In this work, dispersive liquid - liquid microextraction coupled with corona discharge ion mobility spectroscopy (DLLME-CD-IMS) was applied for the extraction and determination of diazinon in apple juice and underground water samples. For the extraction, an appropriate mixture of methanol as dispersive solvent and CCl 4 as extraction solvent was injected rapidly into a glass tube with conical bottom containing aqueous solution of diazinon. This injection led to a cloudy water solution, caused by the fine droplets dispersion of the immiscible extraction solvent (CCl 4 ) in the aqueous sample. The result of this phenomenon was the generation of a high contact area between the aqueous phase and the extraction solvent. The final step of the microextraction procedure was centrifugation (5 min at 3000 rpm) to collect the dispersed tinny CCl 4 droplets in the bottom of the test tube. Afterward, 5.0µL of the solution was directly injected into the IMS, for analysis of the analyte. In order to obtaining optimum condition of the extraction, several parameters affecting on the extraction such as: extraction solvent type, dispersive solvent type, extraction and dispersive solvent volume, salt addition and pH were studied. Under optimum condition (pH 7, 60 µL extraction solvent, 1 mL dispersive solvent and without salt addition), enrichment factor 60 and the limit of detection of 0.2 µg/L were obtained. Good dynamic range was obtained in the range of 0.5 – 100.0 µg/L for extraction of diazinon. The relative standard deviations for analysis of 20 µg/L of diazinon in standard solutions, was 7% (n=3). The obtained recovery for spiked samples was above 89%, indicating the capability of DLLME as rapid and convenience method for real sample analysis.