CN107478763B - A kind of measuring method of whorlleaf oxytropis herb - Google Patents
A kind of measuring method of whorlleaf oxytropis herb Download PDFInfo
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- CN107478763B CN107478763B CN201710912604.7A CN201710912604A CN107478763B CN 107478763 B CN107478763 B CN 107478763B CN 201710912604 A CN201710912604 A CN 201710912604A CN 107478763 B CN107478763 B CN 107478763B
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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
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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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/94—Development
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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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses a kind of measuring methods of whorlleaf oxytropis herb, whorlleaf oxytropis herb is measured using thin-layer chromatography, it include: to take untested medicinal material, it is finely ground, sieving, methanol ultrasound is added, it is extracted with ethyl acetate, test solution is prepared with dehydrated alcohol dissolution after being concentrated to dryness, whorlleaf oxytropis herb control medicinal material solution is separately prepared using same method, above two solution is put respectively on the silica gel g thin-layer plate in same using sodium carboxymethylcellulose as binder, using petroleum ether-hexamethylene-toluene-ethyl acetate as solvent, expansion, it takes out, it dries, spray is with ethanol solution of sulfuric acid, wind is clear to spot development, in sample chromatogram, on position corresponding with reference medicine chromatography, the spot of aobvious same color.Measuring method of the present invention has many advantages, such as that favorable reproducibility, specificity are strong, result is accurate, meets accurate, easy, sensitive, quick principle, can effectively detect the quality of this Chinese medicine of whorlleaf oxytropis herb.
Description
Technical field
The present invention relates to a kind of measuring methods of Chinese medicine, and in particular to the measuring method of this Chinese medicine of whorlleaf oxytropis herb.
Background technique
Whorlleaf oxytropis herb is the herb of pulse family Oxytropis Species whorlleaf oxytropis herb also known as Tibetan crazyweed, beats summer, Da Xia, is born in height above sea level
The scree of 4500-5200m, mountain top, patana, river shoal, lake basin etc., be distributed mainly on Xinjiang, Sichuan, Tibet etc.
Ground has effects that antidiarrheal, hemostasis, removing toxicity for detumescence, cures mainly enteritis, diarrhea, wound hemorrhage, boil swelling and pain, be it is a kind of it is common in
Medicinal material.
But complex chemical composition contained by whorlleaf oxytropis herb, it has existed in the prior art and whorlleaf oxytropis herb chemical component is ground
Study carefully (chemical constitution study of whorlleaf oxytropis herb, Yao Shuying etc., " CHINA JOURNAL OF CHINESE MATERIA MEDICA ", the 16th phase of volume 32,1660-1662
Page), but so far still without the relevant criterion detected to its quality, for this purpose, applicant after study, propose it is a kind of pass through it is thin
Layer chromatography carries out mirror method for distinguishing to this Chinese medicine.
Summary of the invention
Therefore, the purpose of the present invention is to provide a kind of sides being measured by thin layer chromatography to whorlleaf oxytropis herb
Method is controlled with this to realize the quality to this Chinese medicine of whorlleaf oxytropis herb.Measuring method step described herein is simple,
It is easy to implement, and can effectively control the quality of this Chinese medicine.
For above-mentioned purpose, technical scheme is as follows:
A kind of measuring method of whorlleaf oxytropis herb, it is characterised in that: whorlleaf oxytropis herb is determined using thin layer chromatography
Property identify, specifically include:
Untested medicinal material 0.2-0.5g is taken, it is finely ground, 80 meshes are crossed, 20-50mL methanol is added to be ultrasonically treated, filtering, filtrate volatilizes
It after methanol, is dissolved with dehydrated alcohol, dissolved solution is extracted with ethyl acetate, and is concentrated to dryness, and is dissolved to 1- with dehydrated alcohol
2mL separately takes control medicinal material 0.2-0.5g as test solution, prepares wheel blade with preparation method same as test solution
Whin control medicinal material solution, draws test solution and each 10-15 μ L of control medicinal material solution is put respectively in same with carboxymethyl fibre
Tieing up plain sodium is to be unfolded on the silica gel g thin-layer plate of binder with solvent, takes out, dries, spray is 10-15% with percent by volume
Ethanol solution of sulfuric acid, wind is clear to spot development, in sample chromatogram, on position corresponding with reference medicine chromatography, show
The spot of same color.
