Matrix-assisted laser desorption/ionization (MALDI) time-of-flight (TOF) mass spectrometry (MS) has been used to identify eight triacylglycerols (TAG) in Vernonia galamensis oil (VO). The TAC include trivernolin, divernoloylstearoylglycerol, divernoloyloleoylglycerol, divernoloyllinoleoylgylcerol, divernoloylpalmitoylglycerol, vernoloyllinoleoylstearoylglycerol, vernoloyllinoleoyloleoylglycerol, and vernoloyldilinoleoylglycerol. Samples for the MALDI/TOF/MS analysis were prepared with alpha-cyano-4-hydroxycinnamic acid (matrix) in an acetonitrile/tetrahydrofuran solvent system. A mol ratio of matrix/VO (44:1) gave reproducible composite spectra, resulting in resolutions greater than 8,000 and signal-to-noise ratios of above 1000 for the most abundant molecular species. 1,3-Dioleoyl-2-stearoylglycerol and 1,2-dioleoyl-3-patmitoylglycerol were used as calibration standards.