Abstract This paper assesses the use of ion-pair reversed phase-high performance liquid chromatography (RP-HPLC) coupled to a diode array detector (DAD) set at 200nm to determine the acrylamide concentration in cereal-based baby foods. The best sample preparation involved the extraction of acrylamide with 80% methanol in water, defatting with hexane, freezing and cleaning by solid-phase extraction (SPE) with Oasis HLB cartridges. The column used was a Synergi Hydro-RP 80 A with 5mM sodium 1-heptanesulfonate in water/acetonitrile (97/3, v/v) as the mobile phase. The RP-HPLC-DAD method presented a limit of detection (LOD) of 10.0μg/kg, relative standard deviations (RDS) lower than 5.0% and recovery of 106.0%. The proposed method was successfully applied for the determination of acrylamide in four groups of commercial cereal-based baby foods with relatively low levels of acrylamide and including difficult matrices. The acrylamide levels in ready-to-eat and instant baby foods, candy-bars and cakes were 10.8–15.7μg/kg, 19.2–59.9μg/kg, 39.0–61.2μg/kg and 13.3–49.5μg/kg, respectively. The RP-HPLC-DAD method may be used as a convenient, reliable and low-cost alternative system for liquid and gas chromatography coupled to mass spectrometry methods and can be easily adopted by non-specialized analytical laboratories.