International Journal of Environmental Analytical Chemistry, 2026 (SCI-Expanded, Scopus)
In this study, a novel hierarchical hybrid composite, Zn–Al layered double hydroxide integrated with MIL-53(Al) metal–organic framework (Zn–Al-LDH@MIL-53(Al)), was fabricated and utilised as an efficient adsorbent for the micro-solid phase extraction (µ-SPE) of atrazine from wastewater samples. The successful integration of the unique properties of both components, combining the vast porosity and abundant active sites of MIL-53(Al) with the hydrophilic nature of LDH, was confirmed by XRD, FT-IR, FE-SEM, and STEM analyses. Under the optimised experimental conditions (pH 5.0, 75 mg adsorbent dosage, and 5 min extraction time), the method demonstrated excellent analytical performance coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD). The method exhibited a wide linear range of 5–250 μg L−1 (R2 = 0.9925) and a low limit of detection (LOD) of 0.20 μg L−1. Despite the complex matrix of wastewater, which contains various organic and inorganic interferences, the proposed adsorbent maintained high selectivity for the target analytes and relative recoveries ranging from 94% to 102%, demonstrating its exceptional resistance to matrix interferences. Combining rapid extraction kinetics, high sensitivity, and operational simplicity, the Zn–Al-LDH@MIL-53(Al)-based µ-SPE strategy offers a promising and sustainable platform for the trace-level determination of organic pollutants in environmental monitoring.