Heavy metal contamination of aquatic and marine environments continues to pose serious risks to ecosystems and human health, particularly through bioaccumulation in seafood matrices. In this study, a novel dihydroxyphenyl–nitroaryl azomethine (Schiff base) ligand (TSL1) was synthesized, structurally characterized, and immobilized onto a silica support to obtain a functionalized sorbent for ultrasound-assisted dispersive micro-solid-phase extraction (UA-DMSPE). The developed sorbent was applied for the selective extraction and preconcentration of Hg(II), Cu(II), Pb(II), and Cd(II) ions prior to flame atomic absorption spectrometric determination. Key experimental parameters affecting extraction efficiency were systematically optimized and statistically validated using one-way ANOVA. Under optimized conditions, the proposed UA-DMSPE method exhibited high recoveries (≥90%), low detection limits (0.60–1.50 μg L–1), good precision (RSD < 3.0%), and strong tolerance toward common matrix constituents. The method was successfully applied to seawater and mussel samples, demonstrating reliable performance with controlled matrix effects. Density functional theory (DFT) calculations provided insight into the electronic properties and coordination behavior of TSL1, indicating favorable and comparable affinity toward the investigated metal ions, in agreement with the experimental extraction results. Molecular docking studies provided complementary information on potential biological interaction profiles. In addition, in silico toxicity assessment suggested an acceptable preliminary safety profile for analytical applications, and green analytical metrics confirmed the environmental compatibility of the proposed approach. Overall, the developed TSL1-functionalized silica sorbent combined with UA-DMSPE offers an efficient, selective, and environmentally benign strategy for trace-level determination of toxic metals in complex marine and food-related matrices.
Öncüoğlu et al. (Wed,) studied this question.