Process for separating total alkaloids form Chinese medicament extracting solution

A technology for alkaloids and extracting solution, which is applied in the field of extraction and separation of effective components of traditional Chinese medicine and total alkaloids, can solve the problems of low purity of total alkaloids, difficult adsorption, low alkaloid efficiency, etc., and reduce the requirements of industrial production equipment. , Avoid inconvenient operation and ensure the effect of elution effect

Inactive Publication Date: 2008-10-22
山东禹泽药康产业技术研究院有限公司
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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
However, the steps of the above-mentioned method are cumbersome, and it is difficult to realize industrially processes such as organic solvent extraction or organic solvent reflux extraction of the resin, and the efficiency of eluting alkaloids with lye is very low
At present, this method only stays at the level of preparing small samples in the laboratory, and cannot achieve large-scale production.
[0009] In summary, the above methods generally have defects such as 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 the "bottleneck" for the separation of total alkaloids from traditional Chinese medicine. question

Method used

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  • Process for separating total alkaloids form Chinese medicament extracting solution
  • Process for separating total alkaloids form Chinese medicament extracting solution

Examples

Experimental program
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Effect test

Embodiment 1

[0047] Take 1000 g of Sophora flavescens decoction pieces, add water to 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 (001×7, hydrogen type, diameter-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% calcium chloride for 2 hours. Then use 2% calcium chloride and 0.5% 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 solution is neutralized with calcium hydroxide to neutrality, desalted, and the filtrate is concentrated and dried to obtain total alkaloids of Sophora flavescens.

Embodiment 2

[0049] Take 1000g of Radix rhizome decoction pieces, add pH=5 acid water to percolate, add the combined percolation solution to dilute to 10000ml with water, centrifuge, adjust pH=1, centrifuge, and the supernatant is passed through a cation exchange resin (5 times the column volume / hour) ( 001×12, sodium type, diameter-height ratio 1:5), washed with water until the effluent was colorless, and then soaked the resin with a 1% hydrochloric acid solution of 1% sodium chloride for 2 hours. Elute with 2% 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 the total alkaloids of Radix japonica.

Embodiment 3

[0051] Take 5 kg of Sophora japonica decoction pieces, add 70% ethanol for ultrasonic extraction twice, add 5 times the volume each time, ultrasonicate for 0.5 hours, combine the extracts, centrifuge, recover ethanol, add water to 5000ml, adjust pH=2, centrifuge, supernatant Pass through the upper cation exchange resin (001×10, sodium type, diameter-height ratio 1:7) at 2 times the column volume / hour, wash with water until the effluent is colorless, and then soak the resin with 20% sodium chloride and 0.5% hydrochloric acid solution 1 hour. Then use 1% hydrochloric acid solution of 8% sodium chloride to elute, and the elution speed is 5 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 solution is neutralized with sodium hydroxide to neutrality, desalted, and the filtrate is concentrated and dried to obtain the total alkaloids of Sophora japonica...

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Abstract

The invention discloses a method for separating total alkaloid of traditional Chinese medicines, in particular a method for separating the total alkaloid from the extraction solution of traditional Chinese medicines and belongs to the field of traditional Chinese medicines. The method includes the technical proposal as follows: the extraction solution of traditional Chinese medicines is taken; the pH value is adjusted between 1 and 7; the solution is filtered; the filtrate is added to a cation exchange resin column; firstly, water is used for elution and impurity removal; then the resin column is immersed with 0.5 to 20 percent of the salt solution; 0.5 to 20 percent of the salt solution with acid or ethanol is used for elution until no alkaloid is tested; and the eluate is collected; thealkali is added for neutralization and then the total alkaloid of traditional Chinese medicines is obtained after the concentration drying through the desalted treatment. The method overcomes the defects of the low extraction rate, a large amount of organic solvents, too high acid base concentration, complex process, no mass production, etc., in the prior art and can separate the highly purified total alkaloid from the extraction solution of traditional Chinese medicines with high efficiency.

Description

technical field [0001] The invention relates to a method for extracting and separating effective components of traditional Chinese medicines, in particular to a method for extracting and separating total alkaloids from extracts of traditional Chinese medicines, and belongs to the field of traditional Chinese medicines. 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 sequelae have curati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07G5/00
Inventor 代龙张加余贾世伟高鹏赵德峰
Owner 山东禹泽药康产业技术研究院有限公司
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