Photoluminescent nanoparticles (NPs) are of specific interest for biomedical applications, bioimaging, and cell tracking. Here, we report on the synthesis of europium(III)-doped MgAl2O4 spinel NPs by the CO2 laser co-vaporization of a homogeneous raw powder mixture consisting of micrometer-sized MgAl2O4 and Eu2O3 (2 and 4 mol%, respectively). The resulting NPs are spherically shaped, show a narrow size distribution (mean diameter: similar to 30 nm), and are well dispersed. The as-prepared NPs are highly crystalline and consist of MgAl2O4 with small amounts of the secondary phases MgO (similar to 10 mass %) and Eu2O3 (<0.5 mass%). The photoluminescence spectra of the doped spinel nanopowders show an intense red emission (lambda(em) = 615 nm) resulting from the D-5(0) -> F-7(2) transition with a maximum intensity at an excitation wavelength of 470 nm.