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Method for Extracting and Separating Alkaloids from Junggar Aconitum

A technology for aconitum and aconitine in Junggar, which is applied in the field of extraction and separation of alkaloids and can solve problems such as extraction and separation

Active Publication Date: 2016-06-22
XINJIANG MEDICAL UNIV AFFILIATED HOSPITAL OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although existing reports have analyzed the components of total alkaloids in Aconitum aconitum, how to extract and separate the alkaloid components detected in the analysis from Aconitum aconitum is still a problem to be overcome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Junggar aconitum root (10.0kg), crushed (passed through a 20-mesh sieve), extracted by cold soaking in 95wt% ethanol for 3 times, 27L / time, the extract was concentrated by thin film evaporation and then suspended in 5500ml of 2wt% hydrochloric acid to fully dissolve the alkaloids In the suspension, extract and degrease with petroleum ether; adjust the pH of the remaining water to 4 with ammonia water, and then extract with dichloromethane to obtain the dichloromethane phase. The dichloromethane phase is chromatographed on a silica gel column and eluted with a mixture of petroleum ether-ethyl acetate-diethylamine. The volume ratio of petroleum ether-ethyl acetate-diethylamine is 8:2:0.5, and the flow rate is 20ml / min , 1000ml of eluents were collected each time, and the eluents collected from the 18th to 23rd times were combined, crystallized, and filtered to obtain compound 1 (1.5449g), which was determined to be a single compound by TLC thin layer chromatography.

[00...

Embodiment 2

[0018] Junggar aconitum root (10.0kg), crushed (passed through a 20 mesh sieve), extracted by cold immersion in 95wt% ethanol for 3 times, 27L / time, the extract was concentrated by thin film evaporation and then suspended in 5500ml of 2% hydrochloric acid to fully dissolve the alkaloids In the suspension, extract and degrease with petroleum ether; adjust the pH of the remaining water to 8 with ammonia water, and then extract with dichloromethane to obtain the dichloromethane phase. The dichloromethane phase was chromatographed on a silica gel column, eluted with a mixture of petroleum ether-ethyl acetate-diethylamine with a volume ratio of 10:1:0.5, and the flow rate was 20ml / min. Each 1000ml eluent was collected, and the first The eluents collected from 6 to 11 times were combined, crystallized and filtered to obtain compound 2 (1.3345 g), which was confirmed as a single compound by TLC thin layer chromatography.

[0019] Compound 2: colorless prismatic crystal, positive for ...

Embodiment 3

[0021] Junggar aconitum root (10.0kg), crushed (passed through a 20 mesh sieve), extracted by cold immersion in 95wt% ethanol for 3 times, 27L / time, the extract was concentrated by thin film evaporation and then suspended in 5500ml of 2% hydrochloric acid to fully dissolve the alkaloids In the suspension, extract and degrease with petroleum ether; adjust the pH of the remaining water to 8 with ammonia water, and then extract with dichloromethane to obtain the dichloromethane phase. The dichloromethane phase was chromatographed on a silica gel column, eluted with petroleum ether-ethyl acetate-diethylamine with a volume ratio of 10:1:0.5, and the flow rate was 20ml / min. Based on each collection of 1000ml, the first to third The eluent collected for the second time was combined, and the combined eluent was passed through a SephadexLH-20 gel column, and then eluted with a mixture of chloroform-petroleum ether-methanol with a volume ratio of 5:5:1, and the flow rate was 5ml / min, t...

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PUM

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Abstract

The invention discloses a method for extracting and separating alkaloids from acoitum soogaricum. The method comprises the following steps: (1) extracting acoitum soogaricum with ethanol, regulating the pH value of leaching liquid to 4-8, and extracting with dichloromethane; and (2) processing the dichloromethane phase, extracted in the step (1), by a silicagel column, and eluting by using a petroleum ether-ethyl acetate-diethylamine mixed solution, so as to obtain alkaloids. Four single alkaloids which are respectively extracted and separated from roots of acoitum soogaricum by adopting the method disclosed by the invention are respectively aconitine, Junggar aconitine, 16,17-dihydro-12beta, 16-beta-epoxy napelline and 12-epi-napelline.

Description

technical field [0001] The invention belongs to the field of extracting active ingredients of herbal medicines, and in particular relates to a method for extracting and separating alkaloids from Junggar aconitum. Background technique [0002] Junggar aconitum ( Aconitum soongoricum Stapf.) for Ranunculaceae ( Ranunculaceae ) Aconitum ( Aconitum ) perennial herbaceous plants. In our country, it is produced in Xinyuan, Nileke and other counties in Ili, Xinjiang, and is born on the sunny slopes of mountains and grasslands at an altitude of 1800-2600 meters. [1] . Its roots are used for medicine, and the tuberous roots are highly toxic, which can dispel wind and cold, dehumidify, and relieve pain. Although existing reports have analyzed the components of total alkaloids in Aconitum aconitum, how to extract and separate the alkaloid components detected by analysis from Aconitum aconitum is still a problem to be overcome. Contents of the invention [0003] The purpose of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D221/22C07D491/08
CPCC07D221/22C07D491/08
Inventor 赵翡翠赵军聂继红汪芳杨俊玲
Owner XINJIANG MEDICAL UNIV AFFILIATED HOSPITAL OF CHINESE MEDICINE