Preparation method of high-purity carnosol
A carnosol, high-purity technology is applied in the field of preparation of natural active compounds, which can solve the problems of limited sources, difficulties and high manufacturing costs, and achieve the effects of simple operation process and controllable cost.
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Embodiment 1
[0017] Take 2000g of dried rosemary branches and leaves, add petroleum ether 14L, reflux extraction 3 times, each time for 3 hours, combine the extracts 3 times, concentrate and recover petroleum ether to obtain extract; dissolve the extract with 40% ethanol, filter Remove insoluble matter, get 1000ml of mother liquor as the adsorption solution, and use 500ml of D101 macroporous adsorption resin for adsorption. After the adsorption is completed, use 1000ml of purified water to elute, and then use 1500ml of 90% ethanol solution for elution. The eluent is divided into 6 sections, and the middle 4 parts; the combined eluate was concentrated to 100ml under reduced pressure, added 200ml of water, stirred and precipitated, and left for 3 hours; centrifuged to obtain a precipitate containing carnosol; the precipitate was dissolved with 200ml ethyl acetate, and 200ml petroleum ether was added to it , stirred, and precipitated; filtered to obtain carnosol crude product, which was crysta...
Embodiment 2
[0019] Take 2000g of dried rosemary branches and leaves, add 10L of dichloromethane, reflux extraction 3 times, each time for 3 hours, combine the extracts 3 times, concentrate and recover dichloromethane to obtain extract; dissolve the extract with 60% ethanol , filter to remove insoluble matter, get 1000ml of mother liquor as the adsorption solution, and use 500ml of AB-8 macroporous adsorption resin for adsorption. section, combined 4 parts in the middle; the combined eluent was concentrated under reduced pressure to 150ml, added 200ml of water, stirred and precipitated, and left for 5 hours; centrifuged to obtain a precipitate containing carnosol; the precipitate was dissolved in 150ml of dichloromethane, and Add 200ml of petroleum ether, stir, and precipitate out; filter to obtain the crude product of carnosol, which is crystallized with 700ml of methanol to obtain carnosol crystals; filter and dry to obtain 14.7g of crystals, and the content of carnosol as detected by HPL...
Embodiment 3
[0021] Weigh 500g of rosemary extract (the content of carnosol as determined by HPLC is 5.7%), dissolve it in 2500ml of 60% ethanol, filter out the insoluble matter, use the mother liquor as the adsorption liquid, and use 800ml of HZ818 macroporous adsorption resin for adsorption. Use 2000ml of purified water to elute, then use 2000ml of 90% ethanol solution to elute, the eluent is divided into 6 sections, and the middle 4 parts are combined; the combined eluent is concentrated to 300ml under reduced pressure, add 350ml of water, stir to precipitate the precipitate, place 3 hours; centrifuged to obtain a precipitate containing carnosol; the precipitate was dissolved with 300ml ethyl acetate, 200ml petroleum ether was added thereto, stirred, and the precipitate was precipitated; the crude product of carnosol was obtained by filtration, and the crude product was crystallized with 1000ml of methanol to obtain carnosol Carnosol was crystallized; filtered and dried to obtain 23.9 g ...
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