Method for separating and extracting apigenin, acacetin-7-O-beta-D-glucoside and apigenin-7-O-beta-D-glucoside from dendranthema indicum
A technology of Shennong chrysanthemum and glucoside, which is applied in the field of apigenin-7-O-β-D-glucoside, can solve the problems of large environmental pollution, large consumption of reagents, and low product purity, and achieve low environmental pollution and consumption The effect of less organic reagents and high product purity
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Embodiment 1
[0039] Shennong chrysanthemum dried flowers, crushed through a 20-mesh sieve, took 3 kg, soaked in 70% ethanol for 12 hours, then extracted by percolation, collected the percolation liquid to 10 times the amount of the original medicinal material, recovered the solvent to obtain an extract, and distilled the extract with an appropriate amount of distilled water. paste suspension, sequentially extracted with petroleum ether, chloroform, and ethyl acetate to obtain three extraction parts, and then carry out normal pressure and reduced pressure 200-300 mesh silica gel column chromatography on the ethyl acetate part, and use petroleum ether-ethyl acetate, The chloroform-methanol system was repeatedly eluted, and the fractions were collected by TLC as the detection method, separated by semi-preparative high-performance liquid chromatography, concentrated, dried and recrystallized. Chromatographic conditions: mobile phase: methanol:water (63:37), flow rate: 2.5mL / min, column temperat...
Embodiment 2
[0045] Shennong chrysanthemum dried flowers, crushed through a 20-mesh sieve, took 3 kg, soaked in 70% ethanol for 12 hours, then extracted by percolation, collected the percolation liquid to 10 times the amount of the original medicinal material, recovered the solvent to obtain an extract, and distilled the extract with an appropriate amount of distilled water. Paste suspension, sequentially extracted with petroleum ether, chloroform, ethyl acetate to obtain three extraction parts, then carry out normal pressure and reduced pressure silica gel column chromatography on the ethyl acetate part, and use petroleum ether-ethyl acetate, chloroform-methanol system Repeated elution, using TLC as detection means, collected fractions, separated by semi-preparative high performance liquid chromatography, concentrated, dried and recrystallized. Chromatographic conditions: mobile phase: methanol:water (63:37), flow rate: 2.5mL / min, column temperature: 25°C, injection volume: 0.5mL.
[0046...
Embodiment 3
[0051] Shennong chrysanthemum dried flowers, crushed through a 20-mesh sieve, took 3 kg, soaked in 70% ethanol for 12 hours, then extracted by percolation, collected the percolation liquid to 10 times the amount of the original medicinal material, recovered the solvent to obtain an extract, and distilled the extract with an appropriate amount of distilled water. paste suspension, sequentially extracted with petroleum ether, chloroform, and ethyl acetate to obtain three extraction parts, and then carry out normal pressure and reduced pressure 200-300 mesh silica gel column chromatography on the ethyl acetate part, and use petroleum ether-ethyl acetate, The chloroform-methanol system was repeatedly eluted, and the fractions were collected by TLC as the detection means, separated by semi-preparative high performance liquid chromatography, the fractions were collected, concentrated, dried and recrystallized. Chromatographic conditions: mobile phase: methanol:water (63:37), flow rat...
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