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Method for extracting galanthamine from lycoris aurea

A technology of galantamine and galantamine hydrobromide, applied in organic chemistry and other directions, can solve the problems of insufficient drug market supply, weak market competitiveness, and cumbersome operation, so as to enhance market competitiveness and achieve good dissolution effect. , the effect of simplifying the operation

Inactive Publication Date: 2012-01-04
ENSHI QINGJIANG BIO ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

③Insufficient supply of drugs in the market
④ Taking therapeutic drugs for a long time
At the same time, the existing production technology has cumbersome operations, serious losses due to serious emulsification during the extraction process, low yield, high cost, and weak market competitiveness

Method used

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  • Method for extracting galanthamine from lycoris aurea
  • Method for extracting galanthamine from lycoris aurea
  • Method for extracting galanthamine from lycoris aurea

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 1. Extraction: Weigh 70g of Hudixiao dry powder, heat reflux extraction with 500ml methanol in a 2L extraction tank at 65°C for 2 hours, filter, and collect the filtrate; add 450ml methanol and heat reflux extraction in a 2L extraction tank at 65°C After 2 hours, filter and collect the filtrate; add 450ml of methanol and extract under reflux in a 2L extraction tank at 65°C for 2 hours, filter and collect the filtrate; combine 3 times to collect the extract. Concentrate under reduced pressure in a 1L round-bottomed flask at 40°C to 60°C with a rotary evaporator until there is no methanol to obtain the Hudixiao extract.

[0057] 2. Separation: Dissolve the Hudixiao extract with 150 times the volume of 2% acetic acid aqueous solution, stir fully, remove oily foam, centrifuge with a centrifuge, take the supernatant, and load the pretreated 732 cation exchange resin column (723 Wet packing of cation exchange resin to form a 40*300mm column bed, and then pretreatment), TCL de...

Embodiment 2

[0061] 1. Extraction: Weigh 10Kg of raw material powder into a 100-liter multi-functional extractor, add 65 liters of methanol, heat reflux at 65°C for 2 hours, filter, and collect the filtrate; add 65 liters of methanol at 65°C in a 100-liter multi-functional Heat reflux extraction in the extraction tank for 2 hours, filter, and collect the filtrate; add 65 liters of methanol at 65°C, heat reflux extraction in a 100 liter multifunctional extraction tank for 2 hours, filter, and collect the filtrate; combine the 3 extracts. Concentrate under reduced pressure at 40°C-60°C to no methanol in a 100-liter concentration tank to obtain Hudixiao extract.

[0062] 2. Separation: Weigh a certain amount of Hudixiao extract, dissolve it with 150 times the volume of 2% acetic acid aqueous solution, stir well, remove oily foam, centrifuge with a centrifuge, take the supernatant, and load the pretreated 732 cation Exchange resin column, TCL detects the end point of sample loading, after the ...

Embodiment 3

[0066] 1. Extraction: Weigh 200Kg of raw material powder into a 2000-liter extraction tank, add 1300 liters of methanol, heat reflux at 65°C for 2 hours, extract 3 times, and combine the 3 times of extracts. Concentrate under reduced pressure at 40°C-60°C to no methanol in a 500-liter concentration tank to obtain Hudixiao extract.

[0067] 2. Separation: Weigh a certain amount of Hudixiao extract, dissolve it with about 150 times the volume of 2% acetic acid aqueous solution, stir well, remove oily foam, centrifuge with a centrifuge, take the supernatant, and load the pretreated 732 Cation exchange resin column, TCL detects the end point of sample loading, after the resin absorbs alkaloids to saturation, rinse with 2BV of deionized water first, then alkalinize the resin bed with 1BV of 2% NaOH, and then elute the target with acetone (TCL detection Elution end point), concentrate the acetone eluent to about 2BV, and cool to room temperature. Dry with anhydrous sodium sulfate a...

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Abstract

The invention relates to a method for extracting galanthamine from lycoris aurea. The invention aims at carrying out improvement against the problems of low yield, high cost and weak market competitiveness of the existing method and establishing the method for extracting the galanthamine from the lycoris aurea, which has the industrial operatability. The method comprises the following steps: carrying out pretreatment on raw materials; carrying out the pretreatment by a cation exchange resin column; preparing the galanthamine by the thin-layer chromatography method (TCL method); extracting: smashing the lycoris aurea, then using methanol for heat reflux extraction, and concentrating extraction liquid till obtaining a liquid extract; separating: using 2% of acetic acid for dissolving the liquid extract and using resin for absorption; converting into galanthamine hydrobromide: introducing hydrogen bromide gas for obtaining a crude product II of galanthamine hydrobromide; and purifying the galanthamine hydrobromide. The method has the benefits that due to the adoption of the new extraction process, the method can simplify the operation, avoid the extraction process step, reduce the loss, improve the yield, reduce the cost and enhance the market competitiveness of the product.

Description

technical field [0001] The invention relates to a method for extracting galantamine from Hudixiao. Background technique [0002] Lycoris aurea (Lycoris aurea) is a plant of Amaryllidaceae, also known as Lycoris aurea, which is mainly distributed in Hunan, Hubei, Guangxi, Guangdong, Fujian, Taiwan, Sichuan, Yunnan and other places. The main active ingredients are galantamine, ricolamin, etc., which are clinically important medicines for the treatment of sequelae of polio. Hudixiao is the main plant source of natural galantamine. [0003] Galanthamine (Galanthamine), synonym galantamine base. Molecular formula C 17 h 21 NO 3 , molecular weight 287.35. Quite soluble in hot water, easily soluble in ethanol, acetone and chloroform, slightly soluble in benzene and ether. [0004] [0005] Galantamine in Lycoris was previously used as a specific medicine for the treatment of myasthenia gravis and post-poliomyelitis. In recent years, galantamine has a special effect on an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D491/06
Inventor 向极钎王发松杨永康李红英龙澜
Owner ENSHI QINGJIANG BIO ENG
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