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Method for separating lycoramine from plant extract

A technology of plant extracts and separation force, applied in the direction of organic chemistry, can solve the problems such as not seen, and achieve the effect of less consumption of raw materials, high yield and saving man-hours

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 the relevant record of the method for absorbing and eluting chloramine with ion exchange resin identical with the claims of the present invention

Method used

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  • Method for separating lycoramine from plant extract

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Experimental program
Comparison scheme
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 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), rinse the resin with water to neutrality, carry out gradient elution with 5% ammonia water / ethanol solution, follow up and detect with TLC method, Collection has the same R as Ricolamin f 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 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 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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Abstract

The invention relates to a kind of effective constituent separation method in vegetation extract, especially the method of separating lycoramine 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 lycoramine have concentration and enrichment; after get virgin product of lycoramine free alkali, make it have recrystallization with organic solvent; finally, the lycoramine 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 ricolamine from other alkaloids from plant extracts containing Amaryllidaceae alkaloids. (2) Background technology [0002] Lycoramine is a reversible acetylcholinesterase inhibitor, its action intensity is weaker than that of galantamine, and its acute toxicity is lower than that of galantamine, so its therapeutic index is close to or higher. [0003] The structural formula of Likolamin is shown in the figure below. [0004] [0005] Ricolamine is extracted from natural plants. These plants are distributed in the fields of Amaryllis genus, Snowflake Narcissus, Manjusri, Narcissus, Tennis Flower, and Water Ghost Banana. Among them, Lycoris is representative. In the prior art, the method for isolating Ricolamin from plant extracts is mainly organic solvent extraction. Utilizing the properties that lipophilic alka...

Claims

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Application Information

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IPC IPC(8): C07D491/06
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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