Acrylamide represents toxic compound presence of which in heat processed foodstuffs has been proven only recently. This chemical is of a great health concern since it is classified as a human carcinogen by the International Agency for Research on Cancer (IARC). Relatively high amounts of acrylamide have been found mainly in starch rich foods such as potato chips, French fries, roast potatoes, breakfast cereals and crisp bread. Concentrations of this hazardous substance in certain food products may reach up to several mg/kg, depending on the type of raw commodity and the way of its processing. Changes of acrylamide levels in potato chips during frying process were monitored in our study. New analytical procedure employing gas chromatography coupled with high resolution time of flight mass spectrometry (GC/HRTOF-MS) was developed for this purpose. The major factors that affect acrylamide levels in chips such as asparagine and reducing sugars (the main precursors of acrylamide) content in raw potatoes as well as the processing conditions setting (time and temperature) were monitored. Under experimental conditions we used, rapid formation of acrylamide occurred after 150 s, temperature of oil bath was approx. 140°C at that time. In overfried chips the levels of acrylamide exceeded 10 mg/kg.