Conditions for the determination of acrylamide (AA) after derivatisation with 2-mercaptobenzoic acid by capillary zone electrophoresis were established. A derivatisation reagent-acrylamide ratio of 35:1 was selected as optimum and the reagent excess was not removed as it did not affect the determination of acrylamide by CZE. The best separation was achieved using a 40 mM phosphate buffer at pH 8.0, working at 25 kV in un-coated fused silica capillaries. Linear calibration curves over the range studied (0.3-100 mu g mL(-1)), the limit of detection (0.07 mu g mL(-1)), and both run-to-run (RSD values of 5.8 and 2.2% for concentration at low and medium concentration levels, respectively) and day-to-day precisions (up to 11.2 and 6.7% at low and medium concentration levels, respectively) were established. Finally, the applicability of the CZE proposed methodology was demonstrated by analyzing levels of acrylamide present in different foodstuff products such as home made french fries, breakfast cereals and biscuits. (c) 2005 Elsevier B.V. All rights reserved.