Method for separating high-purity oleuropein by combining macroporous resin and preparative liquid chromatography
A technology for preparing liquid phase and oleuropein, which is applied in the preparation of sugar derivatives, chemical instruments and methods, organic chemistry, etc., can solve the problems of high solvent consumption, cumbersome steps, low yield and the like, and achieves low separation cost and low preparation cost. The effect of process safety
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Embodiment 1
[0019] Take 1kg of olive leaves, add 12 liters of 60% ethanol, reflux for 2 hours, pour out the extract, then add 10 times the amount of 60% ethanol for the second extraction, combine the two extracts, and then recover the solvent under reduced pressure until there is no alcohol smell in the solution. Add distilled water to the concentrated extract to make the density equivalent to 0.2g / mL of the original medicinal material. The concentrated extract was passed through a macroporous resin column to enrich oleuropein at a flow rate of 8 BV / h. After the adsorption was completed, it was first eluted with distilled water, and the distilled water eluate was discarded. Then elute with 70% ethanol at a flow rate of 10BV / h, collect the 70% ethanol eluate, and recover the solvent under reduced pressure. Dissolve the 70% ethanol eluted part of the macroporous resin in methanol, and separate by preparative liquid chromatography, using a 20×250mm separation column, with a sample volume of...
Embodiment 2
[0021] Take 1 kg of olive leaves, add 12 liters of water, reflux for 2 hours, pour out the extract, then add 10 times the amount of water for the second extraction, combine the two extracts, and recover the solvent under reduced pressure until the density of the extract is equivalent to The original medicinal material 0.15g / mL. The concentrated extract was passed through a macroporous resin column for oleuropein enrichment at a flow rate of 10BV / h. After the adsorption was completed, the impurities were first washed with distilled water, and the distilled water eluate was discarded. Then elute with 60% ethanol at a flow rate of 10BV / h, collect the 60% ethanol eluate, and recover the solvent under reduced pressure. Dissolve the eluted part of the macroporous resin with 60% ethanol in methanol, and separate by preparative liquid chromatography, using a 50×650mm preparative column, with a sample volume of 150mg, methanol-water gradient elution, a flow rate of 30mL / min, and an onl...
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