Method for preparing kaempferol-3-O-2'',6''-dirhamnosylglucoside
A technology of -3-O-2 and rhamnosyl, which is applied in the field of medicine, can solve the problems of large organic solvent consumption, cumbersome operation steps, time-consuming and labor-intensive, etc., and achieve a high degree of instrument automation, abundant resources, and convenient operation Effect
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Embodiment 1
[0041] Weigh 500g of Ginkgo biloba extract, dissolve it in 1L of 50% methanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 500mg / mL, pass it through a 0.45μm microporous membrane, and prepare it by one-dimensional liquid chromatography. The one-dimensional liquid chromatography adopts XUnion C18, the mobile phase adopts acetonitrile as the organic phase, water as the aqueous phase, and the gradient elution method: the concentration of the organic phase increases from 10% to 25% in 20 minutes. Adopt DAD ultraviolet detector 360nm to select the absorption wavelength, the preparation temperature is room temperature, the injection volume is 500μL / needle, the mobile phase flow rate is 90mL / min, the fractions collected for 9-12 minutes are concentrated to dryness by rotary evaporation, which is one-dimensional preparation Kaempferol-3-O-2",6"-dirhamnosyl glucoside crude product. Dissolve the crude kaempferol-3-O-2”, 6”-dirhamnosyl glucoside in 40...
Embodiment 2
[0043] Weigh 2000g of Ginkgo biloba extract, dissolve it in 2L of 25% methanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 1000mg / mL, pass it through a 0.45μm microporous membrane, and perform one-dimensional liquid chromatography. The one-dimensional liquid chromatography adopts XUnion C8, the mobile phase adopts methanol as the organic phase, water as the aqueous phase, the concentration of the organic phase is 65% isocratic, the absorption wavelength is selected by DAD ultraviolet detector at 360nm, the preparation temperature is 40°C, and the injection volume 200μL / needle, mobile phase flow rate 60mL / min, collect fractions for 5-7 minutes, and concentrate to dryness by rotary evaporation to prepare kaempferol-3-O-2”, 6”-dirhamnosyl for one-dimensional Crude glucoside. Dissolve the crude kaempferol-3-O-2”, 6”-dirhamnosyl glucoside in 50% methanol-water solution to a concentration of 20 mg / mL, filter through a microporous membrane, and p...
Embodiment 3
[0045] Weigh 100g of Ginkgo biloba extract, dissolve it in 10L of 75% methanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 10mg / mL, pass it through a 0.45μm microporous membrane, and prepare it by one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts Click OEG, the mobile phase adopts methanol containing 0.1% formic acid as the organic phase, and water containing 0.1% formic acid as the aqueous phase, and adopts 5% organic equivalence method for elution. The DAD ultraviolet detector is used to select the absorption wavelength at 360nm, the preparation temperature is 30°C, the injection volume is 3000μL / needle, the flow rate of the mobile phase is 120mL / min, and the fractions collected for 22-25 minutes are concentrated to dryness by rotary evaporation. Preparation of crude kaempferol-3-O-2",6"-dirhamnosyl glucoside. Dissolve the crude kaempferol-3-O-2”, 6”-dirhamnosyl glucoside in 60% methanol-water solution t...
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