Trace concentrations of small soluble epoxides are suspected byproducts of drinking water ozonation. However, adequate characterization of epoxide formation is currently limited by the lack of suitable analytical methods to target these chemicals in dilute, but complex aqueous solutions. One potential approach is presented here based on aqueous-phase aminolysis. The method also employs solid-phase extraction, silylation of the solvent extract, and analysis by gas chromatography-mass spectrometry. This approach is demonstrated to be effective for the selective analysis of the epoxides 1,2-epoxybutane, epichlorohydrin, and epifluorohydrin in water with optimized method detection limits of 5-10 ng/L.