Method for separating verticine total alkaloids in traditional Chinese medicine extract
A technology of total alkaloids and fritillary alkaloids, applied in the directions of alkaloids, alkaloids, drug combinations, etc., can solve the problems of small range of alkaloids, cumbersome steps, difficult adsorption, etc., and reduce the process of regenerating resin columns, alkaloids The effect of high transfer rate and simple process flow
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Embodiment 1
[0040] Take 1000g of Fritillaria decoction pieces, add water to decoct 2 times, 10 times the amount each time, decoct for 2 hours, combine the decoction liquid, centrifuge, adjust the pH=3, centrifuge, and the supernatant passes through cations at 4 times the column volume / hour Exchange resin (001×7, hydrogen type, diameter-to-height ratio 1:8), wash with water until the effluent is colorless, add 3% sulfuric acid for elution, and the elution rate is 2 times the column volume / hour, collect the eluent, until The alkaloid test was negative (the effluent was added dropwise with 10% silicotungstic acid without precipitation), neutralized to neutral with sodium hydroxide, desalted, and the filtrate was concentrated and dried to obtain the total alkaloids of Fritillaria chinensis.
Embodiment 2
[0042] Get Chuan Fritillaria decoction pieces 1000g, add the acidic water of pH=5 to infiltrate, combine the infiltrate and add water and dilute to 10000ml, centrifuge, adjust pH=1, centrifuge, supernatant passes through cation exchange resin ( 001×12, sodium type, diameter-to-height ratio 1:5), washed with water until the effluent was colorless, then eluted with 0.5% hydrochloric acid solution, the elution rate was 4 times the column volume / hour, eluted 2 times the column volume and then soaked After 5 hours, elute again until the alkaloid test is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), collect this part of the eluate, neutralize it with calcium hydroxide to neutrality, remove salt, and concentrate and dry the filtrate to obtain Total alkaloids of Fritillaria sichuanensis.
Embodiment 3
[0044] Take 5 kg of Fritillaria decoction pieces, add 70% ethanol to ultrasonically extract twice, add 5 times the amount each time, ultrasonically for 0.5 hours, combine the extracts, centrifuge, recover ethanol, add water to 5000ml, adjust pH = 2, centrifuge, and supernatant Pass through the upper cation exchange resin (001×10, sodium type, diameter-to-height ratio 1:7) at 2 times the column volume / hour, wash with water until the effluent is colorless, and then use 6% hydrochloric acid solution (containing 1mol / L CaCl 2 ) elution, the elution rate is 5 times column volume / hour, collect the eluate until the alkaloid test is negative (the effluent is added dropwise with 10% silicotungstic acid without precipitation), and neutralized to neutral with sodium hydroxide, Desalting, the filtrate is concentrated and dried to obtain the total alkaloids of Fritillaria sichuanensis.
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