A method for extracting fisetin in emblica
A technology of emblica and fisetin, applied in the direction of organic chemistry and the like, can solve the problems of long time, low purity of fisetin, low efficiency and the like, and achieve the effect of few separation steps and high separation purity
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[0035] Embodiment 1, a kind of method of extracting fisetin in Emily
[0036] 1. Carry out secondary extraction with 70% ethanol aqueous solution, the material-liquid ratio of the first extraction is 1:8, the second extraction is 1:4, the extraction temperature is 65 ° C, and the extracts are combined and then concentrated and dried in vacuum;
[0037] 2. Pass the ethanol extract through a 100-mesh normal phase silica gel column, followed by petroleum ether:ethyl acetate (5:5), petroleum ether:ethyl acetate (1:9), ethyl acetate:methanol (5:5) , ethyl acetate: methanol (1:9), ethyl acetate: methanol: water (1:4:5) elution;
[0038] 3. Collect ethyl acetate:methanol (5:5) fractions, concentrate and dry, and then separate and purify by high performance liquid chromatography to obtain fisetin.
[0039] In order to qualitatively detect the obtained fisetin, HPLC-Q-TOF / MS detection technology was used for identification. HPLC-Q-TOF / MS detection conditions are as follows:
[0040]...
Example Embodiment
[0047] Embodiment 2, a kind of method for extracting fisetin in Emily, specifically comprises the steps:
[0048] 1. Carry out secondary extraction with 70% ethanol aqueous solution, the material-liquid ratio of the first extraction is 1:10, the second extraction is 1:4, the extraction temperature is 65°C, and the extracts are combined and then concentrated and dried in vacuum;
[0049] 2. Pass the ethanol extract through a 100-mesh normal phase silica gel column, followed by petroleum ether:ethyl acetate (5:5), petroleum ether:ethyl acetate (1:9), ethyl acetate:methanol (5:5) , ethyl acetate: methanol (1:9), ethyl acetate: methanol: water (1:4:5) elution;
[0050] 3. Collect ethyl acetate:methanol (5:5) fractions, concentrate and dry, and then separate and purify by high performance liquid chromatography to obtain fisetin. The chromatographic column is Diamonsil C18 (250mm×4.6mm, 5um); the column temperature: 30°C; the mobile phase is 0.2% formic acid aqueous solution-methan...
Example Embodiment
[0051] Embodiment 3, a kind of method for extracting fisetin in Emily, specifically comprises the steps:
[0052] 1. Carry out secondary extraction with 70% ethanol aqueous solution, the material-liquid ratio of the first extraction is 1:8, the second extraction is 1:6, the extraction temperature is 55 ° C, and the extracts are combined and then concentrated and dried in vacuum;
[0053] 2. Pass the ethanol extract through a 100-mesh normal phase silica gel column, followed by petroleum ether:ethyl acetate (5:5), petroleum ether:ethyl acetate (1:9), ethyl acetate:methanol (5:5) , ethyl acetate: methanol (1:9), ethyl acetate: methanol: water (1:4:5) elution;
[0054] 3. Collect ethyl acetate:methanol (5:5) fractions, concentrate and dry, and then separate and purify by high performance liquid chromatography to obtain fisetin. The chromatographic column is Diamonsil C18 (250mm×4.6mm, 5um); the column temperature: 30°C; the mobile phase is 0.2% formic acid aqueous solution-metha...
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