A kind of alkaloid compound, preparation method and application
A technology of alkaloids and compounds, which is applied in the preparation of sugar derivatives, chemical instruments and methods, drug combinations, etc., can solve the problems of poor efficacy of complications, prolonged medication time, and prone to drug resistance, etc., to achieve beneficial The effects of large-scale production promotion, low cost, and simple extraction and separation methods
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[0051] The invention provides a kind of preparation method of alkaloid compound, specifically as follows:
[0052] S1, take a certain quality of Jiuzilian dry rhizome;
[0053]Use methanol or ethanol whose volume is 1 to 8 times the mass of the dried rhizome of Jiuzilian, heat and reflux for extraction 1 to 6 times near their respective boiling points, each time for 1 to 3 hours; wherein, if ethanol is used, the volume fraction of ethanol is 10 ~95%.
[0054] Alternatively, extract by cold soaking at room temperature for 1 to 5 times, each time for 1 to 3 hours;
[0055] Merge each extract and concentrate to obtain the total extract;
[0056] S2, the total extract obtained through step S1 is extracted at least once through ethyl acetate and n-butanol successively;
[0057] Liquid-liquid extraction is possible, that is, the total extract is suspended in water, the volume ratio of the total extract to water is 1:1 to 1:4, and the extract liquid is obtained, which is sequentia...
Embodiment 1
[0069] A kind of preparation method of alkaloid compound, concrete method is as follows:
[0070] 1) Take 20 kg of dried rhizomes of Jiuzilian, heat and reflux extract with methanol whose volume is 6 times the mass of dried rhizomes of Jiuzilian, extract 4 times, each time for 2 hours, combine the extracts to recover the solvent under reduced pressure, and obtain the total extract;
[0071] 2) Suspend the total extract in water of 4 times the amount, extract 4 times with ethyl acetate, then extract 4 times with n-butanol equal volume, and remove the organic solvent under reduced pressure in the extraction layer to obtain ethyl acetate and n-butyl alcohol respectively. Alcohol layer.
[0072] 3) Take 200 g of the n-butanol extraction layer, firstly, by using silica gel column chromatography, chloroform / methanol is 100:0~0:100 in volume ratio (v / v) for gradient elution, collect a fraction every 800mL, and pass through TLC A total of 15 fractions were obtained after identificati...
Embodiment 2
[0076] A kind of preparation method of alkaloid compound, concrete method is as follows:
[0077] 1) Take 20 kg of dried rhizomes of Jiuzilian, heat and reflux extraction with ethanol whose volume is 8 times the mass of dried rhizomes of Jiuzilian, and extract them under reflux for 3 times, each time for 3 hours, wherein the volume fraction of ethanol is 10%, and the combined extracts are decompressed Recover the solvent to obtain the total extract;
[0078] 2) Suspend the total extract in 3 times the amount of water, first extract 3 times with ethyl acetate, then extract 3 times with an equal volume of n-butanol, remove the organic solvent from the extraction layer to obtain ethyl acetate and n-butyl alcohol respectively Alcohol layer.
[0079] 3) Take 80 g of the n-butanol extraction layer, firstly, by using silica gel column chromatography, chloroform / methanol is 100:0~0:100 in volume ratio (v / v) for gradient elution, collect a fraction every 500mL, and pass through TLC A...
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