Method for preparing shionone by utilizing high-speed countercurrent chromatography
A high-speed countercurrent chromatography, asterone technology, applied in steroids, organic chemistry and other directions, can solve the problems of complex process operation, high production cost, poor specificity, etc., to achieve large separation, no sample loss, fast separation speed. Effect
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[0015] Example 1:
[0016] Take aster medicinal materials and pulverize, weigh 1kg, add 10L 80% methanol for reflux extraction for 2 hours, extract twice, add 200g medicinal activated carbon to the combined extract to decolorize, filter out the activated carbon while hot, concentrate to 50% alcohol concentration and leave to crystallize for 8 hours, 16 g of crude crystals were obtained by filtration. Take n-hexane, ethyl acetate, methanol, and water, and mix them in a ratio of 5:4:3:3. After standing for stratification, take out the lower phase and fill it with high-speed countercurrent chromatographic column. , after equilibration, adjust the flow rate to 3ml / min, at the same time take the upper phase to dissolve the crude crystals, inject the samples through the injection valve, detect by ELSD detector, collect the target components according to the atlas, concentrate the fractions under reduced pressure and place the crystals, filter out the crystals Vacuum drying to obtai...
Example Embodiment
[0017] Example 2:
[0018] Take aster medicinal materials and pulverize, weigh 1kg, add 8L of 90% methanol for reflux extraction for 2 hours, extract twice, add 300g medicinal activated carbon to the combined extract to decolorize, filter out the activated carbon while hot, concentrate to 70% alcohol concentration and leave to crystallize for 12 hours, 12 g of crude crystals were obtained by filtration. Take n-hexane, ethyl acetate, methanol, and water, and mix them in a ratio of 3:4:2:3. After standing for stratification, take out the lower phase and fill it with high-speed countercurrent chromatographic column. , after equilibration, adjust the flow rate to 1ml / min, at the same time take the upper phase to dissolve the crude crystals, inject the samples through the injection valve, detect by ELSD detector, collect the target components according to the atlas, concentrate the fractions under reduced pressure and place the crystals, filter out the crystals Vacuum drying to ob...
Example Embodiment
[0019] Example 3:
[0020] Take aster medicinal materials and pulverize, weigh 1kg, add 6L of 90% methanol for reflux extraction for 1 hour, extract 3 times, add 200g medicinal activated carbon to the combined extract to decolorize, filter out the activated carbon while hot, concentrate to 60% alcohol concentration and leave to crystallize for 16 hours. 13 g of crude crystals were obtained by filtration. Take n-hexane, ethyl acetate, methanol, and water, and mix them at a ratio of 5:5:2:4. After standing for stratification, take out the lower phase and fill it with a high-speed countercurrent chromatographic column, turn the main engine, and pump the upper phase at 900 rpm. , after equilibration, adjust the flow rate to 3ml / min, at the same time take the upper phase to dissolve the crude crystals, inject the samples through the injection valve, detect by ELSD detector, collect the target components according to the atlas, concentrate the fractions under reduced pressure and pl...
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