Preparation method of sliver-white aglaione A
A technology for silver white milanone and silver white milanone A is applied in the field of preparation of silver white milanone A, which can solve the problems of complicated operation, low sample yield, small preparation amount, etc., and achieves high product purity and simple process. Easy to operate effect
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[0012] Example 1:
[0013] Take the silver-white Mi Zilan leaves, dry and crush, weigh 10kg, add 8 times the amount of 90% ethanol solution, reflux and extract 3 times, shrink the extract to no alcohol and add an appropriate amount of water to dilute it and add it to D101 macroporous resin for adsorption, first use 7 times The column volume is 50% ethanol solution to elute impurities, and then 6 times the column volume 80% ethanol solution is used to elute the effective components. The eluent is recovered and the solvent is placed in the precipitate. The precipitate is filtered out and dissolved in 95% ethanol by heating, and an appropriate amount of water is added to the alcohol concentration 50%, add an equal volume of petroleum ether and stir well, collect the petroleum ether layer and filter with suction, collect the filter cake and dissolve the crystals with 80% ethanol solution 3 times, and dry to obtain 3g of silver-white mizilanone A. The content is 98.3% by HPLC.
Example Embodiment
[0014] Example 2:
[0015] Take the silver-white Mi Zilan leaves, dry them, and crush them, weigh 10 kg, add 10 times the amount of 80% ethanol solution, reflux for 2 times, shrink the extract to alcohol-free and dilute with a proper amount of water, then add it to AB-8 macroporous resin for adsorption, use first 10 times the column volume of 40% ethanol solution to elute impurities, and then 5 times the column volume of 90% ethanol solution to elute the effective ingredients, the eluent is recovered solvent and placed in the precipitate, the precipitate is filtered out and heated with 90% ethanol to dissolve it, and an appropriate amount of water is added to The alcohol concentration is 40%, add an equal volume of petroleum ether and stir well, collect the petroleum ether layer and suction filter, collect the filter cake and then dissolve the crystals with 90% ethanol solution 3 times, and dry to obtain 2.7g of silver white Michelanone A. The content is tested by HPLC. 97.2%...
Example Embodiment
[0016] Example 3:
[0017] Take the silver-white Mi Zilan leaves, dry them, and crush them, weigh 10 kg and add 10 times the amount of 70% ethanol solution, reflux and extract for 2 times. The extract is reduced to alcohol-free and diluted with a suitable amount of water and then added to HZ816 macroporous resin for adsorption, first use 7 times The column volume is 60% ethanol solution to elute the impurities, and then 5 times the column volume 80% ethanol solution is used to elute the effective ingredients. The eluent is recovered and the solvent is placed in the precipitate. The precipitate is filtered out and dissolved in 90% ethanol by heating, and an appropriate amount of water is added to the alcohol concentration 50%, add an equal volume of petroleum ether and stir well, collect the petroleum ether layer and filter by suction, collect the filter cake and dissolve the crystals with 90% ethanol solution 3 times, and dry to obtain 3.5 g of silver-white mizilanone A. The c...
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