Determination of Acrylamide using Solid-phase Extraction and Gas Chromatography-Mass Spectrometry Selected Ion Monitoring in Roasted Cereal Foods

Abstract

An analytical method has been developed for the determination of acrylamide in cereal-based foods. The method is based on extraction of acrylamide with water, cleaned up through a solid phase extraction (SPE) cartridge, followed by bromination of the acrylamide double bond. The reaction product (2,3-dibromopropionamide) is extracted with ethyl acetate and analyzed by gas chromatography coupled to mass spectrometry (GC/MS) in selected ion monitoring (SIM), employing acrylamide-2,3,3-d3 (AA-d3) as internal standard. The SPE process for sample preconcentration was performed on a commercially available SupelcleanTM Coconut Charcoal cartridge packed with active carbon. In this method, correlation coefficients (R2) of calibration curves appeared to be 0.9997 in the concentration range of 2.5~100 μg/kg. The method detection limit (MDL) and the limit of quantitation (LOQ) of acrylamide were 0.76 μg/kg and 2.32 μg/kg, respectively. The calibration curve showed good linearity above 0.9997 in the ranges of the 2.5~100 μg/kg. For validation purposes, recovery studies were carried out at one concentration levels (10 μg/kg, n=3). The intraday assay accuracy and precision were in the range 104% and 5.6%, respectively, and the interday assay accuracy and precision were in the range 95.8% and 5.3%, respectively. Key words: acrylamide, bromination, GC/MS, SPE, limit of quantitation (LOQ)