CN105548452A - Thin-layer chromatography detection method of cape jasmines in heat-clearing and detoxifying powder - Google Patents
Thin-layer chromatography detection method of cape jasmines in heat-clearing and detoxifying powder Download PDFInfo
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- CN105548452A CN105548452A CN201610080397.9A CN201610080397A CN105548452A CN 105548452 A CN105548452 A CN 105548452A CN 201610080397 A CN201610080397 A CN 201610080397A CN 105548452 A CN105548452 A CN 105548452A
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- G—PHYSICS
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- 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
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Abstract
The invention discloses a thin-layer chromatography detection method of cape jasmines in heat-clearing and detoxifying powder, aiming at solving the problem of a thin-layer chromatography detection method of the cape jasmines in the heat-clearing and detoxifying powder in the prior art that the effect is relatively poor. The thin-layer chromatography detection method comprises the following steps: (1) preparing a test sample liquid taking 2g of the heat-clearing and detoxifying powder and adding 25ml of methanol with the concentration of 50%; carrying out ultrasonic treatment for 40 minutes; filtering and evaporating filtrate; adding 2mL of methanol and dissolving; (2) sucking the test sample solution and dropping the liquid on a silica gel thin-layer plate; taking ethyl acetate, acetone, formic acid and water at the ratio of 5 to 5 to 1 to 1 as a developing agent, and developing; taking out a product and airing; and (3) spraying a sulfuric acid ethanol solution and heating until spots are clear. The thin-layer chromatography detection method has the advantages that the developing property is excellent, other ingredients in the heat-clearing and detoxifying powder have no influences on detection effect of the cape jasmines, a spot separation degree in a map is extremely good and the like.
Description
Technical field
The present invention relates to a kind of detection method, be specifically related to the thin-layered chromatography detection method of cape jasmine in qingwen baidu powder.
Background technology
Qingwen baidu powder is the recipe that teacher is stupid formulated more than the Qing Dynasty famous warm disease scholar, is loaded in " A View of Epidemic Febrile Diseases with Rashes " that it shows in book, now includes in " People's Republic of China's veterinary drug allusion quotation " version two in 2010.This medicine is made up of 14 taste medicinal materials such as gypsum, glutinous rehmannia, cornu bubali, the coptiss, is " Baihu Tang ", " huanglian jiedu decoction " and " xijiao Dihuang Tang " tripartite's addition or subtraction of changes and obtaining.The prescription of qingwen baidu powder comprises: plaster stone 120g, radix rehmanniae recen 30g, cornu bubali 60g, coptis 20g, cape jasmine 30g, moutan bark 20g, root of large-flowered skullcap 25g, radix paeoniae rubrathe 25g, radix scrophulariae 25g, wind-weed 30g, capsule of weeping forsythia 30g, balloonflower root 25g, Radix Glycyrrhizae 15g, lophatherum gracile 25g; There is purging intense heat and detonicating, effect of cool blood, be mainly used in treating heat poison clinically at veterinary drug and send out spot, unconsciousness due to high fever.
The quality standard of version " People's Republic of China's veterinary drug allusion quotation " two middle qingwen baidu powders in 2010 only has the TLC distinguish of microscopical characters and the coptis, is difficult to control its quality, ensures the security of product, validity and quality controllability.But the effect of the thin-layer identification method of cape jasmine disclosed in prior art is poor, can not satisfy the demands.
Summary of the invention
Technical matters to be solved by this invention is: in prior art, qingwen baidu powder is poor by cape jasmine thin-layer identification method effect, and object is to provide the thin-layered chromatography detection method of cape jasmine in the qingwen baidu powder of Detection results excellence.
