Method for separating lycoramine from plant extract
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Embodiment 1
[0025] Amaryllidaceae plant extract 10kg, add 1% hydrochloric acid solution to dissolve, adjust and maintain the acidity of the solution. Remove the insoluble particles in the solution by filtration, exchange through a well-balanced STREAMLINE SP cation exchange resin (2L), wash the resin with water to neutrality, carry out gradient elution with 1mol / L sodium chloride solution, track and detect with TLC method, collect Has the same R as Ricolamin f Value fractions were basified to pH 11.2 with saturated sodium carbonate solution, extracted 5 times with ethyl acetate (500ml×2, 250ml×3), dried over anhydrous sodium sulfate, and distilled to dryness under reduced pressure to obtain Ricolamin 35.1 g of the crude free base product was recrystallized with acetone to obtain 24.0 g of free base crystals of Licolamine with a content of about 99%.
Embodiment 2
[0027] Amaryllidaceae plant extract 10kg, add 1% hydrochloric acid solution to dissolve, adjust and maintain the acidity of the solution. Remove the insoluble particles in the solution by filtration, exchange through the transformed Amberlite CG-120 cation exchange resin (10L), wash the resin with water to neutrality, carry out gradient elution with 5% ammonia water / ethanol solution, track and detect with TLC method, collect Has the same R as Ricolamin r Fractions of value, distillation recovery ethanol. The solution was adjusted to pH 11.2, extracted 5 times with chloroform (500ml×2, 250ml×3), dried over anhydrous sodium sulfate, and distilled to dryness under reduced pressure to obtain 40.5g of crude product of Licolamine free base, which was recrystallized with acetone to obtain 25.3 g of Licolamine free alkali crystals with a content of about 99%.
Embodiment 3
[0029] Amaryllidaceae plant extract 10kg, add 1% hydrochloric acid solution to dissolve, adjust and maintain the acidity of the solution. Remove the insoluble particles in the solution by filtration, exchange through the transformed STREAMLINE SP cation exchange resin (2L), wash the resin with water to neutrality, and use 0.1mol / L, 0.2mol / L, 0.3mol / L, 0.4mol / L respectively , 0.6mol / L, 0.8mol / L sodium chloride / 20% ethanol solution for elution, follow-up detection with TLC method, and collect the same R r Value fractions were basified to pH 11.2 with saturated sodium carbonate solution, extracted 5 times with ethyl acetate (500ml×2, 250ml×3), dried over anhydrous sodium sulfate, and distilled to dryness under reduced pressure to obtain Ricolamin 32.5 g of the free base crude product was recrystallized with acetone to obtain 24.1 g of free base crystals of Licolamine with a content of about 99%.
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