In this work, a dispersive liquid–liquid microextraction (DLLME) based on a high density extracting solvent was applied as a simple, quick and sensitive method for extraction and pre-concentration of methamphetamine from human Plasma and urine samples. Subsequently, the sufficiency of positive corona discharge ionization ion mobility spectrometry was investigated for direct analysis of extracted analyte. Some parameters affecting the extraction efficiency such as type and volume of extraction and disperser solvents, Centrifuge time and sample solution pH were optimized. Chloroform and Isopropanol selected as extracting and disperser solvents respectively. Under the optimized conditions, very low limit of detection was calculated 0.2 µg/L. The relative standard deviations (RSDs) of intra-day and inter-day were obtained 4% and 10% respectively. Lnearity range (R 2 =0.9969) was found to be 0.5-18 µg/L. and also average extraction recovery achieved 104 for plusma and urine samples. Enrichment factor (Ef) obtained 15 for methamphetamine.