Crotepoxide preparation method
A technology for the preparation of echinoulenin, stems and leaves, which can solve the problems of complex purification process, serious pollution, and low energy efficiency of the extraction method, and achieve high extraction efficiency and simple process operation , The effect of high product yield
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Embodiment 1
[0016] Take 3 kg of sea wind rattan stems and leaves and grind them into 60 meshes, put them into a supercritical CO2 extraction kettle, feed liquid CO2, set the pressure at 25 MPa, temperature at 45 ° C, and flow rate at 4 ml / g / min, after dynamic equilibrium, feed ethyl acetate solution , the flow rate is 0.2ml / g / min, extract for 60min, and analyze under the conditions of pressure 5MPa and temperature 60℃, the obtained extract is dissolved in 70% ethanol solution, refluxed with 2% activated carbon for decolorization, the decolorized solution is concentrated and then extracted with ethyl acetate , place the extract to 1 / 4 volume to crystallize, then dissolve the crystals with 90% ethanol, pass through a short column of neutral alumina resin (120 mesh), collect the next column liquid, concentrate the crystals, and dry to obtain 1.1 g, content 97.2%.
Embodiment 2
[0018] Take 3 kg of sea wind rattan stems and leaves and grind them into 80 meshes, put them into a supercritical CO2 extraction kettle, feed liquid CO2, set the pressure at 20 MPa, temperature at 55 ° C, and flow rate at 2 ml / g / min, after dynamic equilibrium, feed ethyl acetate solution , the flow rate is 0.3ml / g / min, extract for 40min, and analyze under the conditions of pressure 6MPa and temperature 50℃, the obtained extract is dissolved in 80% ethanol solution, added with 3% activated carbon to reflux for decolorization, and the decolorized solution is concentrated and then extracted with ethyl acetate , put the extract to 1 / 3 volume to crystallize, and then dissolve the crystals with 95% ethanol, pass through a short column of neutral alumina resin (180 mesh), collect the next column liquid, concentrate the crystals, and dry to obtain 1.3 g, content 98.3%.
Embodiment 3
[0020] Take 3 kg of sea wind rattan stems and leaves and grind them into 20 meshes, put them into a supercritical CO2 extraction kettle, feed liquid CO2, set the pressure at 30 MPa, temperature at 40 ° C, and flow rate at 5 ml / g / min, after dynamic equilibrium, feed ethyl acetate solution , the flow rate is 0.2ml / g / min, extract for 50min, and analyze under the conditions of pressure 5MPa and temperature 50℃, the obtained extract is dissolved in 80% ethanol solution, refluxed with 1% activated carbon for decolorization, the decolorized solution is concentrated and then extracted with ethyl acetate , put the extract to 1 / 6 volume for crystallization, dissolve the crystallization with 95% ethanol, pass through a short column of neutral alumina resin (100 mesh), collect the next column liquid, concentrate the crystallization, and dry to obtain 1g of betelene , content 97.1%.
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