In this work, thin film containing ZnTiO 3 nanoparticels was used as a sorbent for microextraction method and coupled to corona discharge ion mobility spectrometry in negative mode. Thin film containing 15% polyacrylonitrile and 5% ZnTiO 3 in dimethylformamide was synthesized via electrospinning technique. Ethion pesticide was selected as a test compound. In order to increase the extraction efficiency, some effective parameters for ethion extraction such as extraction temperature, sample solution pH, extraction time, salt effect, and stirring rate were evaluated. The extraction under optimum conditions was carried out at 45 °C, pH=6 and stirring rate of 900 rpm for 20 min. The detection limit was 0.4 ?g/L and the dynamic range was found in the range of 1.0-100 ?g/L with the correlation coefficient of 0.9986. The intra and inter-day relative standard deviations were 3-5% and 8-10%, respectively. Agricultural wastewater, well water and orange were studied as real samples and the recoveries were obtained between 90-109%.