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An improved analytical method for the determination of acrylamide in coffee is described using liquid chromatography coupled to mass spectrometric detection (LC-MS). A variety of instant, ground and laboratory roasted coffee samples were analysed using this method. The sample preparation entails extraction of acrylamide with methanol, purification with Carrez I and II solutions, evaporation and solvent change to water, and clean-up with an Oasis HLB solid-phase extraction (SPE) cartridge. The chromatographic conditions allowed separation of acrylamide and the remaining matrix co-extractives with accurate and precise quantification of acrylamide during MS detection in SIM mode. Recoveries for the spiking levels of 50, 100, 250 and 500 μ g/kg ranged between 99 and 100% with relative standard deviations of less than 2%. The effects of roasting on the formation of acrylamide and colour development were also investigated at 150, 200 and 225° C. Change in the CIE ( Commission Internationale de l’Eclairage) a* colour value was found to show a good correlation with the change in acrylamide. CIE a* and acrylamide data was fitted to a non-linear logarithmic function for the estimation of acrylamide level in coffee. Measured acrylamide levels in commercial roasted coffees compared well with the predicted acrylamide levels from the CIE a* values.