A microchip CE-based method for the quantification of the thiols mercaptoethanoic acid (MAA) and 2-mercaptopropionic acid (2-MPA) in depilatory cream and cold wave lotions was developed. The thiols were first derivatized with the fluorogenic reagent ammonium-7-fluorobenzo-2-oxa-1,3-diazole-4-sulfonate (SBD-F). The derivatives were separated within only 20 s by microchip CE and detected by their fluorescence. Conventional CE with diode array detection and LC with fluorescence detection were used for validation. The internal standard 3-mercaptopropionic acid (3-MPA) provided RSDs of multiple injections of only 4% or less for the MCE approach. LOD is 2 mu M, LOQ 6 mu M, and the linear range comprises nearly three decades of concentration starting at the LOQ.