Hydroxymethylfurfural determination in cereal and insect bars by high-performance liquid chromatography-mass spectrometry employing a functionalized mesostructured silica as sorbent in solid-phase extraction.

In this work a new method for the determination of 5-hydroxymethylfurfural (HMF) in cereal and insect bars has been developed and validated. The method consisted of a solid-liquid extraction (SLE) followed by a solid phase extraction (SPE), employing functionalized mesostructured silica as sorbent, and prior to high-performance liquid chromatography coupled to mass spectrometry analysis (HPLC-MS/MS). Mesostructured silica with a large pore (SBA-15-LP) functionalized with aminopropyl- groups (SBA-15-LP-NH), octyl- groups (SBA-15-LP-C8) and bifunctionalized with both organic ligands (SBA-15-LP-C8-NH) were prepared, characterized and tested for this purpose. The optimal conditions showed that the best extraction solvent was water acidified with HCl (pH 1.0) and the best material for SPE was SBA-15-LP-NH (recoveries near 100%). Results were compared with other analogous commercial sorbent (Discovery® DSC-NH), evaluated under similar conditions, and SBA-15-LP-NH sorbent showed better recoveries than the commercial one (62 ± 1%). The developed method was validated and good detection and quantification limits (MDL: 11 µg kgand MQL: 38 µg kg), good precision in terms of repeatability and within-laboratory reproducibility (RSD < 8%) and good accuracy (recoveries between 99-102%) were obtained. The method was successfully applied to the determination of HMF in different samples of cereals and insect bars. In all the samples analysed, high concentrations of HMF (ranging from 336 to 962 mg kg) have been found.