A kind of separation and purification method of liquiritin
A technology for separation and purification, liquiritin, applied in the field of separation and purification, can solve the problems of inability to large-scale production, high production cost, low added value, etc., and achieve the effects of improving waste utilization rate, high utilization rate and short cycle.
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Embodiment 1
[0029] (1) Enrichment: Weigh the mother liquor cream in a beaker, add 40% methanol, and under the condition that the mass ratio of solid to liquid is 1:5, stir and extract for 1 hour, take the filtrate and evaporate to dryness, add No. 2 extract (dichloromethane: Methanol=10:1), the mass ratio of solid to liquid is 1:15, stirring and extracting for 1 hour, taking the filtrate and adding 5 times of ethyl acetate to precipitate, filtering to obtain a solid, and then dissolving it with ethanol to obtain a liquiritin enriched solution;
[0030] (2) Purification: add silica gel to the liquiritin enriched solution obtained in step (1) to obtain mixed sample silica gel. Add blank silica gel to the chromatographic column, add the above-mentioned mixed sample silica gel, elute with dichloromethane-methanol 20:1, detect and collect components by TLC until the liquiritin is completely collected. After concentration, add methanol, stir, crystallize, filter, wash with methanol to obtain of...
Embodiment 2
[0032] (1) Enrichment: Weigh the mother liquor cream in a beaker, add 75% ethanol, under the condition that the mass ratio of solid to liquid is 1:10, stir and extract for 2 hours, take the filtrate and evaporate to dryness, add No. 2 extract (ethyl acetate: Ethanol=5:1), the mass ratio of solid to liquid is 1:10, stirring and extracting for 2 hours, taking the filtrate and adding 15 times of acetone to precipitate, filtering to obtain a solid, and then dissolving it with ethyl acetate to obtain a liquiritin enriched solution;
[0033] (2) Purification: add silica gel to the liquiritin enriched solution obtained in step (1) to obtain mixed sample silica gel. Add blank silica gel to the chromatographic column, add the above-mentioned mixed sample silica gel, elute with dichloromethane-ethanol 10:1, collect components for TLC detection, until the liquiritin is completely collected. After concentration, add ethyl acetate, stir, crystallize, filter, and wash with ethyl acetate to ...
Embodiment 3
[0035] (1) Enrichment: Weigh the mother liquor cream in a beaker, add 95% methanol, and under the condition that the mass ratio of solid to liquid is 1:15, stir and extract for 4 hours, take the filtrate and evaporate to dryness, add No. 2 extract (ethyl acetate: Methanol=2:1), the mass ratio of solid to liquid is 1:5, stirring and extracting for 4h, taking the filtrate and adding 20 times of dichloromethane to precipitate, filtering to obtain a solid, and then dissolving it with ethyl acetate and methanol (volume ratio is 3:1) Obtain a liquiritin enriched solution;
[0036](2) Purification: add silica gel to the liquiritin enriched solution obtained in step (1) to obtain mixed sample silica gel. Add blank silica gel to the chromatographic column, add the above-mentioned mixed silica gel, elute with ethyl acetate-ethanol 5:1, collect components for TLC detection, until the liquiritin is completely collected. After concentration, add ethanol, stir, crystallize, filter, and was...
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