A sample preparation method based on modified Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) with aluminum oxide (Al 2 O 3 ) as dispersive solid phase extraction (dSPE) material and high performance liquid chromatography–linear trap quadruple-Orbitrap-mass spectrometry (HPLC LTQ-Orbitrap MS) was established. The performance of two analytical columns namely Kinetex C18 and Rezex ROA-organic acid was compared for acrylamide separation. The method was validated in term of matrix effect, linear range (standard addition method), limit of detection (LOD), limit of quantification (LOQ), precision (RSD%) and recovery. Good linearity (r 2 >0.9979) was achieved using standard addition method in the concentration range 0–200μgkg −1 . The LOD is in the range from 2.91 to 4.04μgkg −1 and 1.50 to 3.94μgkg −1 for C18 and ROA columns, respectively. The precision of the method was ⩽7.3% and 5.6% for C18 and ROA columns, respectively. Recoveries of acrylamide ranging from 90% to 97%, (n=3) were obtained. The proposed Al 2 O 3 dSPE method was successfully applied to the analysis of acrylamide in real food samples.