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
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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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