Tricyclic alkaloid compound and preparation method and application thereof
A technology of alkaloids, compounds, applied in the field of phytochemistry
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[0025] The preparation method of the tricyclic alkaloid compound of the present invention is based on the horsetail lotus as a raw material, and is subjected to extraction from extract, silica gel column chromatography and high-pressure liquid chromatography separation and purification steps, specifically comprising:
[0026] A. Extraction: crush and sieve the cauliflower lotus, reflux and extract with 95% ethanol for 2-3 times, each time for 30-50 minutes, combine the extracts and concentrate to obtain material a, add tartaric acid solution to dilute material a to obtain material b , material b is extracted 1 to 3 times with ethyl acetate, the aqueous phase is collected to obtain material c, material c is saturated with sodium carbonate, extracted with ethyl acetate again 1 to 3 times, the extracted ethyl acetate phases are combined, concentrated under reduced pressure to obtain Extract d;
[0027] B. Silica gel column chromatography: Extraction a uses 160-300 mesh silica gel...
Embodiment 1
[0038] Preparation of tricyclic alkaloid compound C 16 h 17 NNaO 3 , including extracting extract, silica gel column chromatography, and high-pressure liquid chromatography separation, specifically adopting the following steps:
[0039] (1) Extraction of extract: Take the whole plant of Sargassum aureus, dry it in the sun, and crush it to about 30-50 meshes. Weigh 2.8-3.5 kg of crushed samples, place them in a 20-L glass reactor, add 10-15 L of 95% ethanol, reflux for 30-50 min, filter out the extract; add 95% 10-15 L of ethanol, reflux extraction for 30-50 min, and filter the extract. The two extracts were combined and concentrated to a small volume, then diluted with 5-8 L of 3% tartaric acid solution, and extracted twice with 5-8 L of ethyl acetate. After the extraction, the aqueous phase was saturated with sodium carbonate, and then extracted twice with 5-8 L of ethyl acetate. The extracted ethyl acetate phases were combined and concentrated under reduced pressure to o...
Embodiment 2
[0045] The sample of horsetail lotus came from Heqing County, Dali, Yunnan. Take the whole plant of Saccharomyces aureus, dry it in the sun, and crush it to about 35 meshes. Weigh 3.0 kg of the pulverized sample, place it in a 20 L glass reactor, add 12 L of 95% ethanol, reflux for extraction for 40 min, and filter out the extract; add 12 L of 95% ethanol to the residue again, and reflux for extraction After 40 min, the extract was filtered off. The two extracts were combined and concentrated to a small volume, then diluted with 6 L of 3% tartaric acid solution, and extracted twice with 6 L of ethyl acetate. After the extraction, the aqueous phase was saturated with sodium carbonate, extracted twice again with 6 L of ethyl acetate, and the extracted ethyl acetate phases were combined and concentrated under reduced pressure to obtain 36.3 g of alkaloid part extract. The extract was mixed with 45 g (80-100 mesh) crude silica gel, dried, and 180 g silica gel (150-200 mesh) was ...
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