In this research, for the first time combination of ultrasound-assisted extraction and thin film micro-solid phase extraction (UAE-TF-μSPE) was developed, and applied to extract the acetamiprid and thiacloprid from foods. This procedure was shaped to resolving the analytical challenges that arise from analyzing food samples that display matrix effects on analyte recovery. Here, UAE extracts analytes from food matrices using less extraction solvent and is then coupled with TF-μSPE, where the latter performs clean-up and preconcentration of the target compound. NH2-MIL-101(Cr) was synthesized through hydrothermal method, embedded in a polysulfone thin film, and utilized as an adsorbent in μSPE technique. The optimization of factor affecting of procedure was established based on response surface methodology (RSM). The critical parameters, such as pH, volume of extraction solvent, and ultrapure water volume were optimized. The method demonstrated outstanding analytical performance, with a detection limit established at 0.2 μg kg−1, a linearity range of (1.0-200.0) μg kg−1, very good repeatability characterized by relative standard deviation values between 2.7 % and 4.0 %, and excellent relative recovery from 85.0 to 102.0 % spiked levels 30.0-100.0 μg kg−1. The present method was able to extract pesticides from fruit and vegetable matrices using 1.4 mL of organic solvent. The presence of NH2-MIL-101(Cr) in packed thin film at the pipette tip without clogging and back pressure preconcentrated the insecticide with high extraction efficiency. The adsorbent also exhibited a remarkable durability, contributing to repeated use without performance degradation.