The present invention is achieved through the following technical solutions:
The thin-layered chromatography detection method of cape jasmine in qingwen baidu powder, comprises the following steps:
(1) preparation of need testing solution: get qingwen baidu powder 2g, adds the methyl alcohol 25ml that concentration is 50%, ultrasonic 40min, and filter, filtrate evaporate to dryness, adds methyl alcohol 2mL and dissolve;
(2) draw need testing solution point on silica gel thin-layer plate, with ratio be 5: 5: 1: 1 ethyl acetate, acetone, formic acid and water for developping agent, launch, take out, dry;
(3) spray is with ethanol solution of sulfuric acid, is then heated to clear spot;
The developping agent combination variety that in prior art, the TLC distinguish of this cape jasmine adopts is various, but because each composition in different pharmaceutical is different, be applicable to the discriminating that the array mode of the cape jasmine TLC distinguish developping agent of other drug and proportion of composing can not be applicable to cape jasmine in qingwen baidu powder of the present invention.And the processing mode of need testing solution also can shine into larger impact to testing result.
After developping agent by said ratio and the processing mode to need testing solution combine, again need testing solution is launched, its expanding performance is excellent, in qingwen baidu powder other constituents on cape jasmine without impact, and by Chromatogram display known, adopt method of the present invention, in the chromatogram of need testing solution, spot degree of separation is splendid, the position corresponding with the chromatogram of control medicinal material solution, the spot of the Chromatogram display same color of need testing solution, and negative sample solution is noiseless.
In order to reach best separating effect, described silica gel thin-layer plate adopts silica gel g thin-layer plate.
Preferably, the concentration of described ethanol solution of sulfuric acid is 10%, and heating-up temperature is 110 DEG C.
Further, described silica gel thin-layer plate also has control medicinal material solution, reference substance solution, with negative sample solution, the preparation method of this control medicinal material solution, reference substance solution and negative sample solution is as follows:
Get control medicinal material cape jasmine 0.5g, add the methyl alcohol 25ml that concentration is 50%, ultrasonic 40min, filter, filtrate evaporate to dryness, adds methyl alcohol 2mL and dissolves, namely make control medicinal material solution;
Get reference substance Gardenoside again, add methyl alcohol and make the solution of every 1ml containing 4mg Gardenoside, make reference substance solution;
First configure the qingwen baidu powder prescription not comprising cape jasmine, get 1/500 of recipe quantity, add the methyl alcohol 25ml that concentration is 50%, ultrasonic 40min, filter, filtrate evaporate to dryness, adds methyl alcohol 2mL and dissolves, namely make negative sample solution.
The present invention compared with prior art, has following advantage and beneficial effect:
The expanding performance of detection method is excellent, and in qingwen baidu powder, other constituents are on cape jasmine Detection results without impact, and in the chromatogram of need testing solution, spot degree of separation is splendid, and negative sample solution is noiseless to it, effect highly significant.
Accompanying drawing explanation
Described herein
accompanying drawingbe used to provide the further understanding to the embodiment of the present invention, form a application's part, do not form the restriction to the embodiment of the present invention.?
in accompanying drawing:
fig. 1for the thin-layer chromatography of embodiment 1
figure.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with embodiment and
accompanying drawing, the present invention is described in further detail, and exemplary embodiment of the present invention and explanation thereof are only for explaining the present invention, not as a limitation of the invention.
Embodiment 1
The thin-layered chromatography detection method of cape jasmine in qingwen baidu powder, comprises the following steps:
(1) utilize qingwen baidu powder, cape jasmine, Gardenoside respectively and do not comprise the qingwen baidu powder formula preparation need testing solution of cape jasmine, control medicinal material solution, reference substance solution and negative sample solution; Concrete preparation process is as follows:
Get qingwen baidu powder 2g, add the methyl alcohol 25ml that concentration is 50%, ultrasonic 40min, filter, filtrate evaporate to dryness, adds methyl alcohol 2mL and dissolves, make need testing solution;
Get control medicinal material cape jasmine 0.5g, add the methyl alcohol 25ml that concentration is 50%, ultrasonic 40min, filter, filtrate evaporate to dryness, adds methyl alcohol 2mL and dissolves, namely make control medicinal material solution;
Get reference substance Gardenoside again, add methyl alcohol and make the solution of every 1ml containing 4mg Gardenoside, product solution in contrast;
First configure the qingwen baidu powder prescription not comprising cape jasmine, get 1/500 of recipe quantity, add the methyl alcohol 25ml that concentration is 50%, ultrasonic 40min, filter, filtrate evaporate to dryness, adds methyl alcohol 2mL and dissolves, namely make negative sample solution.
(2) draw need testing solution, control medicinal material solution, reference substance solution and negative sample solution point on silica gel g thin-layer plate, with ratio be 5: 5: 1: 1 ethyl acetate, acetone, formic acid and water for developping agent, launch, take out, dry;
(3) spray is with ethanol solution of sulfuric acid, is then heated to clear spot; Wherein, the concentration of ethanol solution of sulfuric acid is 10%, and heating-up temperature is 110 DEG C.
The chromatographic results manifested after drying
as Fig. 1shown in, be followed successively by reference substance solution, control medicinal material solution, need testing solution and negative sample solution from left to right.With the chromatogram opposite position place of control medicinal material solution and reference substance solution on need testing solution, the spot of this Chromatogram display same color, without the spot of respective color in the chromatogram of negative sample solution, represents that this negative sample solution is noiseless.
Embodiment 2
The present embodiment is the comparative examples of embodiment 1, and the preparation process of need testing solution described in the present embodiment is different, and in the present embodiment, this preparation process is as follows:
Get qingwen baidu powder 1g, add the methyl alcohol 10ml that concentration is 50%, ultrasonic 40min, filter, filtrate is as need testing solution.
When adopting the method for the present embodiment to detect, find that other materials treat the interference of detection material more greatly, prove: after filtrate adds methyl alcohol process again after super-dry, effectively reduce the interference of other materials, effect is more remarkable.
Above-described embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only the specific embodiment of the present invention; the protection domain be not intended to limit the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. the thin-layered chromatography detection method of cape jasmine in qingwen baidu powder, is characterized in that, comprise the following steps:
(1) preparation of need testing solution: get qingwen baidu powder 2g, adds the methyl alcohol that concentration is 50%, and after ultrasonic process, filter, filtrate evaporate to dryness, adds methyl alcohol 2mL and dissolve;
(2) draw need testing solution point on silica gel thin-layer plate, with ratio be 5: 5: 1: 1 ethyl acetate, acetone, formic acid and water for developping agent, launch, take out, dry;
(3) spray is with ethanol solution of sulfuric acid, is then heated to clear spot.
2. the thin-layered chromatography detection method of cape jasmine in qingwen baidu powder according to claim 1, is characterized in that, described silica gel thin-layer plate adopts silica gel g thin-layer plate.
3. the thin-layered chromatography detection method of cape jasmine in qingwen baidu powder according to claim 1 and 2, it is characterized in that, the concentration of described ethanol solution of sulfuric acid is 10%, and heating-up temperature is 110 DEG C.
4. the thin-layered chromatography detection method of cape jasmine in qingwen baidu powder according to claim 3, it is characterized in that, described silica gel thin-layer plate also has control medicinal material solution, reference substance solution, with negative sample solution, the preparation method of this control medicinal material solution, reference substance solution and negative sample solution is as follows:
Get control medicinal material cape jasmine 0.5g, add the methyl alcohol 25ml that concentration is 50%, ultrasonic 40min, filter, filtrate evaporate to dryness, adds methyl alcohol 2mL and dissolves, namely make control medicinal material solution;
Get reference substance Gardenoside again, add methyl alcohol and make the solution of every 1ml containing 4mg Gardenoside, make reference substance solution;
First configure the qingwen baidu powder prescription not comprising cape jasmine, get 1/500 of recipe quantity, add the methyl alcohol 25ml that concentration is 50%, ultrasonic 40min, filter, filtrate evaporate to dryness, adds methyl alcohol 2mL and dissolves, namely make negative sample solution.
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