A new amine based microextraction procedure has been established for the separation and preconcentration of lead (II). N,N-dimethyl-n-octylamine was used as extraction solvent and chelating agent for lead (II). Microsampling flame atomic absorption spectrometry was used for the determination of lead. The analytical parameters including pH, amounts of N,N-dimethyl-n-octylamine, sample volume etc. were optimized. The influences of the matrix components were also investigated. The validation of the procedure was done by the analysis of TMDA 64.2 certified reference material. The Limit of detection (LOD) of developed method was 2.6 mu g L-1. The developed microextraction procedure was successfully applied to natural water samples.