Method for separating berberine total alkaloid from extract liquid of traditional Chinese medicine

A technology of total alkaloids and berberine, applied in the direction of alkaloids, alkaloids, drug combinations, etc., can solve the problems of small alkaloid range, low resin adsorption rate, and difficult adsorption, so as to reduce the process of regeneration resin column, The effect of high alkaloid transfer rate and simple process flow

Inactive Publication Date: 2009-07-29
BEIJING HERUN INNOVATION PHARMA TECH DEV
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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 steps such as 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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  • Method for separating berberine total alkaloid from extract liquid of traditional Chinese medicine

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Take 1000g of Coptidis 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 the cation exchange resin at 4 times the column volume / hour (001×7, hydrogen type, diameter-to-height ratio 1:8), wash with water until the effluent is colorless, add 3% sulfuric acid for elution, the elution rate is 2 times column volume / hour, collect the eluate, and reach the alkaloid The 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 Coptis rhizome.

Embodiment 2

[0042] Take 1000g of Coptidis rhizome decoction pieces, add acidic water with pH=5 for percolation, combine the percolation liquid and add water to dilute to 10000ml, centrifuge, adjust pH=1, centrifuge, supernatant passes through cation exchange resin (AmberliteIR- -120, hydrogen type, diameter-to-height ratio 1:6), washed with water until the effluent was colorless, then eluted with 0.5% sulfuric acid solution, the elution rate was 4 times the column volume / hour, after elution was 2 times the column volume, soaked for 5 hours, and then eluted until the alkaloid test was negative (the effluent was added dropwise with 10% silicotungstic acid without precipitation), collected this part of the eluate, neutralized with calcium hydroxide to neutral, desalinated, and the filtrate was concentrated and dried to obtain Coptis rhizome total alkaloids.

Embodiment 3

[0044] Take 5 kg of Chuan Phellodendron 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 the supernatant to 2 times column volume / hour passes through the upper cation exchange resin (001×10, sodium type, diameter-to-height ratio 1:7), washes with water until the effluent is colorless, and then uses 6% sulfuric acid solution (containing 1mol / L of 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, In addition to desalting, the filtrate was concentrated and dried to obtain the total alkaloids of Phellodendron Phellodendri.

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Abstract

The invention discloses a method for separating total alkaloid from traditional Chinese medicine, in particular a method for separating jamaicin total alkaloid from an extracting solution of the traditional Chinese medicine, and belongs to the field of traditional Chinese medicines. The method comprises the following technical proposal: taking the extracting solution of the traditional Chinese medicine; adjusting the pH value of the extracting solution to between 1 and 7; filtering the extracting solution; taking and adding the filtrate to a cation exchange resin column; rinsing the filtrate and removing the impurities; eluting the filtrate with 0.5 to 15 percent acid liquor; collecting eluent; adding alkali to the eluent for neutralization; performing desalting treatment on the mixed solution; and obtaining the jamaicin total alkaloid. The method overcomes the defects of low extracting rate, large using level of organic solvent, complicated process, inability of large-scale production, and the like in the prior art, and can efficiently separate high purity of the jamaicin total alkaloid from the extracting solution of the traditional Chinese medicine.

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 berberine 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 ephedrine in ephedra for relieving asthma, reserpine in Rauwolfia for lowering blood pressure, galantamine in lycoris for sequelae of poliomyelitis, and the Morphine is a famous analgesic; quinine is a valua...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/71A61K36/75A61K36/29A61K36/59A61P29/00A61P1/04A61P1/16A61P17/02C07G5/00C07D455/00
Inventor 朴美善张峰王广录
Owner BEIJING HERUN INNOVATION PHARMA TECH DEV
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