Further, the solvent is petroleum ether-hexamethylene-toluene-ethyl acetate mixed solution.
Further, untested medicinal material 0.3g is taken, it is finely ground, 80 meshes are crossed, 30mL methanol is added to be ultrasonically treated.
Further, 1mL is dissolved to dehydrated alcohol after extracting, being concentrated to dryness.
Further, it draws test solution and each 10 μ L of control medicinal material solution is put in same with carboxymethyl cellulose respectively
Sodium is on the silica gel g thin-layer plate of binder.
Further, petroleum ether-hexamethylene-toluene-ethyl acetate volume ratio in the solvent are as follows: 4-7:10-20:
8-15:5-9.
Further, petroleum ether-hexamethylene-toluene-ethyl acetate volume ratio in the solvent are as follows: 5-6:13-18:
10-12:6-8.
Further, petroleum ether-hexamethylene-toluene-ethyl acetate volume ratio in the solvent are as follows: 5:15:11:8.
Further, the percent by volume of the ethanol solution of sulfuric acid is 12%.
Compared with the prior art, the beneficial effect of measuring method of the present invention is:
The present invention directly controls the quality of this Chinese medicine of whorlleaf oxytropis herb by thin layer chromatography, fills up
Blank in the prior art；The present invention, as solvent, has reproducibility using toluene-cyclohexane-ethyl acetate-petroleum ether
Well, the advantages that specificity is strong, result is accurate, meets accurate, easy, sensitive, quick principle, can effectively detect wheel blade spine
The quality of this Chinese medicine of beans.
Detailed description of the invention
Fig. 1 is the thin-layer chromatogram of measuring method described in the embodiment of the present invention 1；
Fig. 2 is the thin-layer chromatogram of measuring method described in the embodiment of the present invention 2；
Fig. 3 is the thin-layer chromatogram of measuring method described in the embodiment of the present invention 3；
Wherein, a is test solution, and b is control medicinal material solution.
Specific embodiment
Embodiment 1:
Untested medicinal material 0.3g is taken, it is finely ground, 80 meshes are crossed, 30mL methanol is added to be ultrasonically treated, filtering, after filtrate volatilizes methanol,
It is dissolved with dehydrated alcohol, dissolved solution is extracted with ethyl acetate, and is concentrated to dryness, and 1mL is dissolved to dehydrated alcohol, as confession
Test sample solution separately takes control medicinal material 0.3g, and it is molten to prepare whorlleaf oxytropis herb control medicinal material with preparation method same as test solution
Liquid, draws test solution and each 10 μ L of control medicinal material solution is put respectively in same using sodium carboxymethylcellulose as the silicon of binder
On glue G lamellae, with petroleum ether-hexamethylene-toluene-ethyl acetate (volume ratio are as follows: 5:15:11:8) for solvent, expansion is taken
Out, dry, spray with percent by volume be 12% ethanol solution of sulfuric acid, wind is clear to spot development, in sample chromatogram, with
On the corresponding position of reference medicine chromatography, the spot of same color is shown.
Embodiment 2:
Untested medicinal material 0.2g is taken, it is finely ground, 80 meshes are crossed, 20mL methanol is added to be ultrasonically treated, filtering, after filtrate volatilizes methanol,
It is dissolved with dehydrated alcohol, dissolved solution is extracted with ethyl acetate, and is concentrated to dryness, and 1mL is dissolved to dehydrated alcohol, as confession
Test sample solution separately takes control medicinal material 0.2g, and it is molten to prepare whorlleaf oxytropis herb control medicinal material with preparation method same as test solution
Liquid, draws test solution and each 12 μ L of control medicinal material solution is put respectively in same using sodium carboxymethylcellulose as the silicon of binder
On glue G lamellae, with petroleum ether-hexamethylene-toluene-ethyl acetate (volume ratio are as follows: 4:16:10:6) for solvent, expansion is taken
Out, dry, spray with percent by volume be 10% ethanol solution of sulfuric acid, wind is clear to spot development, in sample chromatogram, with
On the corresponding position of reference medicine chromatography, the spot of same color is shown.
Embodiment 3:
Untested medicinal material 0.5g is taken, it is finely ground, 80 meshes are crossed, 50mL methanol is added to be ultrasonically treated, filtering, after filtrate volatilizes methanol,
It is dissolved with dehydrated alcohol, dissolved solution is extracted with ethyl acetate, and is concentrated to dryness, and 2mL is dissolved to dehydrated alcohol, as confession
Test sample solution separately takes control medicinal material 0.5g, and it is molten to prepare whorlleaf oxytropis herb control medicinal material with preparation method same as test solution
Liquid, draws test solution and each 15 μ L of control medicinal material solution is put respectively in same using sodium carboxymethylcellulose as the silicon of binder
On glue G lamellae, with petroleum ether-hexamethylene-toluene-ethyl acetate (volume ratio are as follows: 7:20:15:9) for solvent, expansion is taken
Out, dry, spray with percent by volume be 15% ethanol solution of sulfuric acid, wind is clear to spot development, in sample chromatogram, with
On the corresponding position of reference medicine chromatography, the spot of same color is shown.
The above is only presently preferred embodiments of the present invention, is not intended to limit the scope of the present invention, current row
The technical staff of industry can make some deformations and modification, all technologies according to the present invention under the inspiration of the technical program
Essence still falls within the range of technical solution of the present invention to any modification, equivalent variations and modification made by above embodiment
It is interior.
Claims (7)
1. a kind of measuring method of whorlleaf oxytropis herb, it is characterised in that: carried out using thin layer chromatography to whorlleaf oxytropis herb qualitative
Identify, specifically include:
Untested medicinal material 0.2-0.5g is taken, it is finely ground, 80 meshes are crossed, 20-50mL methanol is added to be ultrasonically treated, filtering, filtrate volatilizes methanol
Afterwards, it being dissolved with dehydrated alcohol, dissolved solution is extracted with ethyl acetate, and is concentrated to dryness, it is dissolved to 1-2mL with dehydrated alcohol,
As test solution, control medicinal material 0.2-0.5g is separately taken, prepares whorlleaf oxytropis herb with preparation method same as test solution
Control medicinal material solution, draws test solution and each 10-15 μ L of control medicinal material solution is put in same with carboxymethyl cellulose respectively
Sodium is to be unfolded on the silica gel g thin-layer plate of binder with solvent, takes out, dries, spray is the sulphur of 10-15% with percent by volume
Sour ethanol solution, wind is clear to spot development, in sample chromatogram, on position corresponding with reference medicine chromatography, shows identical
The spot of color；
The solvent is petroleum ether-hexamethylene-toluene-ethyl acetate mixed solution, petroleum ether-hexamethylene in the solvent
Alkane-toluene-ethyl acetate volume ratio are as follows: 4-7:10-20:8-15:5-9.
2. a kind of measuring method of whorlleaf oxytropis herb according to claim 1, it is characterised in that: take untested medicinal material 0.3g, grind
Carefully, 80 meshes are crossed, 30mL methanol is added to be ultrasonically treated.
3. a kind of measuring method of whorlleaf oxytropis herb according to claim 1, it is characterised in that: extract, be concentrated to dryness after use
Dehydrated alcohol is dissolved to 1mL.
4. a kind of measuring method of whorlleaf oxytropis herb according to claim 1, it is characterised in that: draw test solution and right
It is put on the silica gel g thin-layer plate in same using sodium carboxymethylcellulose as binder respectively according to each 10 μ L of medicinal material solution.
5. a kind of measuring method of whorlleaf oxytropis herb according to claim 1, it is characterised in that: petroleum in the solvent
Ether-hexamethylene-toluene-ethyl acetate volume ratio are as follows: 5-6:13-18:10-12:6-8.
6. a kind of measuring method of whorlleaf oxytropis herb according to claim 5, it is characterised in that: petroleum in the solvent
Ether-hexamethylene-toluene-ethyl acetate volume ratio are as follows: 5:15:11:8.
7. a kind of measuring method of whorlleaf oxytropis herb according to claim 1, it is characterised in that: the ethanol solution of sulfuric acid
Percent by volume is 12%.
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| CN103852554B (en) * | 2012-11-30 | 2015-11-18 | 山东金诃药物研究开发有限公司 | A kind of Tibetan medicinal composition whin disappears the quality determining method of preparation of itching |
| CN103076424B (en) * | 2012-12-26 | 2014-12-17 | 甘肃奇正藏药有限公司 | Oxytropis medical material and detection method of oxytropis medical material preparation |
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