Method for preparing stibene glucoside from fleece-flower root
A technology of stilbene glycosides and Polygonum multiflorum, which is applied in the field of natural medicinal chemistry, can solve the problems of complex stilbene glycosides methods and unsuitability for industrial production, and achieve the effect of high product yield and simple operation
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Embodiment 1
[0015] Take 20kg of fresh Radix Polygoni Multiflori, clean it, chop it into a colloid mill to make pulp, and add appropriate amount of water to get 35kg of slurry, add 70L of 95% edible alcohol, stir for 2 hours, centrifuge, and add hollow cellulose sodium with a molecular weight cut-off of 800 to the centrifuge. Membrane filtration, add an appropriate amount of 70% ethanol for dialysis, collect the permeate, and then recover ethanol under reduced pressure. After the concentrated solution is cooled to room temperature, add 2 times the volume of ethyl acetate for full extraction, collect the ethyl acetate layer, and pass through 160 mesh Add 1 / 7 volume of petroleum ether and stir thoroughly, refrigerate and crystallize for 36 hours, filter out the crystals, dissolve in methanol, add an appropriate amount of ether to refrigerate and crystallize twice, the crystallized stilbene glycosides 71g, Through high-phase liquid phase detection, the content is 95.3%.
Embodiment 2
[0017] Take 20kg of fresh Polygonum multiflorum, clean it, chop it into a colloid mill, and add appropriate amount of water to get 35kg of slurry, add 70L of 95% edible alcohol, stir for 3 hours, centrifuge, and add hollow cellulose sodium with a molecular weight cut-off of 500 to the centrifuge. Membrane filtration, add an appropriate amount of 60% ethanol for dialysis, collect the permeate, and then recover ethanol under reduced pressure. After the concentrated solution is cooled to room temperature, add 2 times the volume of ethyl acetate for full extraction, collect the ethyl acetate layer, pass through 200 mesh Add 1 / 5 of the volume of petroleum ether and stir thoroughly, refrigerate and crystallize for 24 hours, filter out the crystals, dissolve in methanol, add an appropriate amount of ether to refrigerate and crystallize twice, and crystallize stilbene glycosides 56g, Through high-phase liquid phase detection, the content is 97.8%.
Embodiment 3
[0019] Take 20kg of fresh Radix Polygoni Multiflori, clean it, chop it into a colloid mill to make pulp, and add appropriate amount of water to get 35kg of slurry, add 70L of 95% edible alcohol, stir for 3 hours, centrifuge, and add hollow cellulose sodium with a molecular weight cut-off of 700 to the centrifuge Membrane filtration, add an appropriate amount of 50% ethanol for dialysis, collect the permeate, and then recover ethanol under reduced pressure. After the concentrated solution is cooled to room temperature, add 2 times the volume of ethyl acetate for full extraction, collect the ethyl acetate layer, and pass through 120 mesh Add 1 / 5 volume of petroleum ether and stir thoroughly, refrigerate and crystallize for 24 hours, filter out the crystals, dissolve in methanol, add an appropriate amount of ether to refrigerate and crystallize twice, the crystallized stilbene glycosides 63g, Through high-phase liquid phase detection, the content is 99.8%.
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