The quantum size effects of colloid water-organic media synthesized nanocomposites (CdSe–CdS core–shell) in toluene solution is studied. Femtosecond fluorescence up-conversion spectroscopy is used to establish that quantum dots are characterized by a biexponential decay of luminescence kinetics: the decay times are 1.8 and 26.8 ps for nanoparticles with average sizes of 2 nm and 4.5, and 68 ps for nanoparticles with an average size of 2.9 nm.