An effecient gas chromatographic method is described to be used routinely for the rapid profiling and identification of biochemically important organic acids. It involves the solid-phase extraction of organic acids from aqueous samples using Chromosorb P as the solid sorbent and diethyl ether as the eluting solvent, with subsequent triethylamine treatment. The resulting triethylammonium salts of acids were directly converted to volatile tert-butyldimethylsiyl derivatives, which were simultaneously analyzed by two capillary columns of different polarity, DB-5 and DB-1701, under the identical temperature programming condition. The retention index (RI) and area ratio (AR) values of each peak measured on DB-5 and DB-1701 enabled rapid identification of acids by computer RI library search and AR comparison. The application of the present method to the organic acid profiling of various complex samples is demonstrated.