In the present work, malondialdehyde (MDA) levels in infant formulae (IF), human and cow milks were monitored using the thiobarbituric acid method (TBA-test) with third derivative spectrophotometry and the derivatization with 2,4-dinitrophenylhydrazine followed by HPLC-DAD analysis. We compared these two detection methods applied to different clean-up procedures in order to evaluate their applicability and improve the recovery yields and the detection limit. Different commercial types of infant formulae, cow and human milks were analysed. The obtained results showed high reproducibility and precision for both analytical methods and evidenced the importance of the correct clean-up procedure. Some of the applied clean-up procedures allowed obtaining quantitative recovery yields and better results, with a good overlapping between the two tested analytical methods. Infant milk formulae showed MDA levels of 380-410 ng g-1, while in human milk 230-340 ng g-1 levels were found. The formula with hydrolyzed proteic fraction (HA), the long chain polyunsaturated fatty acids (LC-PUFA) added formula and two cow milk samples were also analysed, permitting to demonstrate the extensibility and the effectiveness of the adopted methods.