Method for preparing quercetin-3-o-glucoside from ginkgo leaf extract
A technology of glucoside and extract, which is applied in the field of compound preparation, can solve problems such as less strict and standardized effects, different drug effects, and restrictions on drug quality standards, and achieve improved drug quality standards, simple preparation methods, and convenient separation operations Effect
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Embodiment 1
[0027] Weigh 10 g of Ginkgo biloba extract, dissolve it in 50 mL of 40% ethanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 200 mg / mL, pass it through a 0.45 μm microporous membrane, and perform one-dimensional liquid chromatography separation. One-dimensional liquid chromatography adopts silica gel as the matrix of hydrophilic chromatographic filler 50 × 250mm, 10 μm (Huapu New Innovation Technology Co., Ltd.), and the mobile phase adopts methanol containing 0.1% volume concentration of formic acid as the organic phase, containing 0.1% volume The water with formic acid concentration is the water phase, and the gradient elution method: the concentration of the organic phase decreases from 95% to 90% in step gradient in 0-15min. Use 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 col...
Embodiment 2
[0035] Weigh 1 g of Ginkgo biloba extract, dissolve it in 100 mL of ethanol-water solution with a volume concentration of 80%, and obtain a Ginkgo biloba extract solution with a concentration of 10 mg / mL, pass it through a 0.45 μm microporous membrane, and perform one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts silica gel-based hydrophilic chromatographic packing (50×250mm, 10μm, Huapu Innovation Technology Co., Ltd.), the mobile phase uses ethanol as the organic phase, water as the aqueous phase, and the concentration of the organic phase is 90 % isocratic, using a DAD ultraviolet detector at 360nm to select the absorption wavelength, the preparation temperature is 40°C, the injection volume is 200μL / needle, the flow rate of the mobile phase is 60mL / min, the fractions collected for 15-20 minutes are concentrated to dryness by rotary evaporation , for the one-dimensional preparation of crude quercetin-3-O-glucoside. Dissolve the crude querce...
Embodiment 3
[0038] Weigh 100g of Ginkgo biloba extract, dissolve it in 200mL of 50% ethanol-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. One-dimensional liquid chromatography adopts a hydrophilic chromatographic packing (50×250mm, 10 μ, Huapu Innovation Technology Co., Ltd.) based on silica gel, and the mobile phase adopts ethanol (containing 0.1% formic acid) as the organic phase, water (containing 0.1% % formic acid) is the aqueous phase, and is eluted by 95% organic equivalence. 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, the fractions collected for 15-20 minutes are concentrated to dryness by rotary evaporation, and the one-dimensional Prepare crude quercetin-3-O-glucoside. D...
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Abstract
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