This study was aimed to develop a sensitive and accurate method for the determination of lead in urine. Dispersive liquid-liquid microextraction (DLLME) was applied prior to slotted quartz tube – flame atomic absorption spectrometry (SQT-FAAS). Dithizone was employed in generating water-insoluble forms of lead to isolate the analyte in the microextraction. All variables having a direct effect on extraction and instrumental outputs were systematically optimized. The detection limit was 0.5 µg L−1 which indicates a 305-fold enhancement compared to conventional FAAS. The wide linear range is between 2.0 and 250 µg L−1 with a high regression coefficient (0.9998). Urine samples were used in order to examine the practical application of the developed method. The recovery values were between 98.2 and 107.0%.