A kind of separation and purification method of thonningianin A monomer
A separation and purification, monomer technology, applied in the field of separation and purification of traditional Chinese medicine, to achieve the effect of stable and reliable process, easy cost control, and high academic value
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Embodiment 1
[0052] (1) extract
[0053] Take 1 kg of Herba japonica and cut it into 0.5 cm segments, add 6 L of 70% ethanol solution, reflux extraction 3 times, 2 hours each time, filter, collect and combine the filtrates;
[0054] (2) concentrated
[0055] Recover ethanol from the collected and combined filtrate in step (1), and concentrate to a volume of 3.5L;
[0056] (3) Macroporous adsorption resin enrichment and elution
[0057] Pass the concentrated filtrate of step (2) through a macroporous adsorption resin chromatography column with a diameter of 10 cm for adsorption, first wash the resin with purified water until it is colorless, and then elute the product with 60% ethanol until the effluent Colorless, collect and combine the eluents for a total of 5 L, concentrate the eluents under reduced pressure, recover ethanol, and obtain 1.5 L of concentrated solutions;
[0058] (4) Polyamide resin enrichment and elution
[0059] Pass the concentrated solution obtained in step (3) thr...
Embodiment 2
[0073] (1) extract
[0074] Take 10 kilograms of the herba japonica medicinal material and cut it into 0.5 cm sections, add 60 L of 70% ethanol solution, reflux extraction for 3 times, each time for 2 hours, filter, collect and combine the filtrates;
[0075] (2) concentrated
[0076] Recover the ethanol from the collected and combined filtrate in step (1), and concentrate to a volume of 35 L.
[0077] (3) Macroporous adsorption resin enrichment and elution
[0078] Pass the concentrated filtrate of step (2) through a macroporous adsorption resin chromatography column with a diameter of 10 cm for adsorption, first wash the resin with purified water until it is colorless, and then elute the product with 70% ethanol until the effluent Colorless, collect and combine the eluents for a total of 5 L, concentrate the eluents under reduced pressure, recover ethanol, and obtain 14 L of concentrated solutions;
[0079] (4) Polyamide resin enrichment and elution
[0080] Pass the con...
Embodiment 3
[0094] (1) extract
[0095] Take 50 kilograms of herbal medicinal materials and cut them into 0.5 cm sections, add 300 L of 70% ethanol solution, reflux extraction for 3 times, each time for 2 hours, filter, collect and combine the filtrates;
[0096] (2) concentrated
[0097] The ethanol was recovered from the collected and combined filtrate in step (1), and concentrated to a volume of 180L.
[0098] (3) Macroporous adsorption resin enrichment and elution
[0099] Pass the concentrated filtrate of step (2) through a macroporous adsorption resin chromatography column with a diameter of 25 cm for adsorption, first wash the resin with purified water until it is colorless, and then elute with 65% ethanol until the effluent is free of 220 L of eluents were collected and combined, the eluents were concentrated under reduced pressure, ethanol was recovered, and 14 L of concentrated solutions were obtained;
[0100] (4) Polyamide resin enrichment and elution
[0101] Pass the con...
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