CN105403654A - Method raising radix astragali thin-layer chromatographic identification - Google Patents
Method raising radix astragali thin-layer chromatographic identification Download PDFInfo
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- CN105403654A CN105403654A CN201510923327.0A CN201510923327A CN105403654A CN 105403654 A CN105403654 A CN 105403654A CN 201510923327 A CN201510923327 A CN 201510923327A CN 105403654 A CN105403654 A CN 105403654A
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- radix astragali
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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
Abstract
The invention discloses a method raising radix astragali thin-layer chromatographic identification. The method comprises the following steps: firstly, radix astragali is ground into powder, 2-3g of the powder is weighed accurately by a weighing balance, 75ml of trichloromethane-n-butanol is added, heating backflow is carried out for 3h, then filtering is carried out, the filtrate is evaporated to dryness, 8ml-10ml of KOH-methanol saponification liquor is added in the residues, saponification processing is carried out, 8ml-10ml of KOH-methanol saponification liquor is added again, heating backflow is carried out for 0.5h-1h, evaporation to dryness is carried out, the residues are added with water and dissolved in water, ultrasonic extraction is carried out for 30min-40min, ethyl acetate is added, extraction is carried out twice, the final product is employed as a sample, the sample is dipped on the same silica gel G thin layer plate, the same developing solvent is employed, developing is carried out, then the thin layer plate is taken out and dried in air, then the thin layer plate is inspected under light with 365nm of a JL-P10A film viewer or a daylight ultraviolet light lamp, and shooting is carried out finally. The problem is solved that the sharpness of astragaloside in chromatogram is not high and the provided method is an accurate, distinct and rapid method for identifying radix astragali.
Description
Technical field
The invention belongs to biological technical field, be specifically related to a kind of method improving the qualification of Radix Astragali thin-layer chromatography.
Background technology
This product is the dry root of legume astragalus mongolicus or Astragalus membranacus, and spring, Qiu Erji excavate, and removing fibrous root and root head, rinse well, run through, take advantage of fresh-cut sheet, dry, be called " astragalus mongholicus tablet ", this product surface light brown yellow or light brown brown, have irregular longitudinal furrow line or longitudinal furrow.Matter is hard and tough, and section fibrous is strong, and aobvious mealiness, skin zone's yellow-white, woody part is faint yellow, has radial texture and crack.Gas is micro-, and taste is micro-sweet, and that chews micro-ly has beany flavor.
The work of quality standards in Chinese drugs is now in full swing, and traditional Chinese medicine scholar, in conjunction with relevant issues in current Quality research on standard, proposes some views.First be drafting of title, preferably can embody the foundation of the method for inspection and formulation two contents of standard specification, next is identification experiment importantly, mainly solves the authenticity of tested medicine, has proterties discriminating, microscopical characters and physics and chemistry discriminating etc.Except general chemical experiment is as except color reaction in physics and chemistry discriminating, current extensive application be chromatography, and it is most widely used general with thin-layer chromatography, because it is easy, easy, highly sensitive, specificity is strong, there is Isolation and ldentification dual-use function, be specially adapted to the Chinese medicine of complicated component and the discriminating of preparation thereof, as long as some characteristic spots tool repeatabilities, just can be used as confirmation foundation, chemical monomer, extract, Authentic plant drugs etc. can be selected in thin layer experiment to do contrast and differentiate.
Chinese Pharmacopoeia 2010, (annex VI B), provides according to thin-layered chromatography test, by adding hot reflux to sample, filter, filtrate is added on neutral alumina column, collect eluent, evaporate to dryness, residue dissolves, the steps such as extraction, washing complete, as need testing solution, carry out point sample, but it needed neutral alumina column, cost is high, and its chromatogram sharpness is not high.
Summary of the invention
The present invention is in order to overcome above-mentioned not enough problem in prior art, a kind of method improving the qualification of Radix Astragali thin-layer chromatography is provided, add saponification liquor saponification in residue after reflux and filter, method is simple, removal of impurity successful and improve the sharpness of Astragaloside IV in chromatogram.
To achieve these goals, a kind of method improving the qualification of Radix Astragali thin-layer chromatography of the present invention comprises the following steps:
(1) first the Radix Astragali is ground to powder, this powder 2-3g is accurately taken with weighing balance, add methenyl choloride-normal butyl alcohol 75ml, add hot reflux, after 3h, filter, then by filtrate evaporate to dryness, residue adds the KOH-methyl alcohol saponification liquor of 8mL-10mL again, is placed in 60 DEG C-65 DEG C water bath with thermostatic control 30min-40min; Filter, again add the KOH-methyl alcohol saponification liquor of 8mL-10mL, put 100 DEG C of heating water baths backflow 0.5-1h, evaporate to dryness, the residue 30ml that adds water makes dissolving, moves in separating funnel; Add after 2mL methyl alcohol makes Radix Astragali residue fully dissolve again, after ultrasonic extraction 30min-40min, then add extraction into ethyl acetate twice, each 30mL, evaporate to dryness extract, add methyl alcohol and make it to dissolve, this is as sample;
(2) draw the above-mentioned solution of 5 μ l to put respectively on same silica gel g thin-layer plate, same developping agent, first launch, then take out, then dry, inspect under putting JL-P10A viewbox or under daylight UV light modulation 365nm, finally take pictures, can be very stable on thin plate demonstrate clear band, and in sample, band presents the consistance of rule, in 3 hours, orange-yellow colour developing is comparatively stable, can be judged as the Radix Astragali.
In described step (1), methenyl choloride and normal butyl alcohol volume ratio are 2:1.
In described step (1), ultrasonic extraction power is 40-90W, and ultrasonic temperature is 4 DEG C-10 DEG C, extracts 1-4 time.
Middle KOH-methyl alcohol saponification liquor mass concentration described in described step (1): 20%.
The described developping agent described in step (2) is: methenyl choloride and normal hexane, wherein methenyl choloride: normal hexane=3:1.
The described developping agent described in step (2) is: sherwood oil and ethyl acetate, wherein sherwood oil: ethyl acetate=7:1.
Beneficial effect of the present invention: compared with prior art, the saponification of good fortune liquid is added in the residue of the present invention after first reflux and filter, method is simple, removal of impurity successful, solving the problem that the sharpness of Astragaloside IV in chromatogram is not high, is a kind of accurate, clear and differentiate the method for the Radix Astragali fast.
Accompanying drawing explanation
Fig. 1 is daylight lamp astragalus mongholicus tablet indentification by TLC figure, S-Astragaloside IV reference substance, and No. 1-10 is Radix Astragali sample.
Fig. 2 is ultraviolet lamp astragalus mongholicus tablet indentification by TLC figure, S-Astragaloside IV reference substance, and No. 1-10 is Radix Astragali sample.
Embodiment
Below by way of specific embodiment, the invention will be further described, but the interest field that the present invention protects is not limited only to following examples.
Experimental technique of the present invention and parameter:
1. main material:
2. main agents:
Methenyl choloride, normal butyl alcohol, KOH, methyl alcohol, ethyl acetate, normal hexane, sherwood oil, ethyl acetate.Silica gel g thin-layer plate, polyamide thin plate, distilled water, 90% ethanolic solution etc.
Embodiment 1
(1) be first powder by Radix Astragali ground material different for 10 kinds of places of production, cross 200 object sieves, accurately take this powder 2g with weighing balance, add methenyl choloride-normal butyl alcohol 75ml that volume ratio is 2:1, add hot reflux, after 3h, filter, then by filtrate evaporate to dryness, it is 20% that residue adds massfraction again, the KOH-methyl alcohol saponification liquor of 8mL, is placed in 60 DEG C of water bath with thermostatic control 30min; Filter, again add the KOH-methyl alcohol saponification liquor of 8mL, put 100 DEG C of heating water baths backflow 1h, evaporate to dryness, the residue 30ml that adds water makes dissolving, moves in separating funnel; Add after 2mL methyl alcohol makes Radix Astragali residue fully dissolve again, ultrasonic extraction 30min, ultrasonic power is 50W, ultrasonic temperature is 4 DEG C and extracts after 2 times, then adds extraction into ethyl acetate twice, each 30mL, evaporate to dryness extract, add methyl alcohol and make it to dissolve, this is as supplying sample;
(2) draw the above-mentioned solution of 5 μ L to put respectively on same silica gel g thin-layer plate, same developping agent is methenyl choloride: normal hexane=3:1, first launch, then take out, then dry, under putting JL-P10A viewbox, finally take pictures, can be very stable on thin plate demonstrate clear band, and in sample, band presents the consistance of rule, in 3 hours, orange-yellow colour developing is comparatively stable, can be judged as the Radix Astragali.See Fig. 1.
Embodiment 2
(1) be first powder by Radix Astragali ground material different for 10 kinds of places of production, cross 200 object sieves, accurately take this powder 2g with weighing balance, add methenyl choloride-normal butyl alcohol 75ml that volume ratio is 2:1, add hot reflux, after 3h, filter, then by filtrate evaporate to dryness, it is 20% that residue adds massfraction again, the KOH-methyl alcohol saponification liquor of 8mL, is placed in 60 DEG C of water bath with thermostatic control 30min; Filter, again add the KOH-methyl alcohol saponification liquor of 8mL, put 100 DEG C of heating water baths backflow 1h, evaporate to dryness, the residue 30ml that adds water makes dissolving, moves in separating funnel; Add after 2mL methyl alcohol makes Radix Astragali residue fully dissolve again, ultrasonic extraction 30min, ultrasonic power is 50W, ultrasonic temperature is 4 DEG C and extracts after 2 times, then adds extraction into ethyl acetate twice, each 30mL, evaporate to dryness extract, add methyl alcohol and make it to dissolve, this is as supplying sample;
(2) draw the above-mentioned solution of 5 μ L to put respectively on same silica gel g thin-layer plate, same developping agent is methenyl choloride: normal hexane=3:1, first launch, then take out, then dry, inspect under daylight UV light modulation 365nm, finally take pictures, can be very stable on thin plate demonstrate clear band, and in sample, band presents the consistance of rule, in 3 hours, orange-yellow colour developing is comparatively stable, can be judged as the Radix Astragali.See Fig. 2.
Embodiment 3
(1) be first powder by Radix Astragali ground material different for 10 kinds of places of production, cross 200 object sieves, accurately take this powder 3g with weighing balance, add methenyl choloride-normal butyl alcohol 75ml that volume ratio is 2:1, add hot reflux, after 3h, filter, then by filtrate evaporate to dryness, it is 20% that residue adds massfraction again, the KOH-methyl alcohol saponification liquor of 10mL, is placed in 60 DEG C of water bath with thermostatic control 30min; Filter, again add the KOH-methyl alcohol saponification liquor of 10mL, put 100 DEG C of heating water baths backflow 1h, evaporate to dryness, the residue 30ml that adds water makes dissolving, moves in separating funnel; Add after 2mL methyl alcohol makes Radix Astragali residue fully dissolve again, ultrasonic extraction 30min, ultrasonic power is 50W, ultrasonic temperature is 4 DEG C and extracts after 2 times, then adds extraction into ethyl acetate twice, each 30mL, evaporate to dryness extract, add methyl alcohol and make it to dissolve, this is as supplying sample;
(2) draw the above-mentioned solution of 5 μ L to put respectively on same silica gel g thin-layer plate, same developping agent is sherwood oil: ethyl acetate=7:1, first launches, then takes out, dry again, under putting JL-P10A viewbox, finally take pictures, can be very stable on thin plate demonstrate clear band, and band presents the consistance of rule in sample, in 3 hours, orange-yellow colour developing is comparatively stable, can be judged as the Radix Astragali, can obtain the figure of chromatogram qualification clearly equally.
Claims (6)
1. improve a method for Radix Astragali thin-layer chromatography qualification, it is characterized in that, comprise the following steps:
(1) first the Radix Astragali is ground to powder, this powder 2-3g is accurately taken with weighing balance, add methenyl choloride-normal butyl alcohol 75ml, add hot reflux, after 3h, filter, then by filtrate evaporate to dryness, residue adds the KOH-methyl alcohol saponification liquor of 8mL-10mL again, is placed in 60 DEG C-65 DEG C water bath with thermostatic control 30min-40min; Filter, again add the KOH-methyl alcohol saponification liquor of 8mL-10mL, put 100 DEG C of heating water baths backflow 0.5-1h, evaporate to dryness, the residue 30ml that adds water makes dissolving, moves in separating funnel; Add after 2mL methyl alcohol makes Radix Astragali residue fully dissolve again, after ultrasonic extraction 30min-40min, then add extraction into ethyl acetate twice, each 30mL, evaporate to dryness extract, add methyl alcohol and make it to dissolve, this is as sample;
(2) draw the above-mentioned solution of 5 μ L to put respectively on same silica gel g thin-layer plate, same developping agent, first launch, then take out, then dry, inspect under putting JL-P10A viewbox or under daylight UV light modulation 365nm, finally take pictures, can be very stable on thin plate demonstrate clear band, and in sample, band presents the consistance of rule, in 3 hours, orange-yellow colour developing is comparatively stable, can be judged as the Radix Astragali.
2. a kind of method improving the qualification of Radix Astragali thin-layer chromatography according to claim 1, is characterized in that, described step 1) in methenyl choloride and normal butyl alcohol volume ratio be 2:1.
3. according to claim 1 a kind of improve the Radix Astragali thin-layer chromatography qualification method, it is characterized in that, described step 1) in ultrasonic extraction power be 40-90W, ultrasonic temperature be 4 DEG C-10 DEG C extract 1-4 time.
4. according to claim 1 a kind of improve the Radix Astragali thin-layer chromatography qualification method, it is characterized in that, described step 1) described in middle KOH-methyl alcohol saponification liquor mass concentration: 20%.
5. according to claim 1 a kind of improve the Radix Astragali thin-layer chromatography qualification method, it is characterized in that, described step 1) in developping agent be: methenyl choloride and normal hexane, wherein methenyl choloride: normal hexane=3:1.
6. according to claim 1 a kind of improve the Radix Astragali thin-layer chromatography qualification method, it is characterized in that, described step 1) described in developping agent be: sherwood oil and ethyl acetate, wherein sherwood oil: ethyl acetate=7:1.
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