According to the classification of the International Agency for Research on Cancer (IARC), acrylamide is a compound in “probably carcinogenic for humans” class (Group 2A). Acrylamide is produced through the reactions induced by heating food within the amino group asparagine and the carbonyl group decreasing sugars along side the thermal treatment of initial Maillard reaction products. The purpose of this work is to present and enhance an innovative technique for acrylamide deter-mination in potato chips through CdTe surface-functionalized quantum dots as a reagent for the determination of acrylamide by fluorescence spectroscopy. For this purpose, fluorescence emission spectroscopy was used instead of conventional HPLC/GC methods and data of merit of the suggested technique were assessed. The acrylamide quantity in 4 potato chips specimens, prepared from a local market in Tehran, was determined through utilizing the suggested process. Effective parameters in the process were optimized using the one-factor-at-a-time (OFAT) technique. The optimal quantities of effective parameters such as pH absorption, temperature, and emission wavelength were determined. Comparison between two methods, namely HPLC and fluorescence spectroscopy, was also described. The merit figures for the suggested approach were within the idyllic range. The developed methods showed a high correlation coefficient (0.991), high sensitivity, and repeatability. Results of the fluorescence emission spectroscopy and its comparison with Mass/HPLC revealed the high reliability and performance of the recommended method as an efficient, simple, and quick procedure with reduced cost and time in the determination of acrylamide in potato chip specimens.