Method for separating macranthoidin from lonicerae flos
A technology of honeysuckle saponin B and mountain silver flower, which is applied in the field of natural medicinal chemistry, can solve the problems of serious loss of samples separated by silica gel column, unsuitability for industrial production, and large amount of reagents, and achieve continuous preparation, small amount of solvent, large amount of preparation
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Embodiment 1
[0017] Take 500g of mountain silver flower raw material, soak and extract with 7 times the amount of saturated lime water for 3 times, soak for 3 hours each time, combine the extract solution with hydrochloric acid solution to adjust neutrality, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 2000 after filtration, and the permeate Concentrate by nanofiltration with a hollow cellulose membrane with a cut-off of 1000, add 95% ethanol to the concentrated solution for precipitation, centrifuge, and concentrate the liquid under reduced pressure to obtain an extract. Take ethyl acetate, n-butanol and water and mix them in a ratio of 3:1:3. After fully layering, take the upper phase as the stationary phase and fill the high-speed countercurrent chromatography tube, turn the host at 800 rpm, and pump the lower phase as the mobile phase. After dynamic balance, the flow rate is adjusted to 2ml / min, and the extract is dissolved with the mobile phase at the...
Embodiment 2
[0019] Take 500g of mountain silver flower raw material, soak and extract 3 times with 5 times the amount of saturated lime water, soak for 2 hours each time, combine the extract solution with hydrochloric acid solution to adjust neutrality, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 3000 after filtration, and the permeate Concentrate by nanofiltration with a hollow cellulose membrane with a cut-off of 800, add 95% ethanol to the concentrated solution for precipitation, centrifuge, and concentrate the liquid under reduced pressure to obtain an extract. Take ethyl acetate, n-butanol and water, and mix them in a ratio of 5:2:7. After fully layering, take the upper phase as the stationary phase and fill the high-speed countercurrent chromatography tube, turn the host at 900 rpm, and pump the lower phase as the mobile phase. After dynamic equilibrium, the flow rate was adjusted to 3ml / min, and the extract was dissolved with the mobile phase at t...
Embodiment 3
[0021] Take 1000g of mountain silver flower raw material, soak and extract 2 times with 8 times the amount of saturated lime water, soak for 3 hours each time, combine the extract solution with hydrochloric acid solution to adjust neutrality, add ultrafiltration membrane ultrafiltration with molecular weight cut off 2000 after filtration, and permeate Concentrate by nanofiltration with a hollow cellulose membrane with a cut-off of 600, add 95% ethanol to the concentrated solution for precipitation, centrifuge, and concentrate the liquid under reduced pressure to obtain an extract. Take ethyl acetate, n-butanol and water, and mix them in a ratio of 9:2:7. After fully layering, take the upper phase as the stationary phase and fill the high-speed countercurrent chromatography tube, turn the host at 850 rpm, and pump the lower phase as the mobile phase. After dynamic equilibrium, the flow rate was adjusted to 3ml / min, and the extract was dissolved with the mobile phase at the same ...
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