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Method for separating total alkaloids from dactylicapnos root

A technology of total alkaloids and Zijinlong, which is applied in the direction of drug combination, pharmaceutical formula, plant raw materials, etc., can solve the problems of high requirements on production equipment, difficult adsorption, and many operation steps, so as to reduce the requirements of industrial production equipment and avoid inconvenience. Easy to operate and ensure the effect of the elution effect

Inactive Publication Date: 2009-04-01
北京凯瑞创新医药科技有限公司
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  • Summary
  • 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 liquid must be a dilute solution, and the alkalinity should be suitable: the alkaloids are still in an ionized state when the alkalinity is low, and the resin The adsorption rate is low; the alkalinity is high, the alkaloids are free, and the macromolecular alkaloids are poorly soluble and precipitated, but still cannot be loaded on the column
This method has many operating steps, and the production process is difficult to control; due to the use of more acid and alkali, the requirements for production equipment are very high, which is not conducive to the promotion of large-scale production; The transfer rate is low, resulting in a large waste

Method used

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  • Method for separating total alkaloids from dactylicapnos root
  • Method for separating total alkaloids from dactylicapnos root

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Take 1000 g of Zijinlong 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 (001×2.5, ammonium type, diameter-to-height ratio 1:8), washed with water until the effluent was colorless, and then soaked the resin with a 0.5% hydrochloric acid solution of 2% ammonium chloride for 2 hours. Then use 2% ammonium chloride in 0.1% hydrochloric acid solution to elute, the elution speed is 2 times the column volume / hour, until the alkaloid test is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), and the elution is collected. The filtrate is neutralized to neutrality with sodium hydroxide, desalted, and the filtrate is concentrated and dried to obtain the total alkaloids of Zijinlong.

Embodiment 2

[0048] Take 1000g of Zijinlong decoction pieces, add acid water with pH=5 to percolate, add the combined percolation solution to dilute to 10000ml with water, centrifuge, adjust pH=1, centrifuge, and the supernatant is passed through cation exchange resin (001 ×7, sodium type, diameter-height ratio 1:6), washed with water until the effluent was colorless, and then soaked the resin with a 0.5% hydrochloric acid solution of 1% sodium chloride for 2 hours. Elute with 0.3% hydrochloric acid solution of 5% sodium chloride again, the elution speed is 4 times the column volume / hour, soak for 5 hours after eluting 2 times the column volume, and then elute until the alkaloid check is negative (effluent). 10% silicotungstic acid was added dropwise without precipitation), the eluate was collected, neutralized with sodium hydroxide to neutrality, desalted, and the filtrate was concentrated and dried to obtain Zijinlong total alkaloids.

Embodiment 3

[0050] Take 5 kg of Zijinlong 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 the supernatant is 2 times the column volume / hour passed through the upper cation exchange resin (001×10, sodium type, diameter-height ratio 1:8), washed with water until the effluent was colorless, and then soaked the resin 1 with 20% sodium chloride and 0.5% hydrochloric acid solution Hour. Then use 8% sodium chloride and 0.2% hydrochloric acid solution to elute, the elution speed is 5 times the column volume / hour, until the alkaloid check is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), and the elution is collected. The filtrate is neutralized to neutrality with sodium hydroxide, desalted, and the filtrate is concentrated and dried to obtain the total alkaloids of Zijinlon...

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Abstract

The invention discloses a method for separating total alkaloids in traditional Chinese medicine dactylicapnos root, in particular to the method for separating the total alkaloids from extract liquid of the traditional Chinese medicine dactylicapnos root, and the method belongs to the traditional Chinese medicine field. The method comprises the following technical proposal: the extract liquid of dactylicapnos root is taken, the pH value is adjusted to be 1-7; filtration is carried out, and filtrate is taken and added on a cation exchange resin column; water is firstly used for elution and impurity removal, salt solution of 0.5 percent-20 percent is further used for soaking the resin column, the salt solution of 0.5 percent-20 percent containing acid or ethanol is used for elution until no alkaloids is detected in inspection, eluent is collected, base is added for neutralization, and the total alkaloids in the traditional Chinese medicine dactylicapnos root are obtained by concentration and drying after desalting treatment. The method overcomes the shortcomings of low extraction rate, great using amount of organic solvent, too high acid-base concentration, complicated process, inability of large-scale production, and the like, and the method can effectively separate the high-purity total alkaloids in the dactylicapnos root from the extract liquid of the traditional Chinese medicine dactylicapnos root.

Description

technical field [0001] The invention relates to a method for extracting and separating effective components of traditional Chinese medicine, in particular to a method for extracting and separating total alkaloids of Zijinlong from the extract of traditional Chinese medicine Zijinlong, belonging to the field of traditional Chinese medicine. Background technique [0002] Traditional Chinese medicine alkaloids are a class of important substances in nature, and more than 700 kinds of them have been isolated at present. They are the largest type of active ingredients in traditional Chinese medicine with definite curative effect and wide application, especially for cancer, liver disease, cardiovascular and cerebrovascular diseases, and rheumatism. It has unique curative effects, such as berberine in Coptis chinensis for antibacterial and anti-inflammatory, ephedrine in ephedra for asthma, reserpine in Rauwolfia for blood pressure, and galantamine in Lycoris for children. Paralysis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/66A61P29/00A61P9/12A61K125/00
Inventor 张佳余刘国飞
Owner 北京凯瑞创新医药科技有限公司
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