Al 3+ -Mg 2+ mixed oxides were prepared by coprecipitation and characterized with scanning electron microscopy (SEM), energy dispersive Xray fluorescence (EDXRF), temperature programmed desorption of CO 2 (CO 2 -TPD), and N 2 adsorption/desorption isotherms (BET and BJH methods). By increasing the MgO concentration up to 31.8% (w/w), X-ray diffraction (XRD) measurements suggested an incipient magnesium aluminate spinel (MgAl 2 O 4 ) phase. However, the spinel crystalline structure was obtained only after calcination at 950 °C. These materials were tested as catalysts in the propanolysis reaction of methyl paraoxon. This reaction in the presence of the more efficient incipient MgAl 2 O 4 spinel is of the order of 2.5 × 10 5 -fold faster than the spontaneous propanolysis reaction and results in the formation of a product that is structurally related to a family of flame retardants. The different products of propanolysis and hydrolysis were identified by electrospray ionization mass spectrometry (ESI(+)-MS), ESI(+)-MS/MS) and liquid chromatography mass spectrometry (LC-MS/MS).