An improved analytical method for the rapid, reliable, and sensitive determination of hydroxymethylfurfural (HIVIF) in baby foods is described. It entailed aqueous extraction from food matrix with simultaneous clarification using Carrez I and II reagents, solid-phase extraction cleanup using Oasis HLB, and analysis by liquid chromatography-mass spectrometry. A narrow-bore column allowed fast chromatographic separation with good resolution of HMF and matrix coextractives. In positive atmospheric pressure chemical ionization conditions, precursor and compound-specific ions were sensitively detected in selected ion monitoring mode. Sample preparation with efficient cleanup followed by fast chromatographic analysis allowed the analysis to be completed in < 20 min. Recovery ranged between 91.8 and 94.7% for spiking levels of 0.25, 1.0, and 5.0 mg/kg HIVIF in cereal-based baby foods. The method was shown to be successful when using liquid chromatography coupled to ultraviolet detection at 285 nm.