Method for preparing forsythiaside A
A forsythiaside and drying technology, applied in the field of preparation of forsythiaside A, can solve the problems of difficult regeneration and reuse of separation materials, expensive separation materials, low efficiency and the like, and achieves easy elution and regeneration, simple refining process, simple craftsmanship
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Embodiment 1
[0021] Take 400g of dry forsythia shell, extract twice with 8Kg 50% ethanol solution, extraction temperature is 60°C, extraction time is 60min, combine the extracts, filter, the filtrate is concentrated under reduced pressure at 60°C to a water extract with a specific gravity of 1.08; water The extract was separated on a polyamide column (diameter-to-height ratio: 1:15), and the loading volume was 1:5. First rinse with deionized water until the effluent is brown-yellow, then rinse with 30% ethanol for 3 times the column volume, collect the 30% ethanol eluent, concentrate under reduced pressure to a specific gravity of 1.08 to obtain a preliminary separation concentrate; preliminary separation The concentrated solution was refined on an MDS column (diameter-to-height ratio: 1:15), first rinsed with deionized water until the eluate was pale yellow, then rinsed with 20% ethanol for 4 column volumes, and collected 20% ethanol. lotion. Thin-layer chromatography detection (developi...
Embodiment 2
[0023] Take 400g of dried forsythia shells, extract twice with 15Kg deionized water, extraction temperature is 80°C, extraction time is 45min, the extracts are combined, filtered, and the filtrate is concentrated under reduced pressure at 60°C to a water extract with a specific gravity of about 1.05; the water extract Separation on a D101 column (diameter-to-height ratio: 1:15), with a loading volume of 1:4. First rinse with deionized water until the effluent is brown-yellow, then use 20% ethanol to rinse for 4 times the column volume, collect the 20% ethanol eluate, concentrate under reduced pressure to a specific gravity of 1.05 to obtain a preliminary separation concentrate; The concentrated solution was refined on an MDS column (diameter-to-height ratio: 1:12), rinsed with deionized water until the eluate was pale yellow, then rinsed with 30% ethanol for 4 column volumes, and collected 30% ethanol. lotion. Thin-layer chromatography detection (developing solvent is methyl ...
Embodiment 3
[0025] Take 1Kg of dry forsythia shell, extract twice with 35Kg 40% ethanol solution, extraction temperature is 80°C, extraction time is 80min, combine the extracts, filter, the filtrate is concentrated under reduced pressure at 60°C to a water extract with a specific gravity of 1.10; water The extract was separated on an AB-8 column (aspect ratio of 1:15), and the loading volume was 1:4. First rinse with deionized water until the effluent is brown-yellow, then use 30% ethanol to rinse for 4 times the column volume, collect the 30% ethanol eluate, concentrate under reduced pressure to a specific gravity of 1.06 to obtain a preliminary separation concentrate; The concentrated solution was refined on an MDS column (diameter-to-height ratio: 1:12), rinsed with deionized water until the eluate was pale yellow, then rinsed with 30% ethanol for 4 column volumes, and collected 30% ethanol. lotion. Thin-layer chromatography detection (developing solvent is methyl ethyl ketone: ethyl ...
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