In this study, for the first time, analysis of malathion was done by combining dispersive liquid-liquid microextraction (DLLME) with corona discharge ionization ion mobility spectrometry (CD-IMS) DLLME-CD-IMS with low cost, inexpensive maintenance and very fast analysis make an attractive technique for the determination of malathion in environmental and agricultar samples. In this extraction process, a mixture of 45 µL carbon tetrachloride ( extracting solvent) and 1 mL methanol (disperser solvent) was rapidly injected into the 5 mL aqueuos sample containing the analyte. After centrifuging ( 5 min at 3000 rpm), the fine droplets of carbon tetrachloride were sedimented in the bottom of conical test tube. Sedimented phase was direct injected into the CD-IMS for analysis. Some important parameters, such as kind and volume of extracting and disperser solvent, feasibility direct injection of sedimented phase to CD-IMS, salt addition and effect of pH were investigated and optimized. Under the optimum extraction condition, the enrichment factor and extraction recoveries 150 and 81%, respectively. The method yielded a linear range in the concentration from 4 to 200 µg/L. the limit of detection were 1.83 µg/L, respectively and relative standard deviations were 7.6%. This method could be successfully applied for the determination of malathion pesticides in apple, surface water and underground water.