A method of gas chromatography with nitrogen chemiluminescence detection and using standard addition is described for the determination of acrylamide in heat-processed foods. Using a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) sample preparation method removes the acrylamide precursors completely, and the risk of overestimating acrylamide concentration due to additional analyte formation in the hot gas chromatograph inlet is also avoided. Sample preparation is rapid and inexpensive. A Deans switch device is utilized to heart-cut acrylamide and to prevent interferences from the solvent and matrix from reaching the detector. The pre-column is backflushed at high temperature to maintain a clean baseline and shorten the cycle time compared to baking out the column. Quantitation using standard addition is employed for compensation of potential variability in the acrylamide extraction efficiency in acetonitrile. The limit of detection and the limit of the quantification obtained for this method are 27 and 81 μg/kg, respectively, in food samples (equivalent to 3.5 and 10.6 μg/L in acetonitrile, respectively), and the linear range is 76-9697 μg/kg in food samples (equivalent to 10-1280 μg/L in acetonitrile) with an R(2) value of 0.9999.