Method for extracting qingdainone from isatis tinctoria
A technology of indigo and woad, which is applied in the field of medicine to achieve the effects of improving purity, increasing extraction rate, and saving solvents
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Embodiment 1
[0014] Grind the stems and leaves of Isatis indigo, weigh 1000g, add 95% methanol solution equivalent to three times the amount of raw materials, soak for 2 hours, then heat to 84°C for Soxhlet extraction for 6 hours, collect the extract and take the liquid to recover methanol under reduced pressure until there is no alcohol smell. Add water to dissolve and disperse, centrifuge, put the supernatant on the HZ841 macroporous adsorption resin column, first flush the column with 20% ethanol solution until the eluate flows out colorless, then elute with 60% ethanol solution, collect the 60% ethanol eluate, Concentrate under reduced pressure, extract repeatedly 6 times with diethyl ether, and concentrate and dry the extract to obtain the crude product of Qingdanone. Dissolve the crude Qingdan ketone in methanol, filter it through a microporous membrane, and separate it by preparative high-performance liquid chromatography. Chromatographic column: C18, mobile phase: acetonitrile-water...
Embodiment 2
[0016] Crush the stems and leaves of Isatis indigo, weigh 1000g, add 75% ethanol solution equivalent to 5 times the amount of raw materials, soak for 2 hours, then heat to 93°C for Soxhlet extraction for 8 hours, collect the extract and take the liquid to recover ethanol under reduced pressure until it has no alcohol smell. Add water to dissolve and disperse, centrifuge, put the supernatant on a carboxymethyl-type weakly acidic cationic resin column, first wash the column with water until the eluate flows out colorless, then elute with 5% ammonia water by volume, collect the ammonia water eluate, Concentrate under reduced pressure, extract repeatedly 5 times with diethyl ether, concentrate and dry the extract to obtain crude Qingdan ketone. Dissolve the crude Qingdan ketone in methanol, filter it through a microporous membrane, and separate it by preparative high-performance liquid chromatography. Chromatographic column: C18, mobile phase: acetonitrile-water (60:40), flow rate ...
Embodiment 3
[0018] Grind the stems and leaves of Isatis indigo, weigh 1000g, add 60% methanol solution equivalent to 4 times the amount of raw materials, soak for 1h, then heat to 85°C for Soxhlet extraction for 10h, collect the extract and take the liquid to recover methanol under reduced pressure until there is no alcohol smell. Add water to dissolve and disperse, centrifuge, put the supernatant on D101 macroporous adsorption resin column, first flush the column with 10% ethanol solution until the eluate flows out colorless, then elute with 80% ethanol solution, collect 75% ethanol eluate, Concentrate under reduced pressure, extract repeatedly 3 times with ether, and concentrate and dry the extract to obtain the crude product of Qingdanone. Dissolve the crude Qingdan ketone in methanol, filter it through a microporous membrane, and separate it by preparative high-performance liquid chromatography. Chromatographic column: C18, mobile phase: acetonitrile-water (62:38), flow rate 50ml / min, ...
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