A liquid chromatography triple quadrupole mass spectrometry method was developed and validated for the simultaneous determination of acrylamide and 4-hydroxy-2,5-dimethyl-3(2H)-furanone (HDMF) in baby food. The sample preparation involves acetonitrile-based extraction combined with dispersive primary secondary amine (PSA) cleanup and cation-exchange solid-phase extraction (SPE), which promotes efficient removal of matrix interferences. Analytical selectivity and sensitivity were achieved for the quantification of acrylamide and HDMF in complex matrices such as fruit, cereal and milk-based baby foods; furthermore, adequate linearity (range 10-300μgkg-1) in solvent and matrix-matched calibration curves, and appropriate recoveries (94-110%) and precision (RSD≤10%), under repeatability and within-laboratory reproducibility conditions, were also obtained. Expanded measurement uncertainty was estimated at the 20μgkg-1 level (limit of quantification) on the basis of data obtained from in-house validation, with values of 25.5 and 16.5% for acrylamide and HDMF, respectively. The fitness for purpose of developed method was verified by analyzing 15 commercial baby foods available in the Brazilian market. Acrylamide was detected in one plum-based baby food (35μgkg-1) while HDMF in 67% of the samples analyzed (levels between 25 and 262μgkg-1).
Keywords: 4-hydroxy-2,5-dimethyl-3(2H)-furanone; Acrylamide; Baby food; Food contaminant; LC–MS/MS; Uncertainty estimation.
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