peer reviewed ; Acrylamide (CH2=CHCONH2), a neurotoxic and potentially carcinogenic substance for human health, is in the glare of the spotlights for a few years. This is mostly due to the fact that acrylamide was found worldwide in various heated foodstuffs. Levels reported in the literature vary from 25 to 2000 ìg/kg and potato products are considered as the most contaminated. A possible pathway of synthesis of acrylamide is the Maillard reaction between reducing sugars and the amino acid asparagine. The aim of this study was to develop a liquid chromatography/mass spectrometry method to analyse as quickly as possible acrylamide in a variety of Belgian food samples such as potatoes, French fries, crisp bread, coffee, corn-flakes, etc. The sample preparation consisted in a liquid/liquid extraction, a centrifugation, followed by purification with Solid Phase Extraction (SPE). The instruments used were a Waters 2690 Alliance HPLC system coupled to a Micro-mass Quattro Ultima Platinum triple-quadrupole mass spectrometer. The analysis was performed in MS/MS mode using isotopic dilution technique for quantification. An internal 13C3 labelled standard was added prior to extraction. Quantifica-tion in MS/MS mode was calculated by reconstructing the ion current with the most abundant daughter ions for native and 13C labelled standard (ions of m/z 55 and 58).