plate, dry, spray is with ninhydrin solution, it is clear to be heated to spot colour developing at 105 ℃, in the test sample chromatogram, with the corresponding position of reference substance medicinal material chromatogram on, observe and whether manifest identical punctation, and judgement sample genuine piece Chinese ephedra whether according to this, if that is: manifest identical punctation, then sample is the genuine piece Chinese ephedra; If it is not identical manifesting the result, then sample is pseudo-product Chinese ephedra.
Claims (4)
1. the discrimination method of a Chinese ephedra medicinal material is characterized in that it carries out according to the following steps order:
A. prepare need testing solution: get Chinese ephedra medicinal material sample and add methyl alcohol in right amount, wherein the volume of methyl alcohol is 1～6ml: 1g with the ratio of Chinese ephedra medicinal material sample quality; Sonicated 5～30min filters, and gets filtrate and promptly gets need testing solution, and is standby;
B. prepare reference substance solution: get the Chinese ephedra control medicinal material of having identified and add methyl alcohol in right amount, wherein the volume of methyl alcohol is 1～6ml: 1g with the ratio of Chinese ephedra medicinal material sample quality; Sonicated 5～30min filters, and gets filtrate and promptly gets reference substance solution, and is standby;
C. point sample: draw above-mentioned need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate;
D. launch: with methenyl choloride-methyl alcohol-strong ammonia solution volume ratio be 20: 5: 0.5 mixed liquor as developping agent, launch;
E. inspect: take out silica gel g thin-layer plate, dry, spray is with ninhydrin solution, it is clear to be heated to spot colour developing at 105 ℃, in the test sample chromatogram, with the corresponding position of reference substance medicinal material chromatogram on, observe and whether manifest identical punctation, and judgement sample genuine piece Chinese ephedra whether according to this, if that is: manifest identical punctation, then sample is the genuine piece Chinese ephedra; If it is not identical manifesting the result, then sample is pseudo-product Chinese ephedra.
2. the discrimination method of Chinese ephedra medicinal material according to claim 1 is characterized in that: described sonicated can be to carry out under frequency 42KHz, power 120W condition.
3. the discrimination method of Chinese ephedra medicinal material according to claim 1 is characterized in that: described sonicated also can be to carry out under frequency 40KHz, power 100W condition.
4. according to the discrimination method of each described Chinese ephedra medicinal material among the claim 1-3, it is characterized in that: as optimization of the present invention, the volume of methyl alcohol described in the described step a is 6: 1 with the ratio of the quality of Chinese ephedra medicinal material sample.
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| CN2010105044864A CN102023193A (en) | 2010-10-13 | 2010-10-13 | Ephedra medicinal material identification method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109115544A (en) * | 2018-08-02 | 2019-01-01 | 安徽科技学院 | A method of it is sliced using decalcification method production bone tissue |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101637587A (en) * | 2009-08-27 | 2010-02-03 | 贵州百灵企业集团制药股份有限公司 | Quality detecting method for cough relieving granule |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101637587A (en) * | 2009-08-27 | 2010-02-03 | 贵州百灵企业集团制药股份有限公司 | Quality detecting method for cough relieving granule |
Non-Patent Citations (1)
| Title |
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| 《中华人民共和国药典》 20050131 国家药典委员会 麻黄 第224页 1-4 , 1 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109115544A (en) * | 2018-08-02 | 2019-01-01 | 安徽科技学院 | A method of it is sliced using decalcification method production bone tissue |
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Application publication date: 20110420 |