Acrylamide is a suspected carcinogen required to be listed on food labels in California and products commercially traded within the European Union. Foods like potato products, coffee, crackers, etc., are produced at elevated temperatures, which provide conditions that convert the amino acids, Asn, Arg and Lys, in combination with reducing sugars, into acrylamide via the Maillard reaction. Current methods to detect and quantitate acrylamide in food are costly, time consuming, and dependent on expensive scientific instrumentation (i.e., Liquid Chromatography-Mass Spectrometry (LC-MS)). Near Infrared (NIR) spectroscopy is inexpensive, fast, easy to use, and applicable to acrylamide detection. The purpose of this study is to establish a standard method for quantitative detection of acrylamide in food using NIR spectroscopy. Acrylamide extractions from potato products will be monitored by NIR and the results validated using LC-MS. A standard acrylamide curve, in solution with a coefficient of determination (R2) value of 0.966 and a standard curve in solid matrix with an R2 value of 0.914 was established. A standard matrix spike will be obtained from acrylamide content measured in actual coffee and potato products to determine acrylamide content using NIR coupled with Partial Least Squares computational software. The NIR method will provide a fast and economical alternative to traditional food safety and security industry standards.