Analysis of antitumor active OSW-1 and its analogues by liquid chromatography coupled with electrospray and atmospheric pressure chemical ionization quadrupole mass spectrometry

Three cholestane glycosides including OSW‐1 with antitumor activity and two new analogues with modified steroidal side chains, thienyl OSW‐1 and silylated thienyl OSW‐1, were synthesized. Analyses were performed using optimized, reversed‐phase liquid chromatography (LC) with electrospray ionization and atmospheric pressure chemical ionization quadrupole mass spectrometry (MS). The ionization mode and polarity, cone voltage, and chromatographic conditions were evaluated. The optimum LC/MS conditions to obtain valuable ions, indispensable for identifying the structures, are described. The key fragmentation pathways, which will be useful for confirming the detailed structures of steroidal glycosides, are also proposed. Copyright © 2007 John Wiley & Sons, Ltd.