Two-dimensional proton-proton correlated NMR spectra of concentrated urine from a subject who had ingested a 1-g dose of acetaminophen are reported. These "maps" provide a considerable simplification of the spectrum in comparison with conventional one-dimensional NMR spectra. In the present case, peaks for all the major acetaminophen metabolites, including the L-cysteinyl conjugate, can be unambiguously assigned.