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

Active Publication Date: 2005-05-04
GUANGDONG TECHPOOL BIO-PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But above-mentioned patent literature and non-patent literature all do not see relevant and the record of the method for ion-exchange resin adsorption, eluting lycorine identical with the claims of the present invention

Method used

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  • Method for separating lycorine from plant extract

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Experimental program
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Effect test

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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Abstract

The invention relates to a kind of effective constituent separation method in vegetation extract, especially the method of separating lycorine from vegetation extract containing amaryllidaceae alkaloid. The industrial art is as follows: make vegetation extract containing amaryllidaceae alkaloid have pretreatment; adsorb and elute with cation exchange resin; track and detect the elution flowing composition; make the flowing composition in lycorine have concentration and enrichment; after get virgin product of lycorine free alkali, make it have recrystallization with organic solvent; finally, the lycorine free alkali crystallization with about 99% purity can be acquired.

Description

(1) Technical field [0001] The invention relates to a method for extracting effective medicinal components of plants, in particular to a method for separating lycorine from other alkaloids from plant extracts containing amaryllidaceae alkaloids. (2) Background technology [0002] Lycorine (lycorine) can inhibit the anaerobic glycolysis of mouse ascites cancer cells, and has a significant inhibitory effect on mouse lymphosarcoma, sarcoma 37 and rat lymphosarcoma, liver cancer cells; Hela cells, sarcoma 180, Ehrlich ascites Carcinoma, ascites liver cancer and Yoshida's sarcoma also have inhibitory effect. It is also the raw material for the preparation of anticancer drug lycorine oxide (AT-1840). [0003] The structural formula of lycorine is shown in the figure below. [0004] [0005] Lycorine is extracted from natural plants. These plants are distributed in the genus Amaryllis, Manjusri, Narcissus, Tennis Flower and other fields. Among them, Lycoris is representative...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/16
Inventor 傅和亮王宁何宣扬王晓岩匡卫文
Owner GUANGDONG TECHPOOL BIO-PHARMA CO LTD
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