Fast Detection of 5-Hydroxymethylfurfural in Dulce de Leche by SPE-LC–MS

Abstract This research paper investigates the use of 5-hydroxymethylfurfural (5-HMF) as marker for the heat treatment of spreadable dairy creams ( dulce de leche , DL). The proposed method applies solid-phase extraction (SPE) with final analysis by liquid chromatography coupled with high-resolution mass spectrometry (SPE-LC–MS). The method was successfully applied to analyze spreadable dairy creams prepared by hot melt extrusion using different heating temperatures from 100 to 130 °C. The concentrations of 5-HMF correlated linearly with the applied temperatures, with a signal response in the range from 0.5 to 100 μM ( R 2 = 0.9997). The limit of detection (LOD) was 1.54 ± 0.03 µM with a precision of 1.77%. The results were compared with the analysis of 5-HMF in spreadable dairy creams using reference methods for the determination of 5-HMF in milk products. These methods mainly employed acid digestion and derivatization as pre-processing steps and determined 5-HMF spectrophotometrically and via HPLC–UV. These resulted in higher LOD (2.99 and 2.01 μΜ) and less precision (4.44 and 2.09%) compared to the proposed method. Furthermore, the proposed pre-processing procedure was faster by omitting the acid digestion and derivatization steps and by employing SPE.