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Pollution caused by pesticides have attracted huge attention, and it is of a great significance to develop sensitive methods for trace monitoring these analytes in complicated matrices. Herein, the composite of styrene acrylonitrile copolymer p(St-Co-AC)/zeolitic based metal–organic frameworks (Co-ZIF-67)/Chitosan (CS) electrospun nanofibers was fabricated by using an electrospinning approach. The resultant composite nanofibers were characterized to apply as a novel adsorbent for pipette tip micro solid-phase extraction (PT- μSPE) of four pesticides prior to GC-FID analysis. Incorporating Co-ZIF-67@Chitosan into p(ST-Co-AC) results in increasing the porosity features and surface area of the nanofibers. The effect of different main parameters on extraction efficiency was evaluated. Under the optimal conditions, linearity ranges were 1.5–2000.0 ng mL⁻¹ for ethofumasate, 2.0–2000.0 ng mL⁻¹ for ametryn and …