Alkali precipitation agent for nuciferine extraction and nuciferine extraction method
The technology of a precipitation agent and lotus leaf base is applied in the field of natural medicine extraction, can solve the problems of complicated operation, expensive equipment, low yield and the like, and achieves the effect of simple process and low cost
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Embodiment 1
[0033] Take 10kg of lotus leaves, crush them, add 100L80wt.% ethanol, extract for 2h, filter, collect the filtrate, add 100L80wt.% ethanol to the filter residue, extract for 2h, filter, collect the filtrate, add 80L80wt.% ethanol to the filter residue, extract for 2h, filter, and combine Three filtrates were concentrated under reduced pressure to a volume of 10L, left to stand, and centrifugally dried to obtain the crude extract of lotus leaf; the crude extract of lotus leaf was crushed and sieved to get about 80 mesh particles, and 10L of nuciferine precipitation agent (n-butanol 45wt .%; potassium hydroxide solution 15wt.%, wherein, potassium hydroxide content is 10wt.%; dichloromethane 40wt.%), heated to 50 ℃, 60r / min stirring 5h, static centrifugal drying to get nuciferine crude Nuciferine coarse crystals were dissolved in 0.5L 90wt% methanol, placed at 4°C for 10 hours, crystallized, filtered and dried to obtain 15.5 g of nuciferine with a purity of 98.1%.
Embodiment 2
[0035] Take 20kg of lotus leaves, crush them, extract with 200L90wt.% ethanol for 2 hours, filter, collect the filtrate, add 200L90wt.% ethanol to the filter residue, extract for 2 hours, filter, collect the filtrate, combine the two filtrates, concentrate the volume to 10L, let it stand, and dry it by centrifugation The lotus leaf crude extract is obtained; the lotus leaf crude extract is pulverized and sieved to get about 70 mesh particles, and 20L of nuciferine precipitation agent (55wt.% of ethanol; 8wt.% of sodium hydroxide solution, wherein the sodium hydroxide content of 5wt.%; petroleum ether 35wt.%), heated to 55°C, stirred at 80r / min for 10h, left to stand and centrifuged to dry to obtain nuciferine coarse crystals; dissolve nuciferine coarse crystals with 1L90wt% methanol, and place at 4°C After 10 hours, crystallize, filter and dry to obtain 25.5 g of nuciferine with a purity of 98.2%.
Embodiment 3
[0037] Take 40kg of lotus leaves, crush them, extract with 400L90wt.% methanol for 1.5h, filter, collect the filtrate, add 400L90wt.% methanol to the filter residue, extract for 1.5h, filter, collect the filtrate, extract with 320L90wt.% methanol for 1.5h, filter, and collect the filtrate , combined three filtrates, concentrated under reduced pressure to a volume of 20L, stood still, and centrifuged to dry to obtain the lotus leaf crude extract; the lotus leaf crude extract was crushed and sieved to get about 90 mesh particles, and 40L of nuciferine precipitation agent (ethanol 35wt .%; barium hydroxide solution 10wt.%, wherein, the content of barium hydroxide is 5wt%; petroleum ether 55wt.%), heated to 65 ℃, stirred at 90r / min for 10h, left standing and centrifugally dried to obtain nuciferine coarse crystals Dissolve the coarse crystals of nuciferine with 2L90wt.% methanol, place at 4°C for 10 hours, crystallize, filter and dry to obtain 70.5g of nuciferine with a purity of 9...
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