Liquid chromatography (LC) is frequently employed to study the multiple products of chemical reactions. Often, the amounts and identities of the products must be determined. Unfortunately, LC does not facilitate the identification of the products nearly as well as their quantitation. Not only are the detectors used in LC rather noninformative, but the compounds usually are eluted from the columns in matrices nonconducive to further manipulation, i.e., water-organic mixtures. The present study demonstrates that solid-phase extraction can be effectively used to quantitatively isolate individual compounds collected in the effluent from an LC column. By passing the mobilephase fraction through a correctly chosen adsorbent, the problems of solvent concentration and water removal can be easily solved. The separated compounds can then be isolated from the solid-phase extraction cartridge in 100 to 200 μl of organic solvent. At that point, performing a nuclear magnetic resonance, mass, or Fourier transform infrared spectral study is possible. The use of solid-phase extraction will be discussed with application to the identification of the compounds in the mixture produced in the oxidation of a model carbamate species, methylene diisocyanate bis methyl carbamate.