AbstractThis study presents a detailed investigation of the structural and surface modifications of Fe3O4 nanoparticles (NPs). Fourier Transform Infrared (FTIR) spectroscopy was utilized to analyze the distinct characteristic peaks of Fe3O4 NPs and their subsequent modifications with stearic acid (ST) layers. The FTIR analysis revealed characteristic peaks at 580 cm−1, and 441 cm−1, corresponding to the Fe‐O stretching vibrations of the bulk Fe3O4 NPs. The successful loading of stearic acid onto the Fe3O4 NPs was confirmed by the appearance of new peaks at 1413 cm−1 and 2908 cm−1, indicative of the asymmetric CH2 stretch and CH3 umbrella vibration modes of stearic acid. UV‐Vis spectroscopy further corroborated the efficient loading of tetracycline and ibuprofen onto Fe3O4/DST nanoparticles, as evidenced by changes in absorption spectra. N2 adsorption‐desorption isotherms illustrated the presence of micro and meso pores on the surface of Fe3O4 NPs, with alterations in pore volume and diameter post‐surface modification and drug loading. Evaluation of magnetic properties indicated a reduction in saturation magnetization after surface modification and drug loading, attributed to changes in homogeneity and surface moments. Differential Reflectance Spectroscopy (DRS) and Raman spectroscopy elucidated distinctive peaks and shifts in spectra, confirming the composition and structural changes in drug‐loaded nanofibers.