Method for extracting monomer lycorine from lycoris herb
A technology of lycoris and lycorine, which is applied in the direction of organic chemistry, can solve the problems of complicated operation, polluting the environment, and high content of organic solvents, and achieves the effects of simple operation, high extraction rate, and less solvent consumption
Active Publication Date: 2015-06-03
JISHOU UNIVERSITY
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[0004] Chinese patent 2007100532075 discloses a method for extracting active alkaloids from Lycoris genus plants. The alkaloid purification is based on the different alkalinity of Lycoris alkaloids, using segmented extraction technology to simultaneously obtain a variety of Lycoris alkaloids crude products, Then through column chromatography and repeated recrystallization to obtain high-purity Lycoris alkaloid monomers (galantamine, lycorine, ricolamine, polyflora narcismine), and the organic solvent used for extraction is 0.5-3 times the volume of chloroform, n-butanol, petroleum ether, ethyl acetate, ether and isoamyl alcohol, although the invention has improved the comprehensive utilization of Lycoris, the operation is complicated, the organic solvent content is high, and the environment is polluted
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[0023] The present embodiment comprises the following steps: (1) Extraction: Weigh the processed Lycoris powder, add it to water with a pH of 4.5 at a solid-to-liquid ratio of 1:10, and add 1.0% of the mass of Lycoris powder- 3.0% mixed enzyme of cellulase and pectinase, the mass ratio of cellulase and pectinase is 1:1, enzymolysis at 50°C for 20-100min, then ultrasonic treatment for 5-25min, 5000r / min centrifuged for 20 min, and the supernatant was taken to obtain the lycorine extract;
[0024] (2) Purification
[0025] ①Solvent extraction: adjust the pH of the lycorine extract extracted in step (1) to 10 with NaOH, add the extraction agent chloroform at a volume ratio of 1:1, shake well, let stand overnight, remove the lower chloroform phase, and adjust with HCl pH to 2, suction filtration to obtain lycorine extract concentrate;
[0026] ②Cation exchange resin adsorption: adjust the pH of the concentrated extract in step ① to 2 with HCl, use D-001 type cation exchange res...
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The invention relates to a method for extracting monomer lycorine from lycoris herb. The method comprises the following: (1) extraction: weighing processed lycoris herb powder, adding into water with pH of 4.5 according to the ratio of materials to liquid being 1:10 (unit: g / mL), and adding cellulase and pectinase mixture, which is 1.0%-3.0% mass of the lycoris herb powder, wherein the mass ratio of the cellulase to pectinase is 1:1; performing enzymolysis for 20-100min at 50DEG C, then performing ultrasonic treatment for 5-25min, centrifuging for 20min at 5000r / min, and taking supernatant, namely lycorine extracting liquid; and (2) purification: 1) extracting wiht a solvent; 2) adsorbing with cationic exchange resin; 3) performing C18 reverse phase silica gel column chromatography; 4) performing normal phase silica gel column chromatography; and 5) recrystallizing and performing vacuum drying at 50-60DEG C to obtain lycorine monomer. The method is simple to operate, short in extraction time and high in extraction rate, the use amount of organic solvent is less, the cost is low, and the yield of lycorine is 0.1812% by exaction through an ultrasonic synergetic enzyme method; the extraction and purification technology is environment-friendly, and the purity is high up to 99.4%.
Description
technical field [0001] The invention relates to a method for extracting lycorine, in particular to a method for extracting lycorine monomer from plants of the genus Lycoris. Background technique [0002] The chemical synthesis methods of alkaloids such as lycorine in Lycoris have been reported, but extraction from plants of the genus Lycoris is still an important source of such substances. The extraction methods of Lycoris alkaloids in the prior art mainly include solvent extraction. , ultrasonic extraction, microwave extraction, supercritical fluid extraction and other methods, these methods generally have the disadvantages of serious environmental pollution and high production costs. [0003] Chinese patent 2008102047350 discloses a method for extracting and separating lycorine from Lycoris bulbs. The bulbs of Lycoris are used as raw materials, pretreated with compound enzymes, dilute hydrochloric acid leaching, ultrasonic-assisted extraction, and chloroform extraction to ...
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Login to View More IPC IPC(8): C07D491/16
CPCC07D491/16
Inventor 田春莲王鹏覃基信刘小攀
Owner JISHOU UNIVERSITY