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

Inactive Publication Date: 2009-07-29
BEIJING HERUN INNOVATION PHARMA TECH DEV
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Problems solved by technology

But for the refinement of alkaloids, the biggest deficiency of this method is: firstly, it is difficult to adsorb, and the sample medicine solution must be a dilute solution, and the alkalinity should be suitable. The rate is low, the alkalinity is high, the alkaloids are free, and the macromolecular alkaloids are poorly soluble and precipitated, and they still cannot be loaded on the column. The range of applicable alkaloids is very small and there are too few varieties; The adsorption principle has poor selectivity for the separation of active ingredients of alkaloids and fat-soluble impurities, and in the process of solvent elution, because there is no specific elution solvent, alkaloids and a large amount of fat-soluble impurities are often eluted tog...

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  • Method for separating verticine total alkaloids in traditional Chinese medicine extract

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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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Abstract

The invention discloses a method for separating total alkaloid from traditional Chinese medicine, in particular a method for separating verticine total alkaloid from traditional Chinese medicine extract, which belongs to the field of traditional Chinese medicines. The method comprises the following technical proposal that the traditional Chinese medicine extract is taken and filtered, the pH value of the traditional Chinese medicine extract is adjusted to be between 1 and 7; filtrate is added to a cation exchange resin column, eluted with water to remove impurities and then eluted by use of 0.5 to 15 percent acid liquid; and eluent is collected, added with alkali for neutralization and desalted so as to prepare verticine total alkaloid. The method overcomes the deficiency that the prior art is low in extraction ratio, large in the amount of organic solvents, complex in process, incapable of mass production and the like, and can efficiently separate high-purity verticine total alkaloid from the traditional Chinese medicine extract.

Description

technical field [0001] The invention relates to a method for extracting and separating active ingredients of traditional Chinese medicines, in particular to a method for extracting and separating total alkaloids of fritillary alkaloids from traditional Chinese medicine extracts, belonging to the field of traditional Chinese medicines. Background technique [0002] Traditional Chinese medicine alkaloids are an important class of substances existing in nature, and more than 700 species have been isolated so far. They are the largest class of active ingredients in traditional Chinese medicine with definite curative effects and a wide range of uses, especially for cancer, liver disease, cardiovascular and cerebrovascular diseases, and rheumatism. etc. have unique curative effects, such as berberine in coptis for antibacterial and anti-inflammatory, ephedrine in ephedra for asthma, reserpine in Rauwolfia for lowering blood pressure, galantamine in lycoris for children Paralysis s...

Claims

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Application Information

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IPC IPC(8): A61K36/8966A61P11/10A61P11/14C07G5/00A61K125/00
Inventor 刘英辉朴美善王广录
Owner BEIJING HERUN INNOVATION PHARMA TECH DEV
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