This study describes an innovative method for the microextraction and determination of chlorpyrifos, utilizing a newly synthesized copper-based metal–organic framework (MOF) with 3,3ʹ-thiodipropionic acid as the ligand. This approach offers a sensitive and reliable solution for the ultra-trace determination of chlorpyrifos in various matrices, highlighting its potential for broader environmental and food safety applications. To minimize environmental impact, a hydrothermal method was chosen for MOF synthesis. The MOF was fully characterized using FT-IR, X-ray diffraction, FESEM-EDX, BET, zeta potential analysis, and XPS; and integrated into a dispersive solid-phase microextraction (DSPME) technique, paired with ion mobility spectrometry (IMS) for chlorpyrifos detection. The DSPME procedure has been optimized for extraction efficiency, minimal solvent use, and low absorbent consumption. A low detection limit of 0.65 ng mL−1 was observed and validated along with a linear detection range of 1.0–400.0 ng mL−1 as the result of this optimization. Experiments with water, pear fruit, and soil samples demonstrated the method’s practicality and superior performance compared to existing techniques, showcasing its potential for real-world applications.
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