The metabolism of N,N-dimethylformamide in the Sprague-Dawley rat has been reinvestigated using NMR spectroscopy of urine. In particular, through the use of N,N-dimethylformamide-d7 (DMF-d7) and H-2-NMR spectroscopy, the principal metabolites of this compound have been confirmed in a direct manner. The use of inverse-detected two-dimensional H-2-C-13 correlation with C-13 decoupling aided metabolite identification through the provision of C-13 chemical shifts.