This study is a report on the synthesizing nanodiamond/MoS2 nanorod composite using the hydrothermal method and its application as adsorbent in micro solid phase extraction of lead(II) and copper(II) prior their determination through flame atomic absorption spectroscopy. The nanodiamond/MoS2 nanorod composite was characterized using Raman spectroscopy, BET surface analysis and scanning electronic microscopy (SEM). The optimal conditions including amount of used adsorbent, pH, vortex time, elution condition and volume investigated. Quantitative recoveries for both analytes were obtained at pH 3.0. The preconcentration factor is 35, and the sorption capacity of synthesized adsorbent for lead(II) and copper(II) is 19,87 and 49.33 mg g(-1). The relative standard deviation is 0.9 and 1.5% for lead(II) and copper(lI) at a level of 200 sg L-1 (n = 6), and the detection limit is 42 and 22 lag L-1 for lead(II) and copper(II), respectively. The procedure accuracy was proved via analyzing the standard reference materials (SPS-WW2 Waste water Level 2 and TMDA-53.3). The presented procedure was applied for the determination of copper and lead contents of the water samples from Turkey. (C