Simultaneous Determination of Acrylamide and 5-Hydroxymethylfurfural in Heat-Processed Foods Employing Enhanced Matrix Removal-Lipid as a New Dispersive Solid-Phase Extraction Sorbent Followed by Liquid Chromatography-Tandem Mass Spectrometry

The goal of this study was to develop a method for simultaneous determination of acrylamide (AA) and 5-hydroxymethylfurfural (5-HMF) in heat-processed foods by liquid chromatography-tandem mass spectrometry analysis. Several cleanup methods for the quick, easy, cheap, effective, rugged, and safe (QuEChERS) protocol were investigated and compared: (a) dispersive solid-phase extraction (d-SPE) with Enhanced Matrix Removal-Lipid (EMR-Lipid), (b) d-SPE with primary secondary amine, (c) without the cleanup step, and (d) cleanup with n-hexane. It is the first time that EMR-Lipid sorbent has been used as a d-SPE material to detect AA and 5-HMF in heat-processed foods, and among the four cleanup methods, the EMR-Lipid method provided the best cleanup of co-extracted matrix interferences and the highest extraction efficiency. Validation experiments were carried out for the method using EMR-Lipid as the d-SPE sorbent. Excellent linearity ( R2 > 0.999) was achieved, and the limits of detection (LODs) of AA and 5-HMF were 2.5 and 12.5 μg/kg, respectively. The recoveries of AA and 5-HMF levels obtained were in the ranges of 87.3-103.3 and 83.2-104.3%, with precision [relative standard deviations (RSDs)] of 1.2-6.8 and 1.4-7.4% ( n = 3), respectively. The method is accurate and reliable and was successfully applied to analyze the AA and 5-HMF in eight categories of Chinese heat-processed foods.