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Method for separating high-purity galanthamine from short-tube lycoris crude extract

A technology for galantamine and crude extract, applied in the field of separation of galantamine, can solve the problems of difficulty in extracting and separating pure galantamine, difficulty in removing alkaloid impurities, long cycle, etc., so as to achieve no loss of samples and separation. The effect of mild environment and high recovery rate

Inactive Publication Date: 2006-06-28
浙江一新制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The content of galantamine in Amaryllidaceae plants is very low, only about 1 / 10,000, accompanied by many types of other alkaloids, so it is very difficult to extract and separate pure galantamine
The traditional extraction, extraction and separation process has low yield, poor purity, long cycle time, difficulty in removing impurities similar to alkaloids, and does not meet the current high-quality requirements of galantamine in various countries in the world. There is an urgent need for a stable and high-purity galantamine. Min's production process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The solvent system of this example uses chloroform-methanol-water, and the solvent components are configured according to 4:3:2 and shaken up and then stratified. After a period of equilibrium, the upper phase and the lower phase are separated, and the upper phase is taken as The stationary phase, the lower phase is the mobile phase. Weigh the crude Lycoris extract and dissolve it in the mobile phase, first fill the entire chromatographic column with the stationary phase, adjust the host speed to 500-600rpm, pump the mobile phase into the column at a flow rate of 4.0ml / min, and adjust the balance of the equipment, Inject the sample, collect the eluate with the collector, and receive the target component according to the detector. A solid was obtained, and the purity was over 98% by HPLC.

Embodiment 2

[0018] The solvent system of this example adopts dichloromethane-ethanol-water, and the solvent components are configured according to 4:3:2 and shaken up and then stratified. After a period of equilibrium, the upper phase and the lower phase are separated, and the upper phase is taken as The stationary phase, the lower phase is the mobile phase. Weigh the crude Lycoris extract and dissolve it in the mobile phase, first fill the entire chromatographic column with the stationary phase, adjust the host speed to 500-600rpm, pump the mobile phase into the column at a flow rate of 4.0ml / min, and adjust the balance of the equipment, Inject the sample, collect the eluate with the collector, and receive the target component according to the detector. A solid was obtained, and the purity was over 98% by HPLC.

Embodiment 3

[0020] The solvent system in this example uses diethyl ether-n-hexane-methanol-water, and the solvent components are configured according to 4:1:3:4, shaken evenly and then stratified. After a period of equilibrium, the upper phase and the lower phase are separated, and the The upper phase is the stationary phase and the lower phase is the mobile phase. Weigh the crude Lycoris extract and dissolve it in the mobile phase, first fill the entire chromatographic column with the stationary phase, adjust the host speed to 500-600rpm, pump the mobile phase into the column at a flow rate of 4.0ml / min, and adjust the balance of the equipment, Inject the sample, collect the eluate with the collector, and receive the target component according to the detector. A solid was obtained, and the purity was over 98% by HPLC.

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PUM

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Abstract

A process for separating high-purity galantamin from the coarse extract of short-tube lycoris by counter-current chromatography includes such steps as preparing two-phase solvent system from 2,3,044 of paraffin, halohydrocarbon, emtrol, lipoketone, lipoester, ether, buffering liquid of inorganic salt and water, waving, laying aside for layering, dissolving the coarse extract of short-tube lycoris, and separating. Its advantages are high separating capacity and recovery rate, and less solvent consumption.

Description

technical field [0001] The invention relates to a method for separating galantamine by using countercurrent chromatography technology, in particular to a method for separating high-purity galantamine from crude extract of lycoris by using high-speed countercurrent chromatography technology. Background technique [0002] Galanthamine is a cholinesterase inhibitor developed in the 1950s. It is an alkaloid extracted from plants such as Amaryllidaceae Lycoris. It has been used for many years to treat myasthenia gravis, muscular dystrophy and sequelae of polio . Galantamine (4a, 5, 9, 10, 11, 12-hexahydro-3-methoxy-11-methyl-6H-benzofuro(3a, 3, 2-ef)-(2) Azepine-6-ol) is a tetracyclic alkaloid whose action is similar to that of physostigmine and neostigmine due to its pharmacological properties, but the therapeutic range of galantamine is wider than that of physostigmine and neostigmine Ming wide, less side effects. Galantamine is also used in the treatmen...

Claims

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Application Information

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IPC IPC(8): C07D491/048C07D307/00C07D223/00
Inventor 郑亚津陈红辉
Owner 浙江一新制药股份有限公司
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