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Peganum harmalaL total alkaloids separation method in peganum harmalaL extract

A technology of total alkaloids and camel cape, applied in the direction of alkaloids, alkaloids, drug combinations, etc., can solve the problems of large production troubles, incomplete alkaloid dissociation, low transfer rate, etc., 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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the methods in other reports, the above two methods have improved the purity of alkaloids, and have certain progress, but there are still serious defects: after the two methods use ammonia to alkalize the resin, elute with organic solvent or reflux with chloroform However, due to the low alkalinity of ammonia water and the incomplete dissociation of alkaloids, the transfer rate is still not high; the use of toxic organic solvents such as ether and chloroform has brought hidden dangers to the production operation and the safety of the final preparation The use of organic solvents will bring residues of resin monomer components such as styrene and divinylbenzene into the eluent, which will affect the safety of the preparation; the latter also needs to pour out the resin and put the resin into a Soxhlet extractor The use of diethyl ether for reflux extraction has brought a lot of trouble to large-scale production; at the same time, due to the use of organic solvents in the process, it is also required to increase the ethanol treatment step in the pre-treatment of the resin, and the organic solvent must be recovered later, which increases the process steps and improves the quality of the resin. cost of production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take 1000g of decoction slices of Luotuo Peng, decoct twice with water, 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), washed with water until the effluent was colorless, then eluted with 15% hydrochloric acid solution, the elution rate was 2 times the column volume / hour, and the eluate was collected 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 Camelina camel.

Embodiment 2

[0036] Get 1000g of decoction pieces of camel pods, add pH=5 acidic water for percolation, combine the percolation liquid and add water to dilute to 10000ml, centrifuge, adjust pH=1, centrifuge, supernatant passes through cation exchange resin (Doulex 50, sodium type, diameter-to-height ratio 1:5), wash with water until the effluent is colorless, then elute with 5% hydrochloric acid solution, the elution rate is 4 times the column volume / hour, after elution is 2 times the column volume, soak for 5 hours , and then eluted until the alkaloid test was negative (10% silicotungstic acid was added dropwise to the effluent without precipitation), the acid eluate was collected, neutralized to neutral with calcium hydroxide, desalted, the filtrate was concentrated and dried to obtain the total alkaloids.

Embodiment 3

[0038] Take 5 kg of decoction pieces of Camel Cape, add 70% ethanol and 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 the column volume / hour, pass through the upper cation exchange resin (001×10, sodium type, diameter-to-height ratio 1:7), wash with water until the effluent is colorless, and then wash with 1% hydrochloric acid solution (containing 1% sodium chloride) Elute, the elution rate is 5 times the column volume / hour, collect the eluate until the alkaloid test is negative (the effluent is added dropwise with 10% silicotungstic acid without precipitation), neutralize to neutral with sodium hydroxide, and desalt , and the filtrate was concentrated and dried to obtain the total alkaloids of Camelina.

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Abstract

The invention discloses a method for separating total alkaloid from traditional Chinese medicine, in particular a method for separating total alkaloid from an extracting solution of the traditional Chinese medicine, namely Peganum harmala, and belongs to the field of traditional Chinese medicines. The method comprises the following technical proposal: taking the extracting solution of the Peganum harmala; 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 Peganum harmala 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 Peganum harmala total alkaloid from the extracting solution of the Peganum harmala.

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 camel pontifex from extracts of traditional Chinese medicine ponchos, belonging to the field of traditional Chinese medicines. Background technique [0002] Alkaloids are a large class of basic nitrogen-containing compounds that widely exist in nature, are active ingredients of many Chinese herbal medicines, and are an important class of substances in nature. The source of Camelia is Peganum harmalaL., a plant of Tribulus terrestris, which is used as medicine with the whole plant and seeds. Also known as bitter bitter vegetable, Artemisia camel, stinky grass, stinky peony, safflower peas, etc., it is a commonly used folk Chinese herbal medicine. Studies have shown that the total alkaloids of camels are its main effective parts, including Harmaline, Harmine, Harma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/185A61P11/14A61P17/04A61P29/00A61P35/00C07G5/00A61K131/00
Inventor 李蓉刘英辉
Owner BEIJING HERUN INNOVATION PHARMA TECH DEV
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