As end products of xenobiotic metabolism via glutathione conjugation, mercapturic acids (MCAs) can be used as markers to indicate exposure to allylic compounds as well as the rate and efficiency of their excretion. In addition, the formation of certain MCAs indicates metabolism via the known toxin acrolein, a strong electrophile. High-resolution 1H NMR spectroscopy has been employed to quantitatively measure the presence of MCAs in the urine of Sprague-Dawley rats, collected in the 8 h following 25 and 50 mgkg(-1) i.p. doses of allyl formate (AF), a model toxin. 3-Hydroxypropylmercapturic acid (HPMA) was found to be the only 1H NMR-observable MCA excreted in the urine, exhibiting a percentage recovery of approximately 20% at the 25 mgkg(-1) dose level, and approximately 30% at the 50 mgkg(-1) dose level.