The development of new multicomponent nanoparticles is gaining increasing importance due to their specific functional properties, i.e., synthesised new complex concentrated nanoparticles (CCNPs) in the form of powder using ultrasonic spray pyrolysis (USP) and lyophilisation from the initial cast Ag20Pd20Pt20Cu20Ni20 alloy, which was in the function of the material after its catalytic abilities had been exhausted. Hydrometallurgical treatment was used to dissolve the cast alloy, from which the USP precursor was prepared. As a consequence of the incomplete dissolution of the cast alloy and the formation of Pt and Ni complexes, it was found that the complete recycling of the alloy is not possible. A microstructural examination of the synthesised CCNPs showed that round and mostly spherical (not 100%) nanoparticles were formed, with an average diameter of 200 nm. Research has shown that CCNPs belong to the group with medium entropy characteristics. A mechanism for the formation of CCNPs is proposed, based on the thermochemical analysis of element reduction with the help of H2 and based on the mixing enthalpy of binary systems.