Current approaches for identifying and quantitating surfactants in various product matrices require the use of wet chemical, chromatographic, and spectroscopic techniques. The primary objective of this work is to replace current multiple-technique approaches for identifying surfactants and quantitating their homologue distribution with a single rapid technique. To meet this objective, a simple preparation procedure has been developed to prepare consumer product samples for subsequent analysis by ion-spray mass spectrometry. Quantitation of linear alkylbenzene sulfonates in detergents with this technique is demonstrated.