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Separating method of icariside I monomer in Korean epimedium leaves

A technology of icariin and epimedium leaves, applied in the field of natural medicinal chemistry, can solve the problems of low yield, time-consuming and labor-intensive separation process, and achieve the effect of high efficiency and simple method

Active Publication Date: 2010-11-24
JILIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The separation and purification of flavonoids by column chromatography has the disadvantage of low yield due to irreversible adsorption, and the separation process is very time-consuming and labor-intensive, which is not conducive to the large-scale separation and extraction of flavonoids

Method used

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  • Separating method of icariside I monomer in Korean epimedium leaves
  • Separating method of icariside I monomer in Korean epimedium leaves
  • Separating method of icariside I monomer in Korean epimedium leaves

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] a Measure n-hexane, ethyl acetate, methanol and water in a 1000mL separatory funnel at a volume ratio of 3:7:3:7, shake fully, let stand, and place overnight;

[0029] bUsing the clear upper phase as the stationary phase and the lower phase as the mobile phase, the stationary phase is filled with the helical column at a flow rate of 10mL / min, and then the helical column is rotated at a speed of 1600rpm / min. Pump the mobile phase at a speed of min to make the system reach a hydrodynamic equilibrium;

[0030] c Select the injection volume according to the injection system of high-speed countercurrent chromatography, inject the sample at a solution concentration of 8.0mg / mL, dissolve the crude extract of icariside I in 5mL of the lower phase, and the detector wavelength is 272nm, and the temperature is 40°C.

[0031] d The first large peak is not icariside I, and the second peak is icariside I extracted from Epimedium korean leaves. The color of the solution is fluorescen...

Embodiment 5

[0042] Freeze-dry the solution connected to high-speed countercurrent chromatography at 36-46 minutes, weigh 1.010 mg of powder into a 5 mL volumetric flask, and dissolve in methanol. Take 5uL solution and make high performance liquid chromatogram. The result is as Figure 5 .

[0043] High performance liquid phase conditions: wavelength 272nm, flow rate: 1mL / min, column temperature: 30°C, chromatographic column: Alltima HP C185μm (250×4.6mm)

[0044] Gradient elution:

[0045]

Embodiment 6

[0047] Freeze-dry the solution connected to high-speed countercurrent chromatography at 36-46 minutes, weigh 1.010 mg of powder into a 5 mL volumetric flask, and dissolve in methanol. Mass spectrometry was carried out to the above solution, and the results were as follows: Figure 6 .

[0048] Mass spectrometry conditions: Finnigan MAT LCQ TM The scanning range of the ion trap electrospray mass spectrometer is m / z 0-1000, the spray voltage is 5.0kV, and the temperature of the metal capillary is set at 200°C.

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Abstract

The invention provides a separating method of an icariside I monomer in Korean epimedium leaves, wherein the icariside I monomer is separated from the crude extract of the Korean epimedium leaves by using a high-speed counter current chromatography. The separating method comprises the following steps of: firstly selecting one phase in a pre-balanced two-phase solvent as a fixed phase, filling the fixed phase in a spiral tubular column, then enabling the spiral tubular column to rotate at a high speed at a certain rotating speed, and simultaneously pumping a mobile phase into the column at a certain flow speed. After the fluid dynamic balance of a system is achieved, a sample to be separated is injected into the system, and the components thereof are separated according to the different distribution coefficients of the components in the two phases. Through PLC (Programmable Logic Controller) detection, the purity of icariside I can reach more than 99 percent, and the method is simple and convenient and has high efficiency.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and relates to a separation method for separating icariside I monomers from crude extracts of Epimedium korean leaves by high-speed countercurrent chromatography. Background technique [0002] Epimedium is one of the hot spots of natural medicine research in recent years. The in vivo process of its main component icariin has been fully studied (YE L K, CHEN J M, L IU S H, et al1Pharmacokinetics of icariinin rats[J]1Chin Pharm J (Chinese Journal of Pharmaceutical Sciences), 1999, 34(1): 33-36, but the in vivo process of icariside I has not been reported. From the existing research results, icariside I has good activity at the enzyme level, and is very promising as a therapeutic Effective medication for erectile dysfunction. [0003] Icariside I is one of the in vivo metabolites of icariin, Lenoble et al. (LENOBLE R, R ICHHEIMER S, BA ILEY D T, et al1 Compositions comprising icariside I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 刘忠英刘志强丁一迪
Owner JILIN UNIV