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Preparation of senkyunolide I by reversed-phase high performance liquid chromatography

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Abstract

A method for the isolation of senkyunolide I from Chuanxiong with reversed-phase preparative high performance liquid chromatography (HPLC) is described. After 95% ethanol extract was obtained with solvent extraction and normal-phase silica column separation, a fraction containing senkyunolide I was acquired and subjected to preparative HPLC for the isolation of target component. In the experiment a solvent system consisting of methanol-0.05 mol/L NH4Ac aqueous solution was found effective to eliminate the interference of ferulic acid that was the major compound in the sample. Senkyunolide I and ferulic acid were separated completely by using a stepwise gradient solvent system of 10% methanol in 10 min, and 60% methanol in 10 - 40 min. The subfractions were collected and subjected to an open MCI gel CHP-20P column for desalination respectively. Senkyunolide I was obtained and the structure was identified by mass spectrometry (MS) and nuclear magnetic resonance (NMR). This method is effective and reliable for the preparation of senkyunolide I from Chuanxiong.

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... A RP-preparative-HPLC method for the isolation of compound 30 from CX was described by Zhang et al. [113]. Because it is difficult for traditional methods including semi-preparative HPLC and CE to avoid the adsorption on the solid phase, they are not very suitable for the separation of compounds 19 and/or 20 and their analogues. ...
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