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Abstract Silica nanoparticles (SiNPs) are promising drug delivery nanocarriers due to their tunable size, porous structure, and surface properties. This study compares two synthesis methods: (i) a low‐temperature aqueous sol–gel process yielding SiNPs of 500–700 nm, and (ii) a water‐in‐oil (W/O) microemulsion using either CTAB or TX‐100 surfactants. Surfactant selection significantly affected nanoparticle size, stability, and dispersity. Characterization by dynamic light scattering (DLS), scanning electron microscopy (SEM), X‐ray diffraction (XRD), Brunauer–Emmett–Teller (BET), solid‐state nuclear magnetic resonance spectroscopy (ssNMR), X‐ray photoelectron spectroscopy (XPS), and photoluminescence analysis (PL) confirmed successful synthesis. The TX‐100‐mediated microemulsion method proved particularly effective in achieving highly stable, reproducible, and monodisperse SiNPs, with a size limit of approximately 100 nm, making them ideal candidates for drug encapsulation. Procaine (PRC) incorporation demonstrated the role of reverse micelle dynamics and surfactant‐stabilized interfaces in enhancing encapsulation efficiency. This work highlights the critical role of surfactant and medium selection in SiNPs synthesis, demonstrating their impact on nanoparticle stability, dispersity, and drug loading efficiency. The TX‐100‐mediated microemulsion technique emerges as a superior approach for producing stable, monodisperse SiNPs, advancing the design of nanocarriers for PRC drug delivery applications.