Preparation method of oleuropein
A technology of oleuropein and an entraining agent, applied in the field of preparation of oleuropein, can solve the problems such as the industrialized production process disclosure of no extraction of oleuropein, and achieve the effects of being beneficial to large-scale production operations, low in energy consumption, and low in pollution
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Embodiment 1
[0018] Get 10Kg of dried jasmine flowers and add to CO 2 In the supercritical extractor, ethanol is used as the entrainer, and the volume percentage of the entrainer in the total extraction solvent is 4%, the extraction pressure is 50MPa, the temperature is 30°C, and the CO 2 The flow rate is 10L / min, the extraction time is 100min, the extract is obtained, dissolved in water, extracted once with an equal amount of ethyl acetate, the water layer is taken, adsorbed by an AB-8 macroporous adsorption resin column, eluted with 35% ethanol, and collected for 3 The eluate was twice the volume of the column, the ethanol was recovered under reduced pressure and concentrated, refrigerated for 12 hours, filtered, the filter residue was taken, recrystallized by adding absolute ethanol, separated and crystallized, washed and dried to obtain 253.3g of oleuropein, which was detected by HPLC , with a purity of 98.2%.
Embodiment 2
[0020] Get 10Kg of dried jasmine flowers and add to CO 2 In the supercritical extractor, ethanol is used as the entrainer, and the volume percentage of the entrainer in the total extraction solvent is 6%, the extraction pressure is 70MPa, the temperature is 70°C, and the CO 2 The flow rate was 30L / min, and the extraction time was 250min. The extract was obtained, dissolved in water, extracted three times with an equal amount of ethyl acetate, and the water layer was taken, adsorbed by an AB-8 macroporous adsorption resin column, eluted with 35% ethanol, and collected 8 The eluate was twice the volume of the column, the ethanol was recovered under reduced pressure and concentrated, refrigerated for 36 hours, filtered, the filter residue was taken, recrystallized by adding absolute ethanol, separated and crystallized, washed and dried to obtain 389.0 g of oleuropein, which was detected by HPLC , with a purity of 97.3%.
Embodiment 3
[0022] Get 10Kg of dried jasmine flowers and add to CO 2 In the supercritical extractor, ethanol is used as the entrainer, and the volume percentage of the entrainer in the total extraction solvent is 5%, the extraction pressure is 60MPa, the temperature is 50°C, and the CO 2 The flow rate is 20L / min, and the extraction time is 180min. The extract is obtained, dissolved in water, extracted 1-3 times with an equal amount of ethyl acetate, and the water layer is taken, adsorbed by an AB-8 macroporous adsorption resin column, and eluted with 35% ethanol. Collect the eluate with 3-8 times the column volume, recover the ethanol under reduced pressure and concentrate, refrigerate for 12-36 hours, filter, take the filter residue, add absolute ethanol for recrystallization, separate the crystals, wash and dry to obtain oleuropein 307.2g, detected by HPLC, the purity is 98.9%.
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