Method for extracting Evodine from seeds of Rutaceae plants
A technology of evodiolide and rue, applied in the directions of steroids, organic chemistry, etc., can solve the problems of complicated operation of purification method, large amount of organic solvent, unfavorable scale-up production, etc., and achieves improved efficiency and economy, and less amount of solvent. , the effect of easy operation
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Embodiment example 1
[0027] Take 0.5 kg of orange seeds, add 0.5 L of ethanol with a volume fraction of 20%, heat and reflux to extract three times, extract for 1 hour each time, combine the two extracts, concentrate until the alcohol content of the extract is 3%, add an equivalent volume of petroleum ether Extracted 4 times, combined the extracted aqueous phase, suction filtered, and washed the filter cake with an equal volume of purified water to finally obtain the filter cake, vacuum-dried to obtain 7.032 g of crude product of evodia lactone. Add 10 times the amount of dichloromethane-acetone mixed solvent to the above crude product, heat to reflux to dissolve, filter the insoluble matter while it is hot, cool the filtrate to room temperature, let it stand for crystallization, filter and dry to obtain 1.26 g of evodia lactone with a content of 96.32%.
Embodiment example 2
[0029] Take 0.5kg of lemon seeds, add 3L of ethanol with a volume fraction of 50%, heat and reflux for extraction twice, each extraction for 2 hours, combine the extracts, concentrate until the ethanol content of the extract is 5%, add 3 times the volume of petroleum ether for extraction Once, the aqueous phase was extracted by suction filtration, and the filter cake was washed with 2 times the volume of purified water to finally obtain the filter cake, which was vacuum-dried to obtain 8.261 g of crude product of evodicarpalactone. Add 30 times the amount of dichloromethane-ethyl acetate mixed solvent to the above crude product, heat and reflux to dissolve, filter the insoluble matter while it is hot, and cool the filtrate to room temperature, let it stand for crystallization, and filter and dry to obtain 1.35 g of evodia lactone with a content of 97.13 %.
Embodiment example 3
[0031] Take 1 kg of citrus seeds, add 10 L of ethanol with a volume fraction of 70%, heat and reflux for extraction once, and extract for 3 hours each time, combine the two extracts, concentrate until the ethanol content of the extract is 8%, add an equal volume of petroleum ether to extract 2 For the second time, the extracted aqueous phases were combined, filtered with suction, and the filter cake was washed with an equal volume of purified water to finally obtain the filter cake, which was vacuum-dried to obtain 14.737 g of crude product of evodicarpalactone.
[0032] Add 40 times the amount of dichloromethane-isopropanol mixed solvent to the above crude product, heat and reflux to dissolve, filter the insoluble matter while it is hot, cool the filtrate to room temperature, let it stand for crystallization, and filter and dry to obtain 2.58 g of evodia lactone with a content of 95.86 %.
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