Method for separating lycorine from plant extract
A technology of plant extracts and lycorine, applied in the direction of organic chemistry, can solve unseen problems and achieve the effects of less consumption of raw materials, simple process operation and high yield
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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 lycorine f Value fractions were basified to pH 8.7 with saturated sodium carbonate solution, extracted 5 times (500ml×2, 250ml×3) with ethyl acetate methanol mixed solvent (9 / 1V / V), dried over anhydrous sodium sulfate, and reduced Distilled to dryness under pressure to obtain 53.0 g of crude product of lycorine free base, which was recrystallized with methanol to obtain 47.1 g of lycorine free base crystals 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 lycorine f Fractions of value, distillation recovery ethanol. Adjust the solution to pH 8.7, extract 5 times with chloroform methanol mixed solvent (9 / 2V / V) (500ml×2, 250ml×3), dry over anhydrous sodium sulfate, and distill to dryness under reduced pressure to obtain lycorine free base crude product 54.2 g, recrystallized with methanol to obtain 47.6 g of lycorine 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, collection and lycorine have the same R f Value fractions were basified to pH 8.7 with saturated sodium carbonate solution, extracted 5 times (500ml×2, 250ml×3) with ethyl acetate methanol mixed solvent (9 / 1V / V), dried over anhydrous sodium sulfate, and reduced After pressure distillation, 49.7 g of crude product of lycorine free base was obtained, which was recrystallized with methanol to obtain 45.9 g of lycorine free base crystal with a content of about 99%.
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