Electrospray–Mass Spectrometry-Guided Targeted Isolation of Indole Alkaloids from Leaves of Catharanthus roseus by Using High-Performance Countercurrent Chromatography
2025
Mahdi Yahyazadeh | Dirk Selmar | Gerold Jerz
Electrospray mass spectrometry off-line profiling monitored the recovery of targeted indole alkaloids from a fortified crude extract of Catharanthus roseus (790 mg) using semi-preparative high-performance countercurrent chromatography (HPCCC) fractionation. Visualization of selected single-ion traces projected the HPCCC molecular weight elution profile. Experimental partition-ratio values KD and peak widths for detected metabolites were determined. Structural characterization of metabolites and co-elution effects were monitored in the scan range m/z 100&ndash:2000. In this study, the biphasic solvent system containing n-hexane&ndash:n-butanol&ndash:water with 0.5% ion-pair reagent trifluoro-acetic acid [1:1:2, v/v/v] was used based on partition ratio :KD-value liquid chromatography&ndash:electrospray ionization&ndash:mass spectrometry (LC-ESI-MS) analysis prediction. The monitoring of target ions resulted in the isolation of six major concentrated indole alkaloids (akuammicine, catharanthine, perivine, vindoline, vindorosine, and 19R-vindolinine), which were fully elucidated by 1D and 2D nuclear magnetic resonance (NMR) spectroscopy.
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