This study developed and tested polysulfone (PSF) beads with NH2-MIL-101(Cr) as a sorbent for PT-μ-SPE. Pesticides were extracted and identified using a high-performance liquid chromatography-photodiode array detector (HPLC-PDA) on real samples such as well water, tea, and honey. PSF beads/NH2-MIL-101(Cr) were synthesized and characterized using X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR), thermal gravimetric analysis (TGA), and scanning electron microscopy (SEM). In addition, the kind and quantity of eluent, pH, and sample volume were studied and optimized. The response surface methodology (RSM) was used to create regression models with a central composite design (CCD). The PSF beads/NH2-MIL-101(Cr) sorbent in PT-μSPE has a linear range of 0.7 to 100.0 μg/L. The suggested technique is highly reproducible, with RSD % (intra-day) values ranging from 2.5% to 3.5%. The technique detected pesticides in water and food samples at concentrations of 33.0–100.0 μg/L, with recovery rates ranging from 80.0% to 102.0%.
