Electrospray-Mass Spectrometry-Guided Targeted Isolation of Indole Alkaloids from Leaves of by Using High-Performance Countercurrent Chromatography.

Electrospray mass spectrometry profiling monitored the recovery of targeted indole alkaloids from a fortified crude extract of (790 mg) using semi-preparative (HPCCC) fractionation. Visualization of selected single-ion traces projected the HPCCC molecular weight elution profile. Experimental values and peak widths for detected metabolites were determined. Structural characterization of metabolites and co-elution effects were monitored in the scan range / 100-2000. In this study, the biphasic solvent system containing -hexane--butanol-water with 0.5% ion-pair reagent trifluoro-acetic acid [1:1:2, //] was used based on -value (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 -vindolinine), which were fully elucidated by 1D and 2D (NMR) spectroscopy.