A kind of extract frb4 of She medicine twelve hours and its preparation method and application
An extract and crude extraction technology, which is applied in the direction of medical formula, drug combination, medical preparations containing active ingredients, etc., can solve the problems of quantitative control of drug quality without detection indicators, low extraction efficiency, unstable effect, etc., and achieve the goal of taking Convenience, high curative effect, and convenient detection
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[0018] A preparation method of extract FrB4, it comprises the following steps:
[0019] (1) Preparation of impregnated extract: using She medicine Twelve Hours as raw material, use polar solvent to impregnate and extract She medicine Twelve Hours to obtain the impregnated extract;
[0020] (2) Preparation of crude extract: disperse the soaked extract in water to obtain crude extract;
[0021] (3) Preparation of the total saponin extract: the crude extract is sequentially extracted with petroleum ether, ethyl acetate and n-butanol, then the n-butanol extract is combined, and the n-butanol is removed by vacuum distillation to obtain the total saponin extract;
[0022] (4) Preparation of extract FrB4: the total saponin extract is separated by microporous resin MCI column chromatography, gradient elution is carried out with methanol-water as the eluent, and the eluted fraction FrB of methanol with a mass fraction of 70% is collected. .B4, concentrated under reduced pressure and d...
Embodiment 1
[0031] Twelve hours of root purchased from Ningde Fu'an She Cottage as raw material, after the raw material is crushed into a coarse powder, take 20kg, add 150L methanol to immerse and extract, extract 3 times in total, 7 days each time, combine the extracts, recover methanol under reduced pressure, Obtained 878 g of an infusion extract impregnated with methanol.
[0032] The obtained macerated extract was dispersed in 1.2L of water to obtain a crude extract.
[0033] The crude extract was first extracted 3 times with petroleum ether, 1.2 L each time, the water phase was extracted 3 times with ethyl acetate, 1.2 L each time, and the extracted water phase was extracted 3 times with n-butanol, 1.2 L each time. L, combined n-butanol extracts, and recovered the solvent under reduced pressure to obtain 313.4 g of total saponin extract.
[0034] The obtained total saponin extract was subjected to microporous resin MCI column chromatography, and water, 20% methanol, 50% methanol, 70...
Embodiment 2
[0037] Twelve hours root purchased from Ningde Fu'an She Cottage as raw material, the raw material was crushed into coarse powder, 5kg was taken, added 35L 80% ethanol aqueous solution for immersion extraction, extracted 3 times in total, 7 days each time, combined the extracts, and decompressed The solvent was recovered to obtain 222 g of an infusion extract impregnated with an ethanol aqueous solution.
[0038] The obtained macerated extract was dispersed in 0.3 L of water to obtain a crude extract.
[0039] The crude extract was extracted 3 times with petroleum ether, 0.3 L each time, the water phase was extracted 3 times with ethyl acetate, 0.3 L each time, and the extracted water phase was extracted 3 times with n-butanol, 0.3 L each time. L, combined n-butanol extracts, and recovered the solvent under reduced pressure to obtain 78.3 g of total saponin extract.
[0040] The obtained total saponin extract was subjected to microporous resin MCI column chromatography, and w...
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