A kind of preparation method of privetin reference substance
A kind of technology of special privet glycoside and reference substance, applied in the field of modernization of traditional Chinese medicine, can solve the problem of low purity of special privet glycoside
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Embodiment 1
[0054] A. Raw material extraction: crush 1 kg of Ligustrum lucidum medicinal material into coarse powder, add 10 L of ethanol solution with a volume fraction of 50%, heat extraction twice at 60°C for 2 hours each time, cool to room temperature, suction filter, and combine the filtrates , concentrated to no alcohol smell, a total of 1000ml;
[0055] B. Enrichment of macroporous resin: Weigh 3KgD101 macroporous adsorption resin and pack it into a column, statically adsorb the concentrated solution of step A with macroporous resin for 16 hours overnight, and then use 3L of water and 20% ethanol solution of 2L column volume respectively Elute the impurities, then elute the target substance with 3L of 40% ethanol solution, collect the eluate, and concentrate to 100ml;
[0056] C. Silica gel column chromatography: mix the 100ml concentrated solution of step B with 150g of 100-200 mesh silica gel, dry and crush, take 2kg of 200-300 mesh silica gel, and wet-pack the column with ethyl ...
Embodiment 2
[0061] A. Raw material extraction: crush 5 kg of Ligustrum lucidum medicinal material into coarse powder, add 50 L of ethanol solution with a volume fraction of 55%, heat extraction at 60°C for 2 times, each time for 2 hours, cool to room temperature, suction filter, and combine the filtrates , concentrated to no alcohol smell, a total of 5000ml;
[0062] B. Macroporous resin enrichment: Weigh 18KgD101 macroporous adsorption resin and pack it into a column, use the concentrated solution of step A to statically adsorb the macroporous resin overnight for 18 hours, and then use 15L of water and 10L of column volume of 20% ethanol solution Elute the impurities, then elute the target substance with 15L of 40% ethanol solution, collect the eluate, and concentrate to 500ml;
[0063] C. Silica gel column chromatography: Mix 500ml of the concentrated solution of step B with 600g of 100-200 mesh silica gel, dry and crush, take 10kg of 200-300 mesh silica gel, and wet-pack the column wit...
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