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Method for separating Anisodus acutangulus total alkaloid from extract liquid of Anisodus acutangulus

A technology for total alkaloids and extracts, applied in the directions of alkaloids, alkaloids, drug combinations, etc., can solve the problems of increasing production costs, cumbersome steps, increasing process steps, etc., and achieves reduction in the process of regenerating resin columns and alkaloid transfer. The effect of high 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

Although this method can improve the purity of alkaloids, it has a certain degree of progress, but there are still serious defects: the test found that the resin was alkalized with ammonia water, and the efficiency was low, resulting in a low yield; The three alkaloids need to have good solubility in organic solvents, but the use of organic solvents will bring residues of resin monomer components such as styrene, divinylbenzene, and organic solvents into the eluent, which will affect the safety of the preparation; During the test, the resin needs to be poured out and dried, alkalized with ammonia water, and refluxed with a variety of organic solvents for extraction. The steps are cumbersome, and pipeline production cannot be realized. At the same time, due to the use of organic solvents in the process, ethanol must be added in the resin pretreatment Waiting for the steps of organic solvent treatment, the organic solvent must be recovered later, which increases the process steps and increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take 1000g of Sanfensan 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 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, then elute with 15% hydrochloric acid solution, the elution rate is 2 times the column volume / hour, until the alkaloid test is Negative (the effluent was added dropwise with 10% silicotungstic acid without precipitation), the eluate was collected, neutralized to neutral with sodium hydroxide, desalted, and the filtrate was concentrated and dried to obtain three-thirds of the total alkaloids.

Embodiment 2

[0036] Take 1000g of three-point decoction pieces, add pH=5 acidic water for percolation, combine the percolation solution 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), washed with water until the effluent was colorless, then eluted with 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 the eluate, neutralized to neutral with calcium hydroxide, desalted, and the filtrate was concentrated and dried to obtain three thirds total alkaloids.

Embodiment 3

[0038] Take 5kg of Sanfensan decoction pieces, add 70% ethanol for ultrasonic extraction twice, add 5 times the amount each time, ultrasonicate 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 1% hydrochloric acid solution (containing 1% sodium chloride) Elution, the elution rate is 5 times the column volume / hour, until the alkaloid test is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), the eluate is collected, neutralized to neutral with sodium hydroxide, and removed salt, and the filtrate was concentrated and dried to obtain three-thirds of the total alkaloids.

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PUM

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Abstract

The invention discloses a method for separating total alkaloids of a traditional Chinese medicine, and particularly relates to a method for separating the total alkaloids from an extracting solution of scopolia acutangula, which is a traditional Chinese medicine, and belongs to the field of traditional Chinese medicine. The method comprises the following technical proposal: taking the extracting solution of the scopolia acutangula, adjusting the pH value to 1 to 7, filtering, adding filtrate on a cation exchange resin column, removing impurities by water elution firstly, eluting by 0.5 to 15 percent acid liquor secondly until no alkaloid is checked for existence, collecting the elution solution, adding alkali to the elution solution for neutralization, performing the desalting treatment, concentration and drying, and obtaining the total alkaloids of the scopolia acutangula. The method has the advantages of overcoming the defects of low extraction rate, large consumption of organic solvent, complex process, impossible mass production and the like existing in the prior art, and can separate the total alkaloids of the scopolia acutangula with high purity from the extracting solution of the scopolia acutangula in 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 three-thirds of total alkaloids from an extract of three-thirds of traditional Chinese medicines, 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. Sanfensan, also known as Dasou Shanhu, Shanyeyan, and Shanbai, is a plant belonging to the Solanaceae Solanum genus Anisodus acutangulus C.Y.Wu et C.Chen and Himalayan Scopolia Scopolia lurida Dunal [Anisodus luridus Link et Otto] The roots, stems, leaves and seeds are a kind of folk Chinese herbal medicine commonly used in Yunnan, which has the effects of anesthesia, analgesia, wind and dampness. S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/81A61P19/02A61P19/08A61P29/00C07G5/00A61K125/00A61K127/00A61K131/00A61K135/00
Inventor 武建卓王广录
Owner BEIJING HERUN INNOVATION PHARMA TECH DEV
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