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Preparation method of allocryptopine

A technology to separate cryptic alkali and acid water, applied in organic chemistry and other directions, can solve the problems of large amount of organic solvent and many cryptic alkali impurities, and achieve the effect of removing impurities, high product purity, easy elution and regeneration.

Inactive Publication Date: 2011-11-09
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese Patent Application No. 03118201.1 uses a macroporous resin to separate sanguinarine and chelerythrine, but the allocryptine involved is a mixture with the original opioid, and the allocryptine monomer component is obtained without separation and purification
The method uses a large amount of organic solvent, and the isolated allocryptopine impurities are many

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Grind 500 g of summer free medicinal material into coarse powder, soak in 0.6% (mass volume ratio) hydrochloric acid solution for 10 hours, percolate at a percolation speed of 5ml / min·kg, adjust the percolation solution to pH7.5, pass through DA201 Macroporous resin column, first wash with water to remove impurities, then elute with 30% ethanol, collect and concentrate the eluate, extract with dichloromethane 1.2 times the volume of the concentrated solution, repeat the extraction 4 times, combine the extracts, concentrate, concentrate Mix the sample with an appropriate amount of alumina and put it on the column. The particle size of alumina is 100-300 mesh. The eluent is a mixed solvent of ethyl acetate-methanol. 10:1, 5:1 and 1:1, collect the fractions in sections, combine the allocryptine fractions, concentrate and crystallize under reduced pressure, filter out the coarse crystals, and then weigh them with ethyl acetate-ethanol (5:1). Crystallization to obtain a colo...

Embodiment 2

[0020] Grind 1 kg of summer free medicinal material into coarse powder, soak it with 0.4% (mass volume ratio) hydrochloric acid solution for 16 hours, percolate at a percolation speed of 5ml / min·kg, adjust the percolation solution to pH8.0, pass through DM301 The macroporous resin column was first washed with water to remove impurities, then eluted with 25% ethanol, collected and concentrated the eluate, extracted with chloroform of 1.5 times the volume of the concentrated solution, extracted repeatedly 5 times, combined the extracts, concentrated, and the concentrated solution was mixed with Mix an appropriate amount of alumina and put the sample on the column. The particle size of alumina is 100-300 mesh. The eluent is a mixed solvent of ethyl acetate-methanol. According to the volume ratio, from high to low, the order is 50:1, 20:1, 10: 1, 5:1 and 1:1, collect the fractions in sections, combine the allocryptine fractions, concentrate and crystallize under reduced pressure, f...

Embodiment 3

[0022] Pulverize 1 kg of Boluohuigen into coarse powder, soak for 15 hours with 0.2% (mass to volume ratio) sulfuric acid solution, percolate, the percolation speed is 6ml / min·kg, adjust the percolation solution to pH8.5, pass DS401 macroporous resin column, first wash with water to remove impurities, then elute with 40% ethanol, collect and concentrate the eluate, extract with dichloromethane equal to the volume of the concentrated solution, repeat the extraction 3 times, combine the extracts, concentrate, Mix the concentrated solution with an appropriate amount of alumina and put the sample on the column. The particle size of alumina is 100-300 mesh. The eluent is a mixed solvent of ethyl acetate-methanol. According to the volume ratio, from high to low, the order is 50:1, 20:1 , 10:1, 5:1 and 1:1, collect the fractions in sections, combine the allocryptine fractions, concentrate and crystallize under reduced pressure, filter out the coarse crystals, and reweight with petrole...

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PUM

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Abstract

The invention discloses a preparation method of allocryptopine. The preparation method is performed according to the following process steps: A. acidic water extraction: soaking allocryptopine-rich poppy plants used as raw materials in acidic water, and carrying out percolation extraction; B. macroporous resin enrichment: regulating the pH value of the extract liquid to 7.5-8.5, passing through a macroporous adsorption resin column, and concentrating the eluate; C. solvent extraction: extracting the concentrated eluate with an organic solvent; D. column chromatography: carrying out gradient elution with ethyl acetate and methanol while using alumina or silica gel as the column packing, and collecting eluates segment by segment; and E. crystallization: crystallizing with a mixed solvent to obtain an allocryptopine product with a purity higher than 95%. Compared with the prior art, the preparation method disclosed by the invention has the advantages of simple process, low cost and little environmental pollution, and is suitable for industrial production.

Description

Technical field: [0001] The invention belongs to the technical field of extraction and separation of effective parts of traditional Chinese medicines, and in particular relates to a method for extracting and preparing allocryptine from summer berries. Background technique: [0002] Allocryptopine, molecular formula: C 21 h 23 NO 5 , Molecular weight: 369.40, is a kind of tertiary amine alkaloid isolated from poppy family plants (such as Boluohui, Xueshuicao, celandine, summerless, etc.), colorless, soluble in ethanol, chloroform, ether, acetic acid Ethyl ester and dilute acid, mp.160-161℃. The core structure of allocryptine has an isoquinoline structure similar to that of many antiarrhythmic traditional Chinese medicines. Liu Mohan has proved through experiments that it has various antiarrhythmic effects. Allocryptine resistance is strengthened by the aconitine-induced sympathetic nervous system, and then promotes the release of endogenous catecholamines, which increases...

Claims

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Application Information

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IPC IPC(8): C07D491/056
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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