Method for preparing high-purity rutin via two-dimensional liquid chromatography-mass spectrometry combined technology
A two-dimensional liquid chromatography and two-dimensional preparation technology, which is applied in the field of high-purity rutin preparation by two-dimensional liquid chromatography-mass spectrometry, can solve the problems of insufficient medicinal material resources, low utilization rate of medicinal materials, and doping of hydrolyzed products. Achieve the effects of wide sources of medicinal materials, high purity of rutin, and long application time
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Embodiment 1
[0047] Weigh 10 g of Ginkgo biloba extract, dissolve it in 50 mL of 50% methanol-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 prepare it by one-dimensional liquid chromatography. The one-dimensional liquid chromatography adopts XUnion C18, the mobile phase adopts acetonitrile (containing 0.1% formic acid) as the organic phase, water (containing 0.1% formic acid) as the aqueous phase, and the gradient elution method: the concentration of the organic phase increases from 10% to 25%. DAD ultraviolet detector is used to select the absorption wavelength at 360nm, the preparation temperature is room temperature, the injection volume is 500μL / needle, the mobile phase flow rate is 90mL / min, the fractions collected for 12-14 minutes are concentrated to dryness by rotary evaporation, which is one-dimensional preparation Crude rutin. Dissolve crude rutin in 40% methanol-water solution wit...
Embodiment 2
[0049] Weigh 10 g of Ginkgo biloba extract, dissolve it in 100 mL of 25% methanol-water solution to 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 preparation. The one-dimensional liquid chromatography adopts XTerra, the mobile phase adopts methanol as the organic phase, water as the aqueous phase, the organic phase concentration is 65% isocratic, the DAD ultraviolet detector is used to select the absorption wavelength at 360nm, the preparation temperature is 40°C, and the injection volume is 200 μL / needle, the flow rate of the mobile phase is 60mL / min, the fractions collected for 5-7 minutes are concentrated to dryness by rotary evaporation, and the crude rutin is prepared as one-dimensional. Dissolve crude rutin in 50% methanol-water solution with a concentration of 10 mg / mL, filter through a microporous membrane, and prepare for two-dimensional liquid ...
Embodiment 3
[0051] Weigh 10 g of Ginkgo biloba extract, dissolve it in 20 mL of 75% methanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 500 mg / mL, pass it through a 0.45 μm microporous membrane, and perform one-dimensional liquid chromatography preparation. One-dimensional liquid chromatography adopts Click OEG, the mobile phase uses methanol (containing 0.1% formic acid) as the organic phase, 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 25-30 minutes are concentrated to dryness by rotary evaporation, which is one-dimensional Preparation of crude rutin. Dissolve crude rutin in 60% methanol-water solution with a concentration of 80 mg / mL, filter throu...
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