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A simple and rapid method using liquid chromatography coupled with diode array detection (LC-DAD) was developed for the determination of acrylamide in starch-based foods. The method entails extraction of acrylamide with 75% (v/v) methanol in water, concentration, and cleanup with an Oasis HLB solid-phase extraction (SPE) cartridge. The chromatographic separations were performed on an HC-75H(+) column with 5 mM sulfuric acid as the mobile phase, and acrylamide was well resolved from co-extractives in the shape of a protonated cation. The final extract was analyzed by LC-DAD for quantification and the limit of detection was estimated to be 30 mu g/kg based on the signal-to-noise ratio of 3 recorded at 200 nm. The method was applied for the determination of acrylamide in spiked food samples without native acrylamide yielding recoveries between 92.5% and 104.0%. Finally, commercial samples of potato chips, cookies, and some Chinese fried foods were analyzed to assess applicability of the method to acrylamide, giving results similar with those reported in the literature. (C) 2007 Elsevier Inc. All rights reserved.