Method for extracting and isolating ruscogenin from pseudoleaf tree
A technology for separating ruscogenin and pseudophyllum, which is applied in the fields of steroids and organic chemistry, can solve the problems of long production cycle and low yield, achieve less usage, good selectivity, and less solvent consumption Effect
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Embodiment 1
[0048] Take 100kg of false leaf tree raw material, add 50kg of water to pulverize, add 40kg of diatomaceous earth and 250kg of water after pulverization and stir evenly, add 60kg of glacial acetic acid to the above mixture system (make the mass fraction 20%), stir and hydrolyze at 90°C for 1 hour , filtered, and the precipitate was washed with water until pH=7. Add 10 times the amount of acetone to the precipitate, extract at 70°C for two hours, and filter. The filtrate is concentrated using membrane concentration equipment, the selected membrane has a molecular weight cut-off of 200-400, and is concentrated to 1 / 10 of the original volume to stop concentration. Put the concentrated solution in the refrigerator overnight to obtain white crystals. Add 8 times the amount of ethyl acetate to dissolve the white crystals, add 8% activated carbon, heat at 60°C for 1 hour, filter, concentrate to 1 / 3, place crystals in an ice bath, filter with suction, and dry in vacuo, white powder o...
Embodiment 2
[0050] Take 100kg of false leaf tree raw material, add 50kg of water to pulverize, add 12kg of alumina, 8kg of diatomaceous earth and 250kg of water after pulverization and stir evenly, add 45kg of sulfuric acid to the above mixture system (to make the mass fraction 15%), and stir at 90°C Hydrolyze for 2 hours, filter, and wash the precipitate with water to pH=5. Add 7 times the amount of chloroform to the precipitate, extract at 60°C for two hours, and filter. The filtrate is concentrated using membrane concentration equipment, the selected membrane has a molecular weight cut-off of 200-400, and is concentrated to 1 / 3 of the original volume to stop concentration. Put the concentrated solution in the refrigerator overnight to obtain white crystals. Add 4 times the amount of white crystals to 90% methanol to dissolve, add 5% activated carbon, heat at 50°C for 1 hour, filter, concentrate to 1 / 4, place crystals in an ice bath, filter with suction, and dry in vacuo, white powder ...
Embodiment 3
[0052] Take 100kg of false leaf tree raw material, add 50kg of water to pulverize, add 5kg of silica gel, 5kg of alumina and 250kg of water after pulverization and stir evenly, add 15kg of formic acid to the above mixture system (make the mass fraction 5%), stir and hydrolyze at 50°C for 5 hours, filtered, and washed the precipitate with water to pH=4. Add 5 times the amount of ethanol to the precipitate, extract at 80°C for two hours, and filter. The filtrate is concentrated by membrane concentration equipment, the selected membrane has a molecular weight cut-off of 400-600, and is concentrated to 1 / 6 of the original volume to stop concentration. Put the concentrated solution in the refrigerator overnight to obtain white crystals. Dissolve the white crystals in 5 times the amount of chloroform, add 5% activated carbon, heat at 40°C for 1 hour, filter, concentrate to 1 / 3, place crystals in an ice bath, filter with suction, and dry in vacuo to obtain a white powder of deluscog...
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