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Pulsed laser ablation in liquids was utilized to prepare NiFe₂O₄ (NFO) and CoFe₂O₄ (CFO) nanoparticles from ceramic targets. The morphology, crystallinity, composition, and particle size distribution of the colloids were investigated. We were able to identify decomposition products formed during the laser ablation process in water. Attempts to fractionate the nanoparticles using the high-gradient magnetic separation method were performed. The nanoparticles with crystallite sizes in the range of 5–100 nm possess superparamagnetic behavior and approximately 20 Am²/kg magnetization at room temperature. Their ability to absorb light in the visible range makes them potential candidates for catalysis applications in chemical reactions and in biomedicine.