Acrylamide (AA) is a well-studied industrial toxicant; however, recent findings of AA at ppm levels in cooked starchy foods have refocused attention on the potential for neurotoxicity, germ cell mutagenicity, and carcinogenicity from AA. Oxidative metabolism of AA to glycidamide (GA) in experimental animals has previously been linked with many toxic effects of AA exposure. We report a new sensitive and selective analytical method, based on LC with electrospray tandem mass spectrometry, for the quantification of AA and GA in serum and its application to a preliminary toxicokinetic evaluation of AA and GA in adult B6C3F(1) mice following oral administration of AA.