Traditional microextraction methods, such as micro-solid-phase extraction ( μ SPE) and conventional fiber-based SPME, suffer from complexity, long extraction times, and insufficient surface area, resulting in poor sensitivity for trace-level pesticide analysis. To address these limitations, for the first time, MIL-53(Al) metal-organic framework as a thin-film (TF) was synthesized directly on an aluminum thin sheet for the determination of three insecticides (thiacloprid, imidacloprid, and acetamiprid). To enhance the adsorbent amount, a 25*35 mm of MIL- 53(Al)/Al thin sheet was rolled and placed in a pipette tip. The present approach offers significant advantages: enhanced surface area and rapid extraction in 15 min, and ease of use without the risk of clogging and back pressure in pipette tip μ SPE. Response surface methodology optimization established optimal conditions at pH 6.5 and 50.0 mL sample volume. The TF-MOF-HPLC method achieved superior analytical performance with detection limits of 0.3–1.5 μ and 5.0–450.0 μ g/L and quantification limits of 1.0–5.0 μ g/L. Linear ranges of 1.0–300.0, 3.0–350.0, g/L were obtained for acetamiprid, thiacloprid, and imidacloprid, respectively (R 2 >0.95). The target insecticides were subsequently extracted from cucumber samples by ultrasonic extraction using only 1.4 mL of acetonitrile and pre-concentrated using the TF-MOF microextraction method. Method validation in water, cucumber, and juice samples demonstrated excellent recovery rates (86.0–100.7%) with good precision (relative standard deviation) ≤ 3.3%. These results indicate that the developed TF-MIL-53(Al) method is a simple, rapid, and highly sensitive alternative to conventional microextraction methods for environmental and food safety monitoring.
