Trace level determination of acrylamide in cereal-based foods by gas chromatography–mass spectrometry

A quantitative method has been developed for the determination of trace levels (<50 μg/kg) of acrylamide in cereal-based foods. The method is based on extraction of acrylamide with water, acidification and purification with Carrez I and II solutions, followed by bromination of the acrylamide double bond. The reaction product (2,3-dibromopropionamide) is extracted with ethyl acetate/hexane (4:1, v/v), dried over sodium sulfate, and cleaned up through a Florisil column. The derivative is then converted to 2-bromopropenamide by dehydrobromination with triethylamine and analyzed by gas chromatography coupled to mass spectrometry (GC–MS), employing (13C3)acrylamide as internal standard. In-house validation data for commercial and experimental cereal products showed good precision of the method, with repeatability and intermediate reproducibility relative standard deviations below 10%. The limit of detection and limit of quantitation are estimated at 2 and 5 μg/kg, respectively, and recoveries of acrylamide from samples spiked at levels of 5–500 μg/kg ranged between 93 and 104% after correction of analyte loss by the internal standard. Finally, a comparative test organized with two independent laboratories provided additional confidence in the good performance of the method, particularly at very low concentration levels.