Mesoporous Silica Nanoparticles Functionalized with Bisphenol A for Dispersive Solid-Phase Extraction of 3-Chloroaniline from Water Matrices: Material Synthesis and Sorption Optimization.

Aromatic amines such as 3-chloroaniline (3-CA) are toxic, persistent, and environmentally relevant water contaminants. Their reliable determination in aqueous systems has therefore become increasingly important. The monitoring of trace levels of these pollutants in complex water matrices typically necessitates a preconcentration step, most achieved via solid-phase extraction (SPE). However, conventional SPE sorbents often suffer from limited surface reactivity and slow adsorption kinetics, which compromise their performance at ultra-low concentrations. In contrast, nanomaterials offer a promising upgrade due to their high surface area, tunable chemistry, and rapid mass transfer behavior. In this work, mesoporous silica nanoparticles (MSNs) were synthesized via a green sol-gel route from sodium silicate precursor using polyethylene glycol template and then chemically functionalized with bisphenol A (BPA) to produce BPA-MSNs with π-rich and hydrogen-bonding active sites. Characterization using XRD, BET, FTIR, SEM/EDX, and TGA confirmed the successful synthesis and surface modification of the nanosorbent. BPA-MSNs achieved a maximum adsorption capacity of 30.2 mg/g toward 3-CA, fitting Langmuir and Jovanovic isotherm models. Kinetic analysis followed a pseudo-first-order model, indicating physisorption enhanced by π-π stacking and hydrogen bonding. The optimized dispersive SPE (D-SPE) method allowed a low detection limit (LOD = 0.016 mg/L), recovery of 73-85%, and precision below 5.3% RSD in tap, bottled, synthetic municipal wastewater and groundwater samples. The sorbent retained >90% efficiency over five reuse cycles, demonstrating strong potential as a reusable nanosorbent for preconcentration and remediation of aromatic amines in and treatment water analysis.