Headspace gas chromatographic analysis is suggested for the determination of acetic and propionic acids in aqueous media. Derivatization of the acids was accomplished by tributyl borate. The derivatization and headspace extraction were coupled into a single step. Analytical characteristics of the suggested technique at the optimized derivatization/headspace extraction conditions were determined. The technique was applied for the analysis of bakery products, ketchup, tomato paste and kefir.