Joint preparation method for euscaphic acid and tormentic acid
A technology for the joint preparation of Potentate acid, applied in steroids, organic chemistry, etc., can solve the problems of no simultaneous preparation of two substances, no patent reports, etc., and achieve high recovery rate and high throughput Large, simple effect of solvent system
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Embodiment 1
[0025] Take 1 kg of Gugongguo medicinal material, grind it, add 10L of 40% ethanol solution to heat reflux extraction twice, combine the extracts, concentrate to low alcohol, and absorb on macroporous resin, first use 2BV of water and 3BV of 30% ethanol aqueous solution to elute sugar and other impurities , and then eluted with 5BV65% ethanol aqueous solution, and the eluent was concentrated under reduced pressure to dryness to obtain the total triterpene extract. Reversed-phase preparation of high performance liquid phase for further separation and purification, using C-18 bonded silica gel as the stationary phase, acetonitrile-0.3% trifluoroacetic acid (30:70) solution as the mobile phase, the flow rate was set at 30ml / min, and UV detection was set The wave length of the instrument is 210nm, and the fractions of rosinic acid and palindromic acid are collected in sections, and the reagent is recovered to a small volume, placed for crystallization, and the crystallization is fi...
Embodiment 2
[0027] Take 1Kg of Gugongguo medicinal material, pulverize it, add 5L of 70% ethanol for ultrasonic extraction three times, combine the extracts, concentrate to low alcohol, absorb on macroporous resin, first use 2BV of water and 3BV of 30% methanol aqueous solution to elute sugar and other impurities, then Use 5BV70% methanol aqueous solution for elution, and the eluate is concentrated under reduced pressure to dryness to obtain the total triterpene extract. The obtained total triterpene is dissolved in a small amount of methanol, diluted with mobile phase, filtered through a 0.22 μm filter membrane, and then reversed-phase Prepare high performance liquid phase for further separation and purification, use C-18 bonded silica gel as the stationary phase, acetonitrile-0.3% trifluoroacetic acid (32:68) solution as the mobile phase, set the flow rate to 30ml / min, and set the wavelength of the UV detector 210nm, collect the rosic acid fraction and the potentinic acid fraction in sec...
Embodiment 3
[0029] Take 5Kg of Gugongguo medicinal material, crush it, add 40L50% ethanol to ultrasonically extract twice, combine the extracts, concentrate to low alcohol, and adsorb on macroporous resin, first use 2BV water and 3BV25% propanol aqueous solution to elute sugar and other impurities, Then eluted with 5BV70% propanol aqueous solution, and the eluate was concentrated under reduced pressure to dryness to obtain the total triterpene extract. The total triterpene was dissolved in a small amount of methanol, diluted with mobile phase, filtered through a 0.22 μm filter membrane, and then used Reversed-phase preparation of high performance liquid phase for further separation and purification, with C-18 bonded silica gel as the stationary phase, acetonitrile-0.3% trifluoroacetic acid (35:65) solution as the mobile phase, the flow rate was set at 30ml / min, and UV detection was set The wave length of the instrument is 210nm, and the fractions of rosinic acid and palindromic acid are co...
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