Development, validation and application of an SFC-ESI-QqQ-MS/MS method for simultaneous analysis of malondialdehyde and typical α,β-unsaturated aldehydes in edible oils and oil-containing foods

A novel supercritical fluid chromatography coupled with tandem mass spectrometry (SFC-ESI-QqQ-MS/MS) method was developed for simultaneous quantification of malondialdehyde (MDA) and seven α,β-unsaturated aldehydes (α,β-UAs) in edible oils and oil-containing foods. Combining DNPH derivatization with one-step extraction, the method achieved exceptional performance: linearity (R² ≥ 0.9995), rapid analysis (16 min/sample), recoveries (85.84–106.71 %), and precision (RSD < 7.86 %), with LOD/LOQ at 0.05–0.60/0.15–1.80 μg/kg. This validated technique was subsequently applied to monitor the formation of MDA and α,β-UAs during the heating of eight edible oils, revealing concentration dependencies on fatty acid composition and heating duration. Furthermore, the levels of MDA and seven α,β-UAs in 29 oil-containing foods commonly consumed in China were determined using the developed method, with concentrations ranging from 2.65 to 326.79 μg/kg and 15.67–770.71 μg/kg, respectively. As the first SFC-based approach for comprehensive aldehyde profiling, this method enables precise monitoring of lipid oxidation pathways and supports quality control innovations in the food industry.