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Preparation method of galanthamine

A technology of galantamine and chloroform, applied in the field of preparation of galantamine, can solve the problems of low galantamine content, unfavorable large-scale production operations, large sewage discharge and the like

Active Publication Date: 2012-01-11
江苏永茂普隆汽车配件制造有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, the extraction and separation methods of galantamine are mainly organic solvent methods, etc., with many steps and large amount of sewage discharge, and the content of galantamine obtained by these extraction processes is very low, which is unfavorable for large-scale production operations

Method used

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  • Preparation method of galanthamine

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Effect test

Embodiment 1

[0017] Take 10Kg of Lycoris bulb fine powder, add it into the triethylamine aqueous solution of pH=12, soak overnight, dry, place in CO 2 Supercritical extraction in supercritical extraction device, CO 2 The flow rate is 2ml / min / g crude drug, 90% ethanol aqueous solution is selected as the entrainer, the flow rate is 0.4ml / min / g crude drug, the extraction temperature is 60°C, the pressure is 30MPa, and the extraction time is 2h; the extract is dissolved by adding 2% hydrochloric acid aqueous solution, Filtrate, add CHCl to the filtrate 3 Extract, remove the lower layer, adjust the pH to 13, add CHCl 3 Extraction, take CHCl 3 Layer, separated by alumina chromatographic column, take chloroform-methanol-water (5:3:1) lower layer solution as eluent to elute, collect eluate, concentrate, add acetone-ethanol (1:1) Crystallized, washed and dried to obtain 213 mg of galantamine, which was detected by HPLC with a purity of 94.5%.

Embodiment 2

[0019] Take 10Kg of Lycoris bulb fine powder, add it to the ammonia solution of pH=10 and soak it overnight, dry it, and put it in CO 2 Supercritical extraction in supercritical extraction device, CO 2 The flow rate is 1ml / min / g crude drug, 90% ethanol aqueous solution is selected as the entrainer, the flow rate is 0.1ml / min / g crude drug, the extraction temperature is 20°C, the pressure is 10MPa, and the extraction time is 0.5h; the extract is dissolved by adding 2% hydrochloric acid aqueous solution , filtered, and the filtrate was added with CHCl 3 Extract, remove the lower layer, adjust the pH to 13, add CHCl 3 Extraction, take CHCl 3 layer, separated by alumina chromatographic column, take chloroform-methanol-water (4:5:1) lower layer solution as the eluent to elute, collect the eluate, concentrate, add acetone-ethanol (3:1) Crystallized, washed and dried to obtain 175 mg of galantamine, which was detected by HPLC with a purity of 92.3%.

Embodiment 3

[0021] Take 10Kg of Lycoris bulb fine powder, add it to the triethylamine aqueous solution of pH=13, soak overnight, dry, place in CO 2 Supercritical extraction in supercritical extraction device, CO 2 The flow rate is 5ml / min / g crude drug, 90% ethanol aqueous solution is selected as the entrainer, the flow rate is 0.8ml / min / g crude drug, the extraction temperature is 80°C, the pressure is 50MPa, and the extraction time is 4h; the extract is dissolved by adding 2% hydrochloric acid aqueous solution, Filtrate, add CHCl to the filtrate 3 Extract, remove the lower layer, adjust the pH to 13, add CHCl 3 Extraction, take CHCl 3 layer, separated by alumina chromatographic column, take chloroform-methanol-water (2:1:1) lower layer solution as the eluent to elute, collect the eluate, concentrate, add acetone-ethanol (1:6) Crystallized, washed and dried to obtain 235 mg of galantamine, which was detected by HPLC with a purity of 93.4%.

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Abstract

The invention relates to a preparation method of galanthamine, which is characterized by simple operation and little pollution and comprises the following processing steps: taking raw fine powder, soaking the fine powder in aqueous alkali solution overnight, drying the powder and placing the dried powder in a CO2 supercritical liquid extraction device for supercritical liquid extraction; adding 2% aqueous hydrochloric acid solution to extracts to dissolve the extracts, filtering the extracts, adding chloroform to filtrate for extraction, taking subnatant, adjusting pH value to 13, adding the chloroform for extraction, taking the chloroform layer, carrying out separation by alumina column chromatography, taking chloroform-methanol-water subnatant as an eluting agent for elution, collectingeluent, concentrating the eluent, adding acetone-ethanol for recrystallization, washing and drying the crystal, thus obtaining the galanthamine. By adopting the invention to prepare the galanthamine,the product is high in purity and industrialization enlargement is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of galantamine, in particular to a method for extracting galantamine from plants. Background technique [0002] Galanthamine is a tertiary amine alkaloid, which was first isolated from the Amaryllidaceae plant Galanthus woronowii Losink by Proskurnina and Yakovleva in 1952, and is widely distributed in Amaryllidaceae plants. Its structural formula is as follows: [0003] [0004] Studies have shown that galantamine is effective in treating conditions such as polio sequelae, myasthenia gravis, and traumatic paraplegia with less toxicity. Since the 1990s, the hydrobromide salt of galantamine has been used to treat Alzheimer's disease, and it is expected to become the drug of choice for the treatment of this disease because of its unintentional and hepatotoxic side effects. Among the source plants of galantamine in my country, the bulbs of Lycoris radiata Herb., L.aruea Herb., and L. squamigeric Herb. are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D491/06A61P21/04A61P43/00
CPCY02P20/54
Inventor 王琳范淦彬
Owner 江苏永茂普隆汽车配件制造有限公司