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Method for extracting, separating and purifying strychnine

A technology for separation and purification of strychnine, applied in organic chemistry, pharmaceutical formulations, organic active ingredients, etc., can solve the problem of low safety of strychnine

Active Publication Date: 2018-06-05
BEIJING INCREASEPHARM CORP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been reported in the literature that strychnine and strychnine were administered to mice, and the LD of the two 50 They are 3.27mg / kg and 233mg / kg respectively. From this we can know that the safety of strychnine is very low. If part of strychnine in total strychnine can be removed, its toxicity can be reduced and the Its original anti-inflammatory and analgesic pharmacological activity improves the safety of clinical medication

Method used

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  • Method for extracting, separating and purifying strychnine
  • Method for extracting, separating and purifying strychnine
  • Method for extracting, separating and purifying strychnine

Examples

Experimental program
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Effect test

Embodiment 1

[0147] Take 1000g of Nuxychium chinensis, crush it into coarse powder, add 12 times the amount of 30% ethanol, heat and reflux twice, each time for 0.5h, combine the extracts, filter, concentrate under reduced pressure to recover ethanol until there is no alcohol smell, and concentrate the filtrate to a concentration of 0.4g medicinal material / ml, add hydrochloric acid to adjust the acid content to 2%, add 3 times the amount of ethyl acetate to extract twice, take the raffinate, add sodium hydroxide solution to adjust the pH to 10, add 2 times the amount of ethyl acetate Extract 3 times, combine the extracts, put them on a silica gel column, elute with ethanol, collect the 7th-30th column volume section, combine the eluents, concentrate under reduced pressure to recover the solvent, dry under reduced pressure, pulverize, take the powder and add 6 times the amount of 1% Dissolve in hydrochloric acid, filter, add sodium bicarbonate solution to the filtrate to adjust the pH to 9.5...

Embodiment 2

[0150] Take 1000g of Nuxychnium, crush it into a coarse powder, add 10 times the amount of 50% ethanol, heat and reflux twice, each time for 1.5h, combine the extracts, filter, concentrate under reduced pressure to recover the ethanol until there is no alcohol smell, and concentrate the filtrate to a concentration of 0.5g medicinal material / ml, add hydrochloric acid to adjust the acid content to 1%, add 1 times the amount of chloroform to extract once, take the raffinate, add sodium hydroxide solution to adjust the pH to 11, add 1 times the amount of chloroform Extract 2 times, combine the extracts, put on a silica gel column, elute with methanol, collect the 5th-20th column volume section, concentrate under reduced pressure, recover the solvent, dry under reduced pressure, pulverize, take 10 times the amount of powder, dissolve it with 0.5% hydrochloric acid, and filter , add sodium hydroxide solution to the filtrate to adjust the pH to 9.5, let it sit for crystallization and ...

Embodiment 3

[0153] Take 1000g of Nuxyche, crush it into coarse powder, add 8 times the amount of 60% ethanol, heat and reflux three times, 2 hours each time, combine the extracts, filter, concentrate under reduced pressure to recover ethanol until there is no alcohol smell, and concentrate the filtrate to a concentration of 1g Amount of medicinal materials / ml, add sulfuric acid to adjust the acid content to 0.5%, add 4 times the amount of chloroform to extract 3 times, take the raffinate, add potassium hydroxide solution to adjust the pH to 9, add 4 times the amount of chloroform to extract 4 Once, combine the extracts, put them on a silica gel column, mix and elute with methanol and acetone (1:1), collect the 11th-35th column volume section, concentrate under reduced pressure, recover the solvent, dry under reduced pressure, crush, and add 20 times the amount of powder Dissolve 0.3% sulfuric acid, filter, add potassium hydroxide solution to the filtrate to adjust the pH to 10.6, stand for...

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Abstract

The invention discloses a method for extracting, separating and purifying strychnine, and belongs to the technical field of medicine. The method includes but is not limited to the steps of: taking strychnos nux-vomica L., grinding the taken strychnos nux-vomica L. into coarse powder, performing extraction by using ethanol, combining extract, performing filtration, concentrating filtrate, and recovering the ethanol until no alcohol is smelt so as to obtain concentrated extract of total alkali of strychnos nux-vomica L.; acidifying the concentrated extract of total alkali of strychnos nux-vomicaL., performing extraction for impurity removal by adding an organic solvent, performing alkalinization on raffinate, and performing extraction by adding an organic solvent so as to obtain extract; adding the extract into a silica gel chromatographic column for elution, collecting the strychnine section of eluent, performing combining, concentration and drying, and performing purification by usinga recrystallization method to obtain the strychnine with a purity of 95% or more.

Description

technical field [0001] The invention relates to a method for extracting active ingredients of traditional Chinese medicine, in particular to a method for extracting strychnine from the traditional Chinese medicine Strychnium chinensis, belonging to the technical field of medicines. Background technique [0002] Nuxychia, also known as Pancha, was first recorded in "Compendium of Materia Medica", bitter in taste, cold in nature, highly poisonous, and returned to the liver and spleen meridians. It is clinically used for diseases such as rheumatism obstinate numbness, numbness and paralysis, bruises, carbuncle, sequelae of poliomyelitis, rheumatoid arthritis and other diseases; but its highly toxic characteristics seriously affect its clinical application. The agent is good at resolving serious illnesses". The therapeutic dose of Nuxychnium is 0.3-0.6g, and overdose is prone to poisoning. How to use Nuxychnium reasonably and safely has become one of the research hotspots in re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22A61K31/475A61P29/00
CPCA61K31/475C07D491/22
Inventor 张保献李艳英吴珍珍杨新涛
Owner BEIJING INCREASEPHARM CORP LTD
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