Extraction, separation and purification method for strychnos total alkaloid

Abstract

The invention discloses an extraction, separation and purification method for strychnos total alkaloid, and belongs to the technical field of medicines. The method comprises but is not limited to the following steps of: treating strychnos coarse powder via an acid water extraction-organic solvent extraction method or an alkalization-organic solvent extraction method or an alcohol extraction-organic solvent extraction method to obtain the strychnos total alkaloid; purifying the total alkaloid via a solvent-stepwise extraction method or a column chromatography method or a hydrochloride-sulphate stepwise crystallization method; and then preparing via the hydrochloride-sulphate stepwise crystallization method or the column chromatography method to obtain strychnine having a purity of greater than 90%.

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 Nuxychnami 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...

Examples

Embodiment 1

[0074] Take 1000g of Nuxychnium, crush it into coarse powder, add 10 times the amount of 1mol / L hydrochloric acid, heat and reflux twice for 1.5 hours each time, combine the extracts, filter, add sodium hydroxide to the filtrate to adjust the pH value to 10, add 3 times Extract with ethyl acetate for 3 times, combine the extracts, recover the ethyl acetate under reduced pressure, continue to dry under reduced pressure, and pulverize to obtain the total alkaloids of strychnium; add 6 times the amount of ammonia water to dissolve the total alkaloids, filter, and double the filtrate Measure ethyl acetate and extract 4 times, combine the extracts, recover ethyl acetate under reduced pressure, continue to dry under reduced pressure, and pulverize to obtain the crude product of strychnine; After forming crystals, filter, alkalinize the filtrate, add dilute sulfuric acid to form strychnine sulfate, and recrystallize to obtain strychnine.

[0075] The purity of the obtained strychnine...

Embodiment 2

[0077] Take 1000g of Nuxyche, crush it into a coarse powder, add 12 times the amount of 2mol / L sulfuric acid, heat and reflux once for 2 hours each time, combine the extracts, filter, add sodium hydroxide to the filtrate to adjust the pH value to 11, and add 1 time The amount of ethyl acetate was extracted twice, the extracts were combined, the ethyl acetate was recovered under reduced pressure, and then dried under reduced pressure and crushed to obtain the total alkaloid of strychnium; the total alkaloid was dissolved by adding 5 times the amount of sodium hydroxide solution, filtered, and the filtrate Add 2 times the amount of ethyl acetate to extract 3 times, combine the extracts, recover ethyl acetate under reduced pressure, continue drying under reduced pressure, and pulverize to obtain the crude product of strychnine; add hydrochloric acid solution to the crude product of strychnine, place it, and make Strychnine forms crystals and is filtered. After the filtrate is alka...

Embodiment 3

[0080] Take 1000g of Nuxychnium, crush it into a coarse powder, add 5 times the amount of 0.5mol / L hydrochloric acid, heat and reflux 3 times, each time for 0.5 hours, combine the extracts, filter, add sodium hydroxide to the filtrate to adjust the pH to 10, add 1 Double the amount of ethyl acetate and extract 4 times, combine the extracts, recover the ethyl acetate under reduced pressure, continue to dry under reduced pressure, and pulverize to obtain the total alkaloid of strychnium; Absorb on a porous adsorption column, elute with methanol-water gradient, detect each fraction by thin-layer chromatography, collect the eluate containing strychnine, combine, concentrate under reduced pressure, evaporate to dryness, and pulverize to obtain strychnine Crude product: add strychnine to hydrochloric acid solution, let stand to make strychnine form crystals, filter, add dilute sulfuric acid to the filtrate to make it alkalized to form strychnine sulfate, and recrystallize to obtain s...

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 Nuxychnami 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...

Examples

Embodiment 1

[0074] Take 1000g of Nuxychnium, crush it into coarse powder, add 10 times the amount of 1mol / L hydrochloric acid, heat and reflux twice for 1.5 hours each time, combine the extracts, filter, add sodium hydroxide to the filtrate to adjust the pH value to 10, add 3 times Extract with ethyl acetate for 3 times, combine the extracts, recover the ethyl acetate under reduced pressure, continue to dry under reduced pressure, and pulverize to obtain the total alkaloids of strychnium; add 6 times the amount of ammonia water to dissolve the total alkaloids, filter, and double the filtrate Measure ethyl acetate and extract 4 times, combine the extracts, recover ethyl acetate under reduced pressure, continue to dry under reduced pressure, and pulverize to obtain the crude product of strychnine; After forming crystals, filter, alkalinize the filtrate, add dilute sulfuric acid to form strychnine sulfate, and recrystallize to obtain strychnine.

[0075] The purity of the obtained strychnine...

Embodiment 2

[0077] Take 1000g of Nuxyche, crush it into a coarse powder, add 12 times the amount of 2mol / L sulfuric acid, heat and reflux once for 2 hours each time, combine the extracts, filter, add sodium hydroxide to the filtrate to adjust the pH value to 11, and add 1 time The amount of ethyl acetate was extracted twice, the extracts were combined, the ethyl acetate was recovered under reduced pressure, and then dried under reduced pressure and crushed to obtain the total alkaloid of strychnium; the total alkaloid was dissolved by adding 5 times the amount of sodium hydroxide solution, filtered, and the filtrate Add 2 times the amount of ethyl acetate to extract 3 times, combine the extracts, recover ethyl acetate under reduced pressure, continue drying under reduced pressure, and pulverize to obtain the crude product of strychnine; add hydrochloric acid solution to the crude product of strychnine, place it, and make Strychnine forms crystals and is filtered. After the filtrate is alka...

Embodiment 3

[0080] Take 1000g of Nuxychnium, crush it into a coarse powder, add 5 times the amount of 0.5mol / L hydrochloric acid, heat and reflux 3 times, each time for 0.5 hours, combine the extracts, filter, add sodium hydroxide to the filtrate to adjust the pH to 10, add 1 Double the amount of ethyl acetate and extract 4 times, combine the extracts, recover the ethyl acetate under reduced pressure, continue to dry under reduced pressure, and pulverize to obtain the total alkaloid of strychnium; Absorb on a porous adsorption column, elute with methanol-water gradient, detect each fraction by thin-layer chromatography, collect the eluate containing strychnine, combine, concentrate under reduced pressure, evaporate to dryness, and pulverize to obtain strychnine Crude product: add strychnine to hydrochloric acid solution, let stand to make strychnine form crystals, filter, add dilute sulfuric acid to the filtrate to make it alkalized to form strychnine sulfate, and recrystallize to obtain s...

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