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Method for separating cytospaz total alkaloid from traditional Chinese medicine extract liquid

A technology of total alkaloids and scopolamines, applied in the directions of alkaloids, alkaloids, drug combinations, etc., can solve the problems of small range of alkaloids, low resin adsorption rate, difficult adsorption, etc., so as to reduce the process of regenerating resin columns, 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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  • Abstract
  • Description
  • Claims
  • Application Information

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 cytospaz total alkaloid from traditional Chinese medicine extract liquid

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Experimental program
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Effect test

Embodiment 1

[0040] Take 1000g of Yangjinhua slices, add water and decoct twice, 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 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% hydrochloric 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, desalinated, and the filtrate was concentrated and dried to obtain the total alkaloids of Datura japonica.

Embodiment 2

[0042] Get 1000g of Teng Gong Teng decoction pieces, add acidic water with pH=5 for percolation, combine the percolation solution 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% hydrochloric acid solution, the elution rate was 4 times the column volume / hour, after elution was 2 times the column volume, soaked for 5 hours, 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 to neutral with calcium hydroxide, desalinated, and the filtrate was concentrated and dried to obtain Ding Gongteng total alkaloids.

Embodiment 3

[0044] Take 5 kg of yangjinhua 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% 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, Desalting, the filtrate was concentrated and dried to obtain the total alkaloids of Dajinhua.

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Abstract

The invention discloses a method for separating total alkaloid from traditional Chinese medicine, in particular a method for separating belladonna 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 belladonna 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 belladonna total alkaloid from 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 hyoscyamine from traditional Chinese medicine extracts, which belongs 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 i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/81A61K36/39A61K36/185A61P29/00A61P25/04A61P23/00C07G5/00C07D451/00
Inventor 刘英辉武建卓
Owner BEIJING HERUN INNOVATION PHARMA TECH DEV
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