We report compound-specific radiocarbon analyses of organic matter in ocean sediments from the northeast Pacific Ocean. Chemical extractions and a preparative capillary gas chromatograph (PCGC) were used to isolate phospholipid fatty acids (PLFA) and n-alkanes from 3 cores collected off the coast of California, USA. Mass of samples for accelerator mass spectrometry (AMS) 14C analysis ranged from 13-100 μg C. PLFA extracted from anaerobic sediments in the Santa Barbara Basin (595 m depth) had modern ∆14C values (-20 to +54‰), indicating bacterial utilization of surface-produced, post-bomb organic matter. Lower ∆14C values were obtained for n-alkanes and PLFA from coast (92 m depth) and continental slope (1866 m) sediments, which reflect sources of old organic matter and bioturbation. We present a brief analysis of the blank carbon introduced to samples during chemical processing and PCGC isolation.