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Separation and extraction of icariin A

An extraction method and epimedium technology, which are applied in the field of separation and extraction of icariine A

Inactive Publication Date: 2005-10-12
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most studies on the chemical constituents of Epimedium korean focus on flavonoids, but less on its alkaloids. Since the discovery of magnolanine in 1957, there has been no report on this aspect

Method used

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  • Separation and extraction of icariin A
  • Separation and extraction of icariin A
  • Separation and extraction of icariin A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 3 kg of Epimedium leaves were reflux extracted with 95% ethanol for 3 times, each time for 2 hours, the extracts were combined, concentrated under reduced pressure to obtain a dark green solution, and the chlorophyll was removed to obtain the total alkaloids. Dissolve total alkaloids in 0.2% hydrochloric acid aqueous solution, filter to remove water-insoluble lipophilic impurities, then basify the acidic aqueous solution with ammonia water to pH=9.5, free alkaloids, extract with chloroform to obtain relatively pure total alkaloids . Repeated transsolution with acid and alkali twice.

[0022] The total alkali is eluted by silica gel column chromatography, and then eluted with different gradient eluents. The eluent is monitored by electrospray mass spectrometry, and the eluent is collected. Pass through a basic aluminum oxide chromatography column with chloroform as the eluent, collect fractions, and concentrate. Separation is carried out with high performance liquid ch...

Embodiment 2

[0024] 3.5 kg of Epimedium leaves were refluxed with 90% ethanol and extracted twice for 3 hours each time, the extracts were combined, concentrated under reduced pressure to obtain a dark green solution, and the chlorophyll was removed to obtain the total alkaloids. Dissolve total alkaloids in 0.5% hydrochloric acid aqueous solution, filter to remove water-insoluble lipophilic impurities, then basify the acidic aqueous solution with ammonia water to pH = 10, free alkaloids, extract with chloroform to obtain relatively pure total alkaloids . Repeated transsolution with acid and alkali twice.

[0025] The total alkali was eluted by silica gel column chromatography, and eluted with different gradient eluents successively. The eluent was monitored by electrospray mass spectrometry, and the eluent was collected as chloroform:methanol:ammonia=9.5:2.8:0.5. Pass through a basic aluminum oxide chromatography column with chloroform as the eluent, collect fractions, and concentrate. U...

Embodiment 3

[0027] 3.5 kg of Epimedium leaves were refluxed with 95% ethanol and extracted twice for 3 hours each time, the extracts were combined, concentrated under reduced pressure to obtain a dark green solution, and the chlorophyll was removed to obtain the total alkaloids. Dissolve total alkaloids in 0.4% hydrochloric acid aqueous solution, filter to remove water-insoluble lipophilic impurities, then basify the acidic aqueous solution with ammonia water to pH=10.5, free alkaloids, extract with chloroform to obtain relatively pure total alkaloids . Repeated transsolution with acid and alkali twice.

[0028] The total alkali is eluted by silica gel column chromatography, and then eluted with different gradient eluents. The eluent is monitored by electrospray mass spectrometry, and the eluent is collected. Pass through a basic aluminum oxide chromatography column with chloroform as the eluent, collect fractions, and concentrate. Separation was carried out with high performance liquid...

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Abstract

A separation and extraction of epimedium herb base A is carried out by extracting Korean epimedium herb leaf by alcohol, concentrating, filtering the extract, removing chlorophyll, obtaining total alkaloid, repeating peritectics the total base by acid base, obtaining purified total alkaloid separating with column chromatography method and high-efficient liquid-phase method combing, and obtaining the pure products of the compound with light yellow powder. The chemical structure is determined by nuclear magnetization, Fourier transform ionic cyclotron resonance spectroscopy, electric spraying spectroscopy, and infrared spectrum style. The compound is quaternary natural base. It achieves more chemical ingredients of epimedium herb plant.

Description

technical field [0001] The invention belongs to the separation and extraction method of epimedine A. Background technique [0002] Herba Epimedii (Herba Epimedii), also known as the fairy spleen, is the dry part of the plant of the Berberidaceae (Berberbidaceae) Epimedium (Epimedium) plant on the ground. Epimedium also has the functions of preventing and treating osteoporosis and improving the function of the immune system. The 2000 edition of the Chinese Pharmacopoeia recorded 5 species of plants of the genus Epimedium, and Epimedium korean is one of them, and it is one of the authentic Chinese medicinal materials in Changbai Mountain. Most studies on the chemical constituents of Epimedium korean focus on flavonoids, but less on alkaloids. Since the discovery of magnolanine in 1957, there has been no report on this aspect. Invention content: [0003] The purpose of this invention is to provide a kind of separation and extraction method of epimedine A. [0004] Alkaloid...

Claims

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Application Information

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IPC IPC(8): C07D221/00C07D311/00C07D493/04
Inventor 刘志强刘春明刘淑莹宋凤瑞窦建鹏李丽
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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