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Abstract
A method for the determination of acrylamide in roasted coffee was subjected to method validation by collaborative trial. The aim was to extend the scope of a method already standardized for the determination of acrylamide in bakery and potato products to include roasted coffee. Modifications of the already standardized method were therefore kept to a minimum. The method was based on aqueous extraction of the roasted coffee matrix and solid-phase extraction (SPE) clean-up followed by isotope dilution high-performance liquid chromatography with tandem mass spectrometric detection (LC-MS/MS). The test portion of the sample was spiked with stable isotope-labelled acrylamide and extracted on a mechanical shaker with n-hexane and water for 1 h. The sample extract was centrifuged, the organic phase discarded, and a portion of the aqueous extract further cleaned-up by SPE on an Isolute Multimode cartridge followed by a second clean-up step on an Isolute ENV + cartridge. The volume of the acrylamide-containing fraction eluted from the second SPE column was reduced by evaporation and analysed by LC-MS/MS. Three coffee samples and one aqueous acrylamide standard solution were sent to eleven laboratories from eight European Union Member States. All samples were sent as blind duplicates. Based on the reported results, the relative standard deviations for reproducibility (RSDR) were 11.5% at a level of 160 µg kg−1, 10.1% at a level of 263 µg kg−1, and 9.6% at a level of 585 µg kg−1. The values for repeatability (RSDr) in those materials ranged from 1.0% to 3.5%. The method performance parameters satisfied internationally accepted criteria. Hence, the method would be suitable for the enforcement of regulatory limits.
Acknowledgements
The organizers are very grateful for the support given by Nestlé. They would like to thank in particular Dr Richard Stadler for the preparation and supply of suitable test materials. The authors would like to thank NMKL for technical support in the organization of the study. The authors would also like to thank following institutes for participating in the study: Eurofins Analytik GmbH, Hamburg, Germany; Finnish Food Safety Authority EVIRA, Helsinki, Finland; ICT Prague, Prague, Czech Republic; Laboratoire Départemental de la Sarthe, Le Mans, France; Landesuntersuchungsanstalt Sachsen, Dresden, Germany; Livsmedelsverket, Uppsala, Sweden; Department of Food Chemistry, National Food Institute, Søborg, Denmark; Unilever Italia–Laboratorio Centrale, Cisterna di Latina, Italy; and VWA Region South, Eindhoven, the Netherlands.