Marsdenia tenacissima saponins H and preparation method and application thereof
A technology of black bone vine and saponin, which is applied in the field of medicine, can solve problems such as difficult separation and purification, failure to meet the requirements of clear structure of active ingredients and controllable quality, etc.
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Embodiment 1
[0042] Take 20kg of the medicinal material of Aegypti sinensis, add 140L of 80% ethanol to extract under reflux for 3 times, each time for 1.5 hours, and combine the extract; After the column is completed, add water to elute to remove the large polar impurities, and then use 80% ethanol to elute until there is no black bone saponin H in the eluent. Drying under reduced pressure, crushing into 80 mesh powder, to obtain 440g of crude product of Aegypti japonica total saponins;
[0043] Add 2.2L of ethyl acetate to the above-mentioned crude total saponins of Acacia japonica, heat and reflux for extraction for 3 times, filter, discard the residue, combine and concentrate the extracts to 2.0L, cool, add a small amount of acacia saponin H with a purity of 99.1% The crystal was used as a seed crystal, and it was left to stand for 12 hours to crystallize, filtered, and dried to obtain 106 g of off-white crude Aeginaside H.
[0044] The above-mentioned crude product of ebonyside H was...
Embodiment 2
[0046] Take 50kg of Chinese herbal medicine, add 250L of 95% ethanol to heat and reflux for extraction 4 times, each time for 1 hour, and combine the extract; the extract is concentrated to 250L, filtered, and the filtrate is put on the D-101 macroporous adsorption resin column, and the column is completed Finally, add water to elute to remove the large polar impurities, then use 200L 95% ethanol to elute until there is no black bone saponin H in the eluent, collect the eluate, concentrate under reduced pressure at 65°C to a thick paste, and store the thick paste in Dried under reduced pressure at 65°C, crushed into 60-mesh powder, and obtained 1.4kg of crude product of total saponins of Aegypti japonica;
[0047] Add 14L of isopropyl ether to the above-mentioned crude total saponins of Aegia saponins, heat and reflux to extract twice, filter, discard the residue, combine and concentrate the extracts to 7.0L, cool, add a trace amount of crystals of Aegia saponin H with a purity...
Embodiment 3
[0050] Take 50kg of Aegypti sinensis medicinal material, add 500L of water, heat and reflux for extraction 3 times, each time for 2 hours, and combine the extract; After removing the large polar impurities by elution, use 300L 50% ethanol for elution, until there is no black bone saponin H in the eluent, collect the eluate, concentrate under reduced pressure at 75°C to a thick paste, and reduce the thick paste at 75°C. Compressed and dried, crushed into 100 mesh powder to obtain 1.6kg of crude product of Aegypti saponins;
[0051] Add 13L of isopropyl ether-ethyl acetate (1:1) to the above-mentioned crude total saponins of Acacia japonica, heat and reflux for extraction 3 times, filter, discard the residue, combine and concentrate the extracts to 6.5L, cool, add a trace amount of 99.3% of the keloidin H crystals were used as seed crystals, left to crystallize for 18 hours, filtered, and dried to obtain 252 g of white-like keloidin H crude product.
[0052] The above-mentioned...
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