Process for preparing chlorogenic acid from honeysuckle
A technology of chlorogenic acid and honeysuckle, which is applied in the separation/purification of carboxylate, organic chemistry and other directions, can solve the problems of inability to carry out large-scale industrial production, inability to declare national first-class new drugs, etc., and achieve the effect of increasing the extraction cost.
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Embodiment 1
[0021] 500g of honeysuckle is packed into the extractor, water with 5 times the weight of honeysuckle is added, and heating is extracted three times, each time being 3.5 hours. Medicinal solution is filtered and decompressed to recover solvent, and medicinal ethanol is added for precipitation, so that the final alcohol content reaches 75%, let stand overnight, filter or centrifuge, discard the precipitate, concentrate the filtrate to no ethanol, add water to make every milliliter contain 2g of crude drug. 0.5g, let it stand overnight, filter or centrifuge to discard the precipitate, and put the filtrate on a macroporous resin column. Elute with water and 10% ethanol, check by thin layer chromatography, collect the components containing chlorogenic acid, put it on a polyamide column, elute with water and 10% ethanol, collect the components containing chlorogenic acid, and collect the components containing chlorogenic acid The acid eluate was concentrated to 2 g crude drug per m...
Embodiment 2
[0023] Put 250g of honeysuckle into the extractor, add ethanol with 5 times the weight of the crude drug, heat and reflux to extract three times for 3 hours, filter, recover the solvent from the filtrate, add water to make the crude drug content per ml 0.5g, let stand overnight, filter or centrifuge Remove precipitation, put the filtrate on a macroporous resin column, elute with water and 10% ethanol, collect the components containing chlorogenic acid, put it on a polyamide column, elute with water and 10% ethanol, collect the components containing chlorogenic acid, concentrate To contain 2g crude drug per milliliter, extract with ethyl acetate. The solvent was recovered to obtain a concentrate, which was dried to obtain 4 g of fine chlorogenic acid with a content greater than 95%.
Embodiment 3
[0025] Put 1250g honeysuckle into the extractor, add 5 times the amount of 30% ethanol, heat and extract three times for 2.5 hours, filter, recover the solvent from the filtrate, add medicinal ethanol to make the alcohol content 50%, let it stand overnight, filter or centrifuge and discard Remove precipitation, put the filtrate on a macroporous resin column, elute with water and 10% ethanol, collect the components containing chlorogenic acid, put it on a polyamide column, elute with water and 10% ethanol, collect the components containing chlorogenic acid, concentrate to the extract form, dried under reduced pressure, applied to a silica gel chromatographic column, eluted with ethyl acetate-ethanol, recovered the eluent, and obtained chlorogenic acid crystals with a content greater than 98%.
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