Preparation method of bicuculline and fumarine

A technology of bikokoline and proto-opiate, which is applied in the field of preparation of bikokoline and proto-opioid, and can solve the problems of low yield and difficulty in industrialized production, etc.

Active Publication Date: 2018-02-09
成都瑞芬思德丹生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the current technology, there is no preparation method that can separate and purify bikokolinine from plants, and

Method used

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  • Preparation method of bicuculline and fumarine
  • Preparation method of bicuculline and fumarine
  • Preparation method of bicuculline and fumarine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Extraction: Take one or more of the medicinal materials Xia Wu, Corydalis Corydalis or Corydalis rhizome, pulverize, and extract with acidic methanol or ethanol solution, the acidic methanol or ethanol solution contains hydrochloric acid with a volume percentage of 0.1-2%, and 50-100% by volume of methanol or ethanol, reflux extraction to obtain extract A, extract 1-2 hours each time, extract 3-6 times, combine the extracts, concentrate under reduced pressure at 50-70°C until alcohol-free, Concentrate B was collected.

[0026] 2) Separation and enrichment: Take the concentrated solution B, adjust the pH to 3-5 with 0.1%-2% hydrochloric acid solution, and perform adsorption on the reverse polymerization filler C. The reverse polymerization filler C is AB-8 macroporous resin. 3 column volumes of water were eluted to obtain washing solution D, and then analyzed with 3 times column volume of alcohol solution E, alcohol solution E was 30-50% methanol or ethanol, collected...

Embodiment 2

[0035] 1) Extraction: take the medicinal material Xia Xia, grind it, and extract it with an acidic methanol or ethanol solution, which contains 0.1-2% hydrochloric acid by volume, and extract it under reflux to obtain the extract A, and extract 1-2% each time. After 2 hours, extract 3-6 times, combine the extracts, concentrate under reduced pressure at 50-70°C until there is no alcohol, and collect the concentrated solution B.

[0036] 2) Separation and enrichment: Take the concentrated solution B, adjust the pH to 3-5 with 0.1%-2% hydrochloric acid solution, and perform adsorption on the reverse polymerization filler C. The reverse polymerization filler C is AB-8 macroporous resin. 3 column volumes of water were eluted to obtain washing solution D, and then analyzed with 3 times column volume of alcohol solution E, alcohol solution E was 30-50% methanol or ethanol, collected analysis solution F, and then analyzed with alcohol solution G, The alcohol solution G is 80-95% metha...

Embodiment 3

[0044] 1) Extraction: Take the summer medicinal material, grind it, and extract it with an acidic methanol or ethanol solution containing 0.1-2% hydrochloric acid by volume and 50-100% methanol or ethanol by volume. Any one of the extraction methods is selected from reflux extraction, ultrasonic extraction or percolation extraction to obtain extract A, extract 1-2 hours each time, extract 3-6 times, combine the extracts, and concentrate under reduced pressure at 50-70°C until alcohol-free , to collect the concentrate B.

[0045] 2) Separation and enrichment: Take the concentrated solution B, adjust the pH to 3-5 with 0.1%-2% hydrochloric acid solution, and perform adsorption on the reverse polymerization filler C. The reverse polymerization filler C is AB-8 macroporous resin. 3 column volumes of water were eluted to obtain washing solution D, and then analyzed with 3 times column volume of alcohol solution E, alcohol solution E was 30-50% methanol or ethanol, collected analysi...

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Abstract

The invention discloses a preparation method of bicuculline and fumarine. The preparation method comprises the following steps: 1) extracting: pulverizing a medicinal material, extracting with an acidmethanol or ethyl alcohol solution to obtain an extracting solution A, and conducting vacuum concentration to obtain a concentrated solution B; 2) separating and enriching: taking the concentrated solution B, regulating the PH, adsorbing through an inverse polymerization filler C, eluting with water firstly to obtain a washing solution D, then desorbing with an alcoholic solution E, collecting adesorbed solution F, and desorbing with an alcoholic solution G to obtain a desorbed solution H; 3) purifying: taking the desorbed solution H, conducting vacuum concentration to regulate the PH, standing, filtering a precipitate, stirring and mixing the precipitate, obtaining a solution J through silica gel chromatograph; conducting vacuum concentration on the desorbed solution F, regulating the PH to 9-10, and separating out a precipitate K; and regulating the PH of the washing solution D to 9-10, and separating out a precipitate L; and 4) crystalizing and drying: conducting vacuum concentration on the solution J, crystalizing and drying the solution J to obtain a pure product of bicuculline; and crystalizing and drying the precipitate K and the precipitate L to obtain a pure product of fumarine. By using the method, the yield is high, the purity is high, and the method can be applied to industrial production.

Description

technical field [0001] The invention relates to the field of natural medicinal chemicals, in particular to a method for preparing bikokolinine and protopine. Background technique [0002] Bicuculline (+)-Bicuculline molecular formula is C 20 h 17 NO 6 , molecular weight 367.36, CAS No. 485-49-4, light yellow powder, soluble in benzene, chloroform, ethyl acetate, slightly soluble in ethanol and ether; the molecular formula of Protopine is C 20 h 19 NO 5 , Molecular weight 353.37, CAS No. 130-86-9, white powder, soluble in benzene, chloroform, ethyl acetate, slightly soluble in ethanol and ether, these two compounds are alkaloid substances, and their structural formula is as follows. [0003] [0004] In the current technology, there is no preparation method that can separate and purify bikokolinine from plants, and the extraction method for the original opioidine also has the problems of low yield and difficulty in industrial production. Contents of the invention ...

Claims

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Application Information

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IPC IPC(8): C07D491/153C07D519/00
CPCC07D491/153C07D519/00
Inventor 董维珍常建红寇俊闯
Owner 成都瑞芬思德丹生物科技有限公司
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