Isocoumarin compound and preparation method and application thereof
A technology of isocoumarin and compounds, applied in the field of extraction and separation of plant effective components
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[0027] The preparation method of the isocoumarin compound of the present invention is to use the three tendons of dry Lauraceae plant hairy leaves ( Lindera caudata ) as a raw material obtained through extract extraction, organic solvent extraction, MCI decolorization, silica gel column chromatography, and high-pressure liquid chromatography separation steps, specifically:
[0028] A, extraction of extract: the three tendons of Lauraceae plant hairy leaves ( Lindera caudata ) was crushed to 20-40 mesh, ultrasonically extracted 2-5 times with an organic solvent, 30-60 minutes each time, the extracts were combined, filtered, concentrated extracts under reduced pressure, left to stand, filtered to remove sediment, concentrated into extract a;
[0029] B. Organic solvent extraction: Add 1 to 2 times the amount of water by weight to the extract a, extract 3 to 5 times with an organic solvent equal to the volume of water, combine the organic solvent extraction phase, and concentrat...
Embodiment 1
[0044] Take 1.5 kg of dry three-leaved lauraceae plant hairy leaves, coarsely crush to 40 mesh, ultrasonically extract 4 times with 70% acetone, 60 min each time, combine the extracts; filter the extracts, concentrate under reduced pressure to 1 / 2 of the volume 4; Stand still, filter out the precipitate, concentrate into 120g of extract a; add 240g of water to extract a, extract 5 times with chloroform equal to the volume of water, combine the extraction phases, concentrate under reduced pressure into 50g of extract b; extract b is packed with MCI, add 100 g of 80% methanol water to the extract b to dissolve, then put it on the column, elute with 1 to 4 liters of 90% methanol water, collect the eluate, and concentrate under reduced pressure to obtain 30g extract c; extract c is packed with 200 mesh silica gel 160 g column, add 60 g acetone to dissolve in extract c, then add 100 mesh silica gel 60 g to mix the sample, and put on the column after mixing the sample; 20:1, 9:1, 8:...
Embodiment 2
[0046] Dried 3 kg of lauraceae hairy leaves, coarsely crushed to 20 mesh, ultrasonically extracted 5 times with 100% ethanol for 30 minutes each time, and the extracts were combined; the extracts were filtered and concentrated under reduced pressure to 1 / 4 of the volume; Stand still, filter out the precipitate, concentrate into 240 g of extract a; add 360 g of water to extract a, extract 3 times with ethyl acetate equal to the volume of water, combine the extract phases, and concentrate under reduced pressure to obtain 100 g of extract a. Extract b; extract b is packed with MCI, add 150 g of 80% methanol water to the extract b to dissolve, then put it on the column, elute with 2 to 6 liters of 90% methanol water, collect the eluate, and concentrate under reduced pressure Obtain 60 g of extract c; use 320 g of 200-mesh silica gel to pack column for extract c, add 120 g of acetone to dissolve extract c, then add 120 g of 100-mesh silica gel to mix the sample, and put it on the co...
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