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 microg/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 microg/kg, respectively, and recoveries of acrylamide from samples spiked at levels of 5-500 microg/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.
Pittet
Alain
A
Nestlé Research Center, Nestec Ltd., Vers-chez-les-Blanc, PO Box 44, CH-1000 Lausanne 26, Switzerland. alain.pittet@rdls.nestle.com
Périsset
Adrienne
A
Oberson
Jean-Marie
JM
D020106:Acrylamide / Q000032:analysis*; D002138:Calibration; D002523:Edible Grain / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D020106:Acrylamide