In this study, a bio-derived precipitating agent/ligand, palm kernel oil, has been used as an alternative route for the green synthesis of nanoparticles of Fe-doped Co3O4 via the co-precipitation reaction. The palm oil was extracted from dried palm kernel seeds by crushing, squeezing and filtration. The reaction of the palm kernel oil with potassium hydroxide, under reflux, yielded a solution containing a mixture of potassium carboxylate and excess hydroxide ions, irrespective of the length of saponification. The as-obtained solution reacts with an aqueous solution containing iron and cobalt ions to yield the desired metallo-organic precursor, iron cobalt carboxylate. Characterization of the precursors by IR and gas chromatography (GC) attests to the presence of carboxylate fatty acids in good agreement with the proportion contained in the oil, and ICP confirms that the metallic ratios are in the proportion used during the synthesis. Analysis of the products thermally decomposed between 400 °C and 600 °C by XRD, EDX, TEM and ToF-SIMS, established that cobalt iron oxide nanoparticles (Co(1−x)Fex)3O4 were obtained for x ≤ 0.2 and a nanocomposite material (Co(1−x)Fex)3O4/Fe3O4 for x ≥ 0.2, with sizes between 22 and 9 nm. ToF-SIMS and XRD provided direct evidence of the progressive substitution of cobalt by iron in the Co3O4 crystal structure for x ≤ 0.2.