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Herein, an electrospun polyacrylonitrile/nickel-based metal–organic framework nanocomposite (PAN/Ni-MOF) coating on a stainless steel wire was synthesized and employed as a novel nanosorbent for headspace solid-phase microextraction (HS-SPME) of organophosphorus pesticides (OPPs), diazinon (DIZ), and chlorpyrifos (CPS) from the diverse aqueous media followed by corona discharge ion mobility spectrometry (CD-IMS). Under the optimum experimental conditions, the calibration plots were linear in the range of 1.0–250.0 ng mL⁻¹ for DIZ and 0.5–300.0 ng mL⁻¹ for CPS with r² > 0.999. The detection limits (S/N = 3) were 0.3 and 0.2 ng mL⁻¹ for DIZ and CPS, respectively. The intra-day relative standard deviations (RSDs%) (n = 5) at the concentration levels of 20.0, 40.0, and 100.0 ng mL⁻¹ were ≤ 5.2%. To investigate the extraction efficiency, PAN/Ni-MOF was employed to analyze various juice …