In this research, coupling of dispersive liquid–liquid microextraction and negative corona discharge-ion mobility spectrometry (DLLME-NCD-IMS) was employed for preconcentration and determination of ethion in grape and underground water. The most commonly used solvents in DLLME method are chlorinated ones which are dangerous for human and environment. On the other hand, chlorinated solvents have a high electron affinity, resulting in complication of mobility spectrum in addition to diminution in sensitivity. To overcome these problems, cyclohexane was used as the extraction solvent which is lighter than water and therefore, the extraction solvent containing analyte can be accumulated in upper layer of aqueous phase. In this method, dispersive solution containing 500 ?L disperser solvent (methanol) and 40 ?L extraction solvent (cyclohexane) was injected rapidly into an aqueous solution contains ethion in a special vessel with a syringe. After centrifuging of solution at 3000 rpm for 5 min, the fine droplets of cyclohexane were collected from the upper area of the extraction vessel. Then, 2 mL distilled water was injected through the septum located in the bottom of extraction vessel, so that the organic phase could be easily collected using a syringe. 5 ?L of the collected phase was injected into the NCD-IMS to analyze the extracted ethion. Some important parameters such as the kind of extraction and dispersive solvents and their volume, salt concentration, and sample pH were investigated. Under optimized conditions, linear range (0.2-100.0 ?g/L ), detection limit (0.075?g/L), and RSD (7%) were obtained. In analysis of spiked samples, the enrichment factor and extraction recoveries were 60 and 68-92%, respectively. In addition, some samples of underground water and grape were also analyzed and the satisfactory results reveal the capability of DLLME-NCD-IMS for convenient and very rapid alalysis of real samples.