Refined cherimoya total inner ester with anti-tumor activity and preparation method thereof
A technology of anemone lactones and total lactones, which is applied to the application field of refining total anemone lactones and its preparation and preparation of antitumor drugs, and can solve the problems of difficult control of drug quality and efficacy, low active ingredient content, high Unclear ingredients and other issues, to achieve the effect of controllable quality and safety, less active ingredients, and clear ingredients
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Embodiment 1
[0039] The extraction of the total lactones of cherimoya, get 2 kilograms of dry seeds of cherimoya, pulverize, and percolate twice with chloroform of 10 times the amount of seed meal, detect with silica gel thin-layer chromatography, the nearly percolation extraction of cinnamon lactones is complete, in Recover under reduced pressure below 60°C to obtain the concentrate, let it stand for 24 hours, centrifuge at 3000 rpm, and then take the centrifuged upper layer concentrate (88.7g) to obtain the crude extract of total lactones of custard apple.
[0040] Take 80g of the crude extract of total lactones of custard apple, add 1 times the amount of petroleum ether, heat and dissolve in a water bath at 60°C, mix well, and after standing for layers, absorb the upper layer of petroleum ether, concentrate, dry, and repeat the above operation for 3 times, to obtain the total lactones of custard apple 46g.
[0041] Take 46g of the above-mentioned total lactones of custard apple, mix it wi...
Embodiment 2
[0043] Extract the crude extract of total lactones of cherimoya according to the method of Example 1, extract 86.6g of total lactones from 2 kilograms of dry seeds of custard apple, get the crude extract of total lactones of custard apple 82g, add 10 times the amount Petroleum ether-water (5:1), heat and dissolve in a water bath at 80°C, mix evenly, and after standing to separate layers, absorb the upper petroleum ether layer, concentrate, dry, and repeat the above operation 3 times to obtain the total lactones of custard apple 47g.
[0044] Take 47g of the above-mentioned total lactones of custard apple, mix with the same amount of silica gel, grind it evenly, apply silica gel (400g, 200 to 300 mesh, Qingdao Ocean Chemical Factory) column chromatography, and use petroleum ether-ethyl acetate gradient elution, petroleum ether Ether-ethyl acetate (50:1) 1 to 21 fractions, petroleum ether-ethyl acetate (20:1) 22 to 55 fractions, petroleum ether-ethyl acetate (10:1) 56 to 70 frac...
Embodiment 3
[0046] The extraction of the total lactones of cherimoya, take 2 kilograms of dry seeds of cherimoya, pulverize, percolate twice with ethyl acetate of 10 times the amount of seed powder, detect with silica gel thin-layer chromatography, the cherimolides are nearly extracted completely, in The concentrate was recovered under reduced pressure below 60°C, left to stand for 24 hours, centrifuged at 3000 revolutions per minute, and then the supernatant concentrate (76.8g) obtained by centrifugation was taken, that is, the crude extract of total lactones of cherimoya.
[0047] Take 75g of the crude extract of total lactones of custard apple, add 5 times the amount of petroleum ether-water (1:1), heat and dissolve in a water bath at 50°C, mix well, and after standing for layers, absorb the upper petroleum ether layer and concentrate , dried, and the above operation was repeated once to obtain 41 g of total lactones of custard apple.
[0048] Get 40g of the above-mentioned total lacto...
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