Novel technique for preparing schizandrol A and schizandrol B
A technology of schisandra alcohol A and schisandra alcohol B, which is applied in the field of medicine, can solve problems such as quality decline, low purity, and price rise, and achieve the effects of alleviating the shortage, simple process, and convenient operation
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Embodiment 1
[0018] 5.2 kg of schisandra leaves were crushed, added with 80% acetone and extracted under reflux for 3 times, each time for 2 hours, filtered, and the combined filtrates were concentrated under reduced pressure to 3.5 L of medicinal solution with a density of 0.982. An equal volume of petroleum ether was added for extraction 6 times, and the petroleum ether layer was concentrated to dryness under reduced pressure to obtain 150 g of the extract. Gradient elution of the mixed solution, roughly divided into 6 sections, TLC detection, collecting the second section rich in schisandra alcohol B, and then performing a second silica gel column chromatography, using cyclohexane-ethyl acetate (10:1- 1:1) mixed solution with a volume ratio of 1:1) was eluted, detected by TLC, and the part rich in Schisandrin B was collected, and recrystallized repeatedly with methanol-water, which was 140 mg of pure Schisandrin B, and its purity could reach 98.9%. Collect the 5th section rich in schisa...
Embodiment 2
[0020] 5.2 kg of schisandra leaves were crushed, added with 75% ethanol, heated and refluxed for 3 times, 2 hours each time, filtered, and the combined filtrate was concentrated under reduced pressure to 4.5 L of medicinal solution with a density of 0.982. An equal volume of petroleum ether was added for extraction 6 times, and the petroleum ether layer was concentrated to dryness under reduced pressure to obtain 203 g of the extract. The extract was subjected to silica gel column chromatography, and the volume ratio of dichloromethane-methanol (300:0.5-300:5) was Gradient elution of the mixed solution, roughly divided into 6 sections, TLC detection, collecting the second section rich in schisandra alcohol B, and then performing a second silica gel column chromatography, using cyclohexane-ethyl acetate (10:1- 1:1) mixed solution with a volume ratio of 1:1) was eluted, TLC was detected, and the part rich in schisandra alcohol B was collected, petroleum ether-methanol-water was r...
Embodiment 3
[0022] 5.2 kg of schisandra leaves were crushed, added with 75% ethanol, heated and refluxed for 3 times, 2 hours each time, filtered, and the combined filtrate was concentrated under reduced pressure to 4.5 L of medicinal solution with a density of 0.982. Adsorbed on HPD 100 macroporous resin on the medicinal solution, and eluted with water, 30%, and 40-90% ethanol in sequence, collected 40-90% ethanol eluate, recovered ethanol and evaporated to dryness in a water bath to obtain 160.8 g of eluate, and The eluate was subjected to silica gel column chromatography, eluted with a gradient mixture of dichloromethane-methanol (300:0.5-300:5) volume ratio, roughly divided into 6 sections, and detected by TLC. For the second section, perform silica gel column chromatography for the second time, eluting with a mixture of cyclohexane-ethyl acetate (10:1-1:1) volume ratio, TLC detection, and collecting the part rich in schisandra alcohol B , Petroleum ether-methanol-water repeated recry...
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