Method for purifying sennoside A
A purification method, the technology of sennoside, which is applied in the field of purification of sennoside A, can solve the problems such as the rare separation and research of sennoside A, achieve the simultaneous completion of separation, purification and preparation, facilitate separation and preparation, and save organic The effect of the solvent
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Embodiment 1
[0018] Take 1kg of senna leaves, add 5L of petroleum ether to reflux and degrease for 30min, filter out the degreased matter and dry it, add 10L of ethanol for percolation extraction for 2h, keep the extraction temperature at 50°C, concentrate the extract to extract, and use an appropriate amount of 1 % sodium bicarbonate solution was dissolved, the insoluble matter was filtered out, and an equal amount of dichloromethane was added to extract twice, the raffinate was adjusted to neutrality by adding dilute hydrochloric acid, allowed to stand for precipitation, and the precipitate was filtered out and dried to obtain crude sennoside;
[0019] Measure ethyl acetate-methanol-water according to the ratio of 20:3:20, mix well and take the upper phase as the stationary phase, and the lower phase as the mobile phase, dissolve the crude sennoside in the upper phase to make a sample solution, and use 10ml Pump the stationary phase into the chromatographic column at a flow rate of / min. ...
Embodiment 2
[0021] Take 1kg of senna leaf medicinal material, add 7L petroleum ether to reflux and degrease 3 times, 20min each time, filter out the degreased matter and dry, add 20L ethanol for percolation extraction for 2h, keep the extraction temperature at 80°C, and concentrate the extract to extract Dissolve with an appropriate amount of 5% sodium bicarbonate solution, filter out the insoluble matter, add an equal amount of dichloromethane to extract 5 times, add dilute hydrochloric acid to the raffinate to neutral, let it stand for precipitation, filter out the precipitate and dry to obtain sennoside Crude;
[0022] Measure ethyl acetate-methanol-water according to the ratio of 20:1:20, mix well and take the upper phase as the stationary phase, and the lower phase as the mobile phase, dissolve the crude sennoside in the upper phase to make a sample solution, and use 10ml Pump the stationary phase into the chromatographic column at a flow rate of / min. After the stationary phase is f...
Embodiment 3
[0024] Take 5kg of senna leaves, add 30L of petroleum ether to reflux and degrease for 40min, filter out the degreased matter and dry, add 60L of ethanol for percolation extraction for 2h, keep the extraction temperature at 70°C, concentrate the extract to extract, and use an appropriate amount of 3 % sodium bicarbonate solution was dissolved, the insoluble matter was filtered out, and an equal amount of dichloromethane was added to extract 3 times, the raffinate was adjusted to neutrality by adding dilute hydrochloric acid, allowed to stand for precipitation, and the precipitate was filtered out and dried to obtain crude sennoside;
[0025] Measure ethyl acetate-methanol-water according to the ratio of 20:2:20, mix well and take the upper phase as the stationary phase, and the lower phase as the mobile phase, dissolve the crude sennoside in the upper phase to make a sample solution, and use 10ml Pump the stationary phase into the chromatographic column at a flow rate of / min. ...
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