Electrospray–Mass Spectrometry-Guided Targeted Isolation of Indole Alkaloids from Leaves of Catharanthus roseus by Using High-Performance Countercurrent Chromatography
Mahdi Yahyazadeh, Dirk Selmar, Gerold Jerz
TL;DR
Scientists isolated six major indole alkaloids from Catharanthus roseus leaves using a mass spectrometry-guided chromatography method.
Contribution
A novel electrospray-mass spectrometry guided HPCCC method was developed for targeted isolation of indole alkaloids.
Findings
Six indole alkaloids were successfully isolated and identified using NMR spectroscopy.
The biphasic solvent system with trifluoroacetic acid improved separation efficiency.
Electrospray mass spectrometry enabled real-time monitoring of metabolite recovery.
Abstract
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 100–2000. In this study, the biphasic solvent system containing n-hexane–n-butanol–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–electrospray ionization–mass spectrometry (LC-ESI-MS) analysis prediction. The monitoring of target ions resulted in the…
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Taxonomy
TopicsChromatography in Natural Products · Natural product bioactivities and synthesis · Pharmacological Effects of Natural Compounds