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An electrospun composite of poly(vinyl alcohol) (PVA)/citric acid (CA)/MIL-88A@ carbon nanotubes (CNTs) was synthesized, and employed as an efficacious adsorbent for thin-film micro-extraction of penconazole and propiconazole in agricultural water and soil along with different food samples (milk, honey, fruits, and vegetables). From the evaluation of field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, and X-ray diffraction analysis, the synthesis of the composite nanofibers was corroborated. The presence of MIL-88A@CNTs with porous structure and high content of chemical functional groups in the PVA/CA dedicates a high extraction efficiency to the nanofibers. The effect of MOF@CNTs%, the weight of the composite, pH, salt concentration, extraction time, eluent type and its volume, and stirring rate all were optimized. The calibration plot …