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A kind of preparation method of high-purity rhynchophylline monomer

A technique of urticine and high purity, which is applied in the field of preparation of high-purity urticine monomer, can solve the problems such as unseen uricine monomer, and achieves the effects of softening the separation environment, saving solvent and shortening the separation time.

Inactive Publication Date: 2016-08-24
GUIZHOU ACADEMY OF TESTING & ANALYSIS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The products obtained by the technologies described in Chinese patents CN102311435A, CN102093359A, etc. are only a kind of rhynchophylline monomer, and there is no report on the simultaneous preparation of two kinds of high-purity rhynchophylline monomers

Method used

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  • A kind of preparation method of high-purity rhynchophylline monomer
  • A kind of preparation method of high-purity rhynchophylline monomer
  • A kind of preparation method of high-purity rhynchophylline monomer

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Weigh 10 kg of Uncaria vine, coarsely crush it, and carry out reflux extraction with 95% ethanol solution in mass percent concentration. The number of extractions is 3 times, and each extraction is 2 hours. The 3 extractions are combined and concentrated under reduced pressure to obtain an extract. The extract was dissolved in 1000 milliliters of water, the pH value was adjusted to 9.5 with ammonia water, and then extracted with chloroform. After the chloroform extract was concentrated, 42.6 g of Uncaria uncaria extract was obtained.

[0029] The rhynchophylline extract was loaded on the silica gel column chromatography, and the chloroform-methanol ratio was 50:1, 30:1, 20:1, 10:1 to elute successively according to the volume ratio, and the eluate was collected and subtracted. Concentrate under pressure to get crude rhynchophylline;

[0030] According to the volume ratio, take petroleum ether: ethyl acetate: isopropanol: water as 2:6:3:9 to measure each solvent, after m...

Embodiment 2

[0034] Weigh 10 kg of Uncaria vine, coarsely crush it, and carry out reflux extraction with 90% ethanol solution in mass percent concentration. The number of extractions is 2 times, and each extraction is 3 hours. The 2 extractions are combined and concentrated under reduced pressure to obtain an extract. The extract was dissolved in 1000 milliliters of water, the pH was adjusted to 10 with ammonia water, and then extracted with chloroform. After the chloroform extract was concentrated, 44.3 g of Uncaria uncaria extract was obtained.

[0035] The rhynchophylline extract is loaded on a silica gel column chromatography, and the chloroform-methanol ratio is 20:1 for elution according to the volume ratio, the eluate is collected, concentrated under reduced pressure, and the crude rhynchophylline is obtained;

[0036] According to the volume ratio, take petroleum ether: ethyl acetate: ethanol: water as 2:7:2:9 to measure each solvent, after mixing, take 10mL of mixed separation solv...

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Abstract

The invention relates to a method for preparing a high-purity rhynchophylline monomer and belongs to the technical field of separation and purification of active ingredients of a traditional Chinese medicine. The method comprises the following steps: a, loading a rhynchophylline extract sample on a silica gel chromatographic column, eluting with a halogenated alkane-alcohol system, collecting eluate and concentrating to obtain a rhynchophylline crude product; and b, loading the rhynchophylline crude product dissolving solution on high-speed countercurrent chromatograph to respectively obtain a rhynchophylline monomer and a corynoxeine monomer. The method has the advantage that two monomers, namely, rhynchophylline and corynoxeine each of which the purity is more than 96% can be effectively prepared.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines, and in particular relates to a preparation method of high-purity rhynchophylline monomer. Background technique [0002] Uncaria is Uncaria rhynchophylla (Miq.) Miq.ex Havil, U. macrophylla Wall., U. hirsuta Havil., U. sinensis (Oliv.) Havil. , or the dry hooked stems of U.sessilifructus Roxb. Uncaria is slightly cold in nature, sweet in taste, and returns to the liver and pericardium meridians. It can clear away heat and calm liver, calm wind and calm convulsions, and has the effects of clearing heat, calming convulsions, calming liver and quenching wind. [0003] The main active ingredients in Uncaria are alkaloids. Among them, rhynchophylline accounts for 28.9% of the total alkaloids, has low toxicity, small side effects, and has good medicinal curative effect. In recent years, its pharmacological research reports can...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/20
CPCC07D471/20
Inventor 张清海林昌虎谭红林绍霞洪江罗文敏蒋影张继东宋光林
Owner GUIZHOU ACADEMY OF TESTING & ANALYSIS
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