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An electrospun composite of polyvinyl chloride/ethylene–vinyl acetate/chitosan/starch (PVC/EVA/CS/Str) was synthesized and used as a novel sorbent for thin-film micro-solid-phase extraction (TFME) of atrazine (ATZ) and ametryn (AMT) prior to corona discharge ion mobility spectrometry (CD-IMS) analysis. The fabricated sorbent was characterized using scanning electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. Based on the investigations, thanks to the presence of CS/Str, the synthesized composite nanofiber exhibited high porosity, large surface area and acceptable reusability. Also, the sorbent provided various interactions with the intended analytes (hydrogen bonding, hydrophobic contacts and π-π stacking interactions), resulting in the improvement of extraction efficiency. Effective factors on adsorption and desorption steps were optimized by using both one at time method …