A kind of stemodane type diterpenoid compound and its preparation method and application
A technology of compounds and diterpenoids, applied in the application of antitumor drugs, in the field of preparation of stemodane-type diterpenoids, can solve rare problems and the like
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Embodiment 1
[0017] Embodiment one: the preparation method of compound trigoheterone A (one)
[0018] After crushing the branches and leaves of Samboa heterophyllum (26.2kg, Hainan) dried in the shade, use 85% ethanol solution to extract three times by cold soaking, each time extracting for one week, filtering, collecting the filtrate, and concentrating under reduced pressure to obtain the ethanol extract; adding water to the ethanol extract Suspension was prepared, extracted with petroleum ether and ethyl acetate successively, and the ethyl acetate extract was concentrated under reduced pressure to obtain 327.9 g of ethyl acetate extract; the ethyl acetate extract was subjected to column chromatography separation and purification: ethyl acetate The ester extraction extract was separated by silica gel column chromatography, petroleum ether-acetone gradient elution (95:5, 85:15, 70:30 and 50:50), and petroleum ether-acetone (volume ratio 70:30) was collected for washing To remove the substa...
Embodiment 2
[0026] Embodiment two: the preparation method of compound trigoheterone A (two)
[0027] The shade-dried branches and leaves of Samboa heterophyllum (100.8kg, Hainan) were crushed and extracted three times by cold immersion in methanol, each time for 3 days, filtered, the filtrate was collected, and concentrated under reduced pressure to obtain the ethanol extract. Add water to the methanol extract to make a suspension, sequentially extract with petroleum ether and ethyl acetate, concentrate the ethyl acetate extract under reduced pressure to obtain 1386.2 g of ethyl acetate extract; separate and purify the ethyl acetate extract by column chromatography : The ethyl acetate part extract is separated by silica gel column chromatography, petroleum ether-acetone gradient elution (95:5, 85:15, 70:30 and 50:50), and petroleum ether-acetone (volume ratio 70 :30) eluate, get sherwood oil-acetone (volume ratio 70:30) eluate removes pigment with MCI resin column chromatography, use meth...
Embodiment 3
[0029] Example 3: Research on antitumor activity of compound trigoheterone A
[0030] 1. Experimental method: Five common tumor cell lines HL-60, A549, SMMC-7721, MCF-7 and SW480 were respectively used in RPMI-1640 medium containing 10% calf serum at 37°C and 5% CO 2 cultured in an incubator. The MTT method was used to carry out the cell proliferation inhibition test. The main operation was: take the tumor cell line in the logarithmic growth phase, digest it with 0.25% trypsin, and prepare 5×10 RPMI-1640 culture solution with 10% newborn calf serum 4 cells / mL of cell suspension, inoculated in 96-well plate, inoculated 180 μL per well. at 37°C, 5% CO 2 Cultivate for 8-10 hours under saturated humidity conditions, and when they adhere to the wall, add sample solution prepared with PBS to each well so that the final concentrations of the samples are 0.1, 1, and 10 μg / mL, respectively. For each concentration, 3 wells were paralleled, and after 44 hours of continuous culture, 50...
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