Process for separating matrine-like total alkaloids form Chinese medicament extract

A technology of total alkaloids and ginsenosides, applied in the direction of alkaloids, alkaloids, drug combinations, etc., can solve the problems of small range of alkaloids, cumbersome steps, difficult adsorption, etc., to reduce the process of regenerating resin columns, alkaloids The effect of high transfer rate and simple process flow

Inactive Publication Date: 2008-10-22
代龙
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AI Technical Summary

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 separation selectivity of the adsorption principle to the active ingredients of alkaloids and fat-soluble impurities is too poor, 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 washed down together, and finally refined to obtain The purity of the total alkaloids is not high
However, the steps of this method are cumbersome, and the steps of organic solvent extraction and resin column reflux extraction with organic solvent are difficult to realize in industry, and the efficiency of elution with lye is very low, and it only stays at the level of preparing small samples in the laboratory. Unable to achieve mass production
[0007] The above methods generally have the disadvantages of high cost, large consumption of organic solvents, poor selectivity, low purity of total alkaloids, and inability to realize large-scale production. Therefore, purification technology is still a "bottleneck" problem for the separation of alkaloids in traditional Chinese medicine.

Method used

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  • Process for separating matrine-like total alkaloids form Chinese medicament extract

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Take 1000g of Sophora flavescens decoction pieces, add water and decoct twice, 10 times the amount each time, decoct for 2 hours, combine the decoction liquid, centrifuge, adjust pH=3, centrifuge, and the supernatant is passed through cation exchange at 4 times the column volume / hour 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 eluate, and transfer to biological The alkali test was negative (the effluent was added dropwise with 10% silicotungstic acid without precipitation), neutralized with sodium hydroxide to neutral, desalted, and the filtrate was concentrated and dried to obtain the total alkaloids of Sophora flavescens.

Embodiment 2

[0042] Get 1000g of mountain bean root decoction pieces, add the acidic water of pH=5 to percolate, combine the percolate 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 bean root.

Embodiment 3

[0044] Take 5 kg of decoction pieces of Sophora japonica, 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, concentrating and drying the filtrate to obtain the total alkaloids of Sophora japonica.

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Abstract

The invention discloses a method for separating total alkaloid of traditional Chinese medicines, in particular a method for separating the matrine type total alkaloid from the extraction solution of traditional Chinese medicines and belongs to the field of traditional Chinese medicines. The method includes the technical proposal as follows: the extraction solution of traditional Chinese medicines is taken; the pH value is adjusted between 1 and 7; the solution is filtered; the filtrate is added to a cation exchange resin column; firstly, water is used for elution and impurity removal; then the acid solution of 0.5 to 15 percent is used for elution; the eluate is collected; the alkali is added for neutralization and then the matrine type total alkaloid is obtained through desalted treatment. The method overcomes the defects of low extraction rate, a large amount of organic solvents, complex process and no mass production, etc., in the prior art and can separate the highly purified matrine type total alkaloid from the extraction solution of traditional Chinese medicines with high efficiency.

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 matrine alkaloids from 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 sequelae have curative effect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07G5/00A61K36/48A61P31/12A61P1/16A61P25/28
Inventor 代龙赵德峰高鹏张加余冯新刚
Owner 代龙
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