Separation and purification method of populus diversifolia glucoside A and B monomers
A technology for separation and purification of monomers, which is applied in the field of separation and purification of myricin A and B monomers
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Embodiment 1
[0035] A method for separating and purifying miyanin A and B monomers, comprising the steps of:
[0036] 1) Take 10 kg of dried Mi Yang leaves, add 10 times the raw material mass ratio of 65% ethanol aqueous solution (volume ratio), heat and reflux for extraction 3 times in sequence, the time is 3 hours, 2 hours, and 2 hours, combine the filtrates, and recover ethanol under reduced pressure , get extract;
[0037] 2) Dilute the extract of step 1) 50 times with distilled water, absorb it on a D101 macroporous adsorption resin chromatographic column, wash and rinse with 4 column volumes of distilled water to remove unadsorbed impurities, and then use each 4 column volumes of Elution with 10% ethanol aqueous solution and 30% ethanol aqueous solution, discard the eluent, then elute with 40% ethanol aqueous solution, concentrate the eluent to obtain the eluted fraction rich in myricin A and B;
[0038] 3) Take the 40% ethanol eluate obtained in step 2), and through silica gel colu...
Embodiment 2
[0049] A method for separating and purifying miyanin A and B monomers, comprising the steps of:
[0050] 1) Get 10kg of dried Mi Yang leaves, add 12 times of 73% ethanol aqueous solution (mass ratio of raw materials), heat and reflux and extract 3 times successively, the time is 3 hours, 2 hours, 2 hours, combine the filtrates, reclaim ethanol under reduced pressure, and obtain extract;
[0051] 2) Take the extract and suspend it in 50L of water, absorb it through a D101 macroporous adsorption resin chromatographic column, wash it with water, and then elute it with 20% and 50% ethanol to obtain 20%, 50% ethanol eluate and 50% ethanol eluate respectively. The detoxification is used as the extract of Mi Yang choke leaf which is rich in Mi Yang glycosides A and B;
[0052] 3) Take 625.0 g of the 50% ethanol eluate obtained in the above step 2), through silica gel column chromatography, use 4 column volumes of 4% dichloromethane and 96% methanol mixed solution, 10% Mixed solutio...
Embodiment 3
[0057] A method for separating and purifying miyanin A and B monomers, comprising the steps of:
[0058] 1) Get 10kg of dried Mi Yang leaves, add 15 times of 75% ethanol aqueous solution (mass ratio of raw materials), heat and reflux and extract 3 times successively, the time is 3 hours, 2 hours, 2 hours, combine the filtrates, reclaim ethanol under reduced pressure, and obtain extract;
[0059] 2) Suspend the medicinal extract of step 1) in 50L of water, absorb on a D101 macroporous adsorption resin chromatographic column, wash with water, and then elute with 20% and 50% ethanol to obtain 20% and 50% ethanol eluates respectively, The 50% ethanol eluate is used as the extract of Mi Yang choke leaf which is rich in mi Yang glucosides A and B;
[0060] 3) Take the 50% ethanol eluate obtained in the above step 2), and through silica gel column chromatography, use 4 column volumes of 5% dichloromethane and 95% methanol mixed solution, 10% dichloromethane Chloromethane and 90% me...
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