Forsythoside A and preparation method thereof
A technology for forsythiaside and forsythia, which is applied in the field of preparation of extracting forsythiaside A, achieves the effects of low production cost, good stability and strong practicability
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Embodiment 1
[0027] Take 50kg of forsythia medicinal material, add 350L water to heat and reflux to extract twice, each time for 2 hours, combine the extracts, filter, and cool; adjust the pH value of the filtrate to 9.0 with NaOH, add 350L ethyl acetate to extract three times, the upper layer Concentrate the extract at 65°C to a thick paste, weigh 5.4kg; add 100kg of purified water to the thick paste, heat to dissolve at 40°C, and filter; put the filtrate on a HPD-100 macroporous adsorption resin column, after the column is completed, add water After fully eluting to remove the large polar impurities, use 150L of ethanol with a concentration of 50% to elute until there is no forsythiaside A in the eluent, collect the eluate, concentrate under reduced pressure to a thick paste; add to the thick paste 2 L of methanol was heated to dissolve, cooled, and a small amount of forsythiaside A crystals with a purity of 90.2% were added as seed crystals, stirred, allowed to stand for 12 hours to crys...
Embodiment 2
[0031]Take 50kg of Forsythia medicinal material, add 350L of ethanol, heat and extract once at 75°C, extract for 2 hours, collect the extract, filter, and cool; adjust the pH value of the filtrate to 11.0 with NaOH, add 350L of n-butanol to extract twice , the upper layer extract was concentrated at 85°C to a thick paste, weighing 5.2kg; adding 100kg of purified water to the thick paste, heated to dissolve at 40°C, and filtered; the filtrate was placed on a HPD-400 macroporous adsorption resin column, and after the , after adding water to fully elute and remove the large polar impurities, use 150L of ethanol with a concentration of 20% to elute until there is no forsythiaside A in the eluent, collect the eluate, concentrate under reduced pressure to a thick paste; Add 2L of acetone, heat to dissolve, cool, add a small amount of forsythiaside A crystals with a purity of 90.5% as seed crystals, stir, let stand for crystallization for 10 h, filter, and dry to obtain 256 g of forsy...
Embodiment 3
[0034] Take 100kg of forsythia medicinal material, add 700L of water to heat and reflux for extraction once, extract for 2 hours, collect the extract, filter, and cool; adjust the pH value of the filtrate to 8.0 with sodium carbonate, add 700L of ethyl acetate to extract three times, and extract the upper layer Concentrate the liquid at 65°C to a thick paste, weighing 10.7kg; add 200kg of purified water to the thick paste, heat to dissolve at 40°C, and filter; put the filtrate on the HPD-500 macroporous adsorption resin column, after the column is completed, add water fully After removing the large polar impurities by eluting, use 300L of ethanol with a concentration of 35% to elute until there is no forsythiaside A in the eluent, collect the eluate, concentrate under reduced pressure to a thick paste; add ethanol to the thick paste 4L, heated to dissolve, cooled, added a small amount of forsythiaside A crystal with a purity of 91.4% as a seed crystal, stirred, allowed to stand...
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