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Method for separating huperzia serrata total alkaloids by ion exchange resin

A technology of total alkaloids, thousand-layer tower, applied in the direction of anion exchanger materials, ion exchange, cation exchange, etc., can solve the problems of low purity of total alkaloids, difficult adsorption, low alkaloid efficiency, etc., and achieve industrial production equipment. Reduce requirements, avoid inconvenient operation, and ensure the effect of elution effect

Inactive Publication Date: 2010-04-28
BEIJING HERUN INNOVATION PHARMA TECH DEV
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  • 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
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 huperzia serrata total alkaloids by ion exchange resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Take 1000g of Melaleuca decoction slices, 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 passes through cations at 4 times the column volume / hour Exchange resin (001×2.5, ammonium type, diameter-to-height ratio 1:8), wash with water until the effluent is colorless, then soak the resin with 0.5% hydrochloric acid solution of 2% ammonium chloride for 2 hours. Then elute with 0.1% hydrochloric acid solution of 2% ammonium chloride, the elution rate is 2 times column volume / hour, until the alkaloid test is negative (10% silicotungstic acid is added dropwise to the effluent without precipitation), collect and elute liquid, neutralized to neutral with sodium hydroxide, desalted, and the filtrate was concentrated and dried to obtain the total alkaloids of Melaleuca tower.

Embodiment 2

[0046] Get Melaleuca pagoda decoction piece 1000g, add the acidic water of pH=5 to infiltrate, combine percolate and add water and dilute to 10000ml, centrifuge, adjust pH=1, centrifuge, supernatant passes through cation exchange resin ( 001×7, sodium type, diameter-to-height ratio 1:5), washed with water until the effluent was colorless, then soaked the resin with 0.5% hydrochloric acid solution of 1% sodium chloride for 2 hours. Then elute with 0.3% hydrochloric acid solution of 5% sodium chloride, the elution speed is 4 times of column volume / hour, soak for 5 hours after elution of 2 times of column volume, and then elute until the alkaloid inspection is negative (effluent 10% silicotungstic acid was added dropwise without precipitation), the eluate was collected, neutralized to neutral with sodium hydroxide, desalted, and the filtrate was concentrated and dried to obtain the total alkaloids of Melaleuca tower.

Embodiment 3

[0048] Take 5 kg of Melaleuca 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 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 soak the resin with 0.5% hydrochloric acid solution of 20% sodium chloride 1 hour. Then elute with 0.2% hydrochloric acid solution of 8% sodium chloride, 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 liquid, neutralized to neutral with sodium hydroxide, desalted, and the filtrate was concentrated and dried to obtain the total alkaloids of Melaleuca tower.

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Abstract

The invention discloses a method for separating traditional Chinese medicine huperzia serrata total alkaloids, in particular to a method for separating total alkaloids from traditional Chinese medicine huperzia serrata extract, belonging to the traditional Chinese medicine field. The method includes the following technical scheme: huperzia serrata extract is taken, pH value is adjusted to be 1-7, filtering is carried out, filtrate is taken and added onto cation exchange resin, eluting by water is firstly carried out to remove impurities, and then 0.5-20% saline solution is used for socking the resin, and then 0.5-20% saline solution containing acid or alcohol is used for eluting until no alkaloid is detected, eluant is collected and added with alkali to be natural, and desalinization treatment and concentrated drying are carried out, thus obtaining the traditional Chinese medicine huperzia serrata total alkaloids. The method overcomes the defects of low extraction rate, high organic solvent dosage, excessive high acid-base concentration, complex technology and impossible for large production and the like of the prior art and can efficiently separate high purity huperzia serrata total alkaloids in traditional Chinese medicine huperzia serrata extract.

Description

technical field [0001] The invention relates to a method for extracting and separating active ingredients of traditional Chinese medicine, in particular to a method for extracting and separating total alkaloids of Melaleuca pagoda from the extract liquid of traditional Chinese medicine Melaleuca pagoda, belonging to the field of traditional Chinese medicine. 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 f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/36B01D15/36
Inventor 武建卓朴美善李蓉
Owner BEIJING HERUN INNOVATION PHARMA TECH DEV
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