Method for separating total alkaloid from sophora flavescens ait by using ion exchange resin

A total alkaloid and cation exchange technology, applied in the field of traditional Chinese medicine, can solve the problems of low purity of total alkaloids, cumbersome steps, difficult adsorption, etc., and achieve the effects of reducing requirements for industrial production equipment, simple process flow, and cost reduction.

Active Publication Date: 2010-02-17
ANHUI BIOLOGICAL PEPTIDE IND RES INST
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  • Abstract
  • Description
  • Claims
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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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  • Method for separating total alkaloid from sophora flavescens ait by using ion exchange resin

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Experimental program
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Effect test

Embodiment 1

[0042] Take 1kg of summer-free 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, sodium type, diameter-to-height ratio 1:8), washed with water until the effluent was colorless, and then soaked in 20% sodium chloride solution for 2 hours. Then elute with 5% sodium chloride solution containing 60% ethanol, the elution rate 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 eluate is collected , neutralized to neutral with sodium hydroxide, desalted, and the filtrate was concentrated and dried to obtain no total alkaloids in summer.

Embodiment 2

[0044] Take 10kg of Fangji decoction pieces, add water to decoct twice, 10 times the amount each time, decoct for 2 hours, combine the decoction liquid, filter, concentrate the filtrate to a relative density of 1.1 (60°C), add ethanol to a concentration of 70% , stand still, ethanol is recovered from the supernatant, add water to 10000ml, adjust pH=3, centrifuge, and the supernatant passes through the upper cation exchange resin (001×4, potassium type, diameter-to-height ratio 1:8) with 3 times of column volume / hour ), washed with water until the effluent was colorless, and soaked the resin with 15% sodium chloride solution for 3 hours. Then elute with 0.05% sodium chloride solution containing 80% ethanol, the elution rate is 6 times column volume / hour, until the alkaloid test is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), collect and elute solution, neutralized to neutral with sodium hydroxide, desalinated, and the filtrate was ...

Embodiment 3

[0046] Take 5 kg of Stephania vine 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 the supernatant to 2 times the column volume / hour is passed through the upper cation exchange resin (001×10, sodium type, diameter-to-height ratio 1:7), washed with water until the effluent is colorless, and then soaked in the resin with 10% sodium chloride solution for 1 hour. Then elute with 6% sodium chloride solution containing 50% ethanol, the elution rate is 5 times column volume / hour, until the alkaloid test is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), collect and elute solution, neutralized to neutral with sodium hydroxide, desalted, and the filtrate was concentrated and dried to obtain the total alkaloids of Stephania vine.

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Abstract

The invention discloses a method for separating total alkaloid from sophora flavescens ait by using ion exchange resin, which belongs to the field of Chinese medicament. The method comprises the following technical schemes: taking Chinese medicament extract, adjusting the pH value to 1-7, carrying out filtration, passing the extract through a cation exchange resin column, washing the extract by using deionized water until the pH value reaches 5-7, soaking the resin column in saline solution at appropriate concentration; eluting the extract by using saline solution containing ethanol until no alkaloid is detected, collecting the eluent, adding alkali to the eluent for neutralization, and obtaining Chinese medicament total alkaloid after desalination, concentration and drying. The method overcomes the disadvantages of low extraction efficiency, large consumption of organic solvent, excessively high acid and alkali concentration, complicated technique, unavailable mass production and thelike in the prior art. Moreover, the method can efficiently separate high-purity Chinese medicament total alkaloid from the Chinese medicament 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 traditional Chinese medicines from extracts of traditional Chinese medicines, belonging 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 berberine in coptis for antibacterial and anti-inflammatory, ephedrine in ephedra for asthma, reserpine in Rauwolfia for lowering blood pressure, galantamine in lycoris for children...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/13A61K36/185A61K36/24A61K36/28A61K36/29A61K36/56A61K36/59A61K36/60A61K36/62A61K36/66A61K36/714A61K36/718A61K36/75A61K36/756A61K36/758A61K36/81A61K36/88A61K36/896A61K36/8966A61K36/904A61K36/9066C07G5/00
Inventor 代龙
Owner ANHUI BIOLOGICAL PEPTIDE IND RES INST
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