This study describes the results of the simultaneous detection and quantitation of morphine, 6-acetylmorphine, and cocaine in toenail and hair samples obtained from 18 forensic autopsies of drug abusers who had died in various manners. After external decontamination, each specimen was submitted to hot acid hydrolysis (1 mL of HCl 37%) in the presence of internal standards, followed by liquid-liquid and solid-phase extraction techniques. The extracts were then derivatized with propionic anhydride and analyzed by gas chromatography-mass spectrometry, operating in the selected ion monitoring mode. The limit of quantitation for all analytes was 0.5 ng on column. Results showed that both cocaine and morphine are more concentrated in toenails than in hair. Mean concentrations were 0.99 ng/mg (toenails) versus 0.48 ng/mg (hair) for cocaine and 1.27 ng/mg (toenails) versus 0.79 ng/mg (hair) for morphine. Distribution of 6-acetylmorphine showed no significant variations between the two (mean concentrations 0.46 ng/mg vs. 0.50 ng/mg in hair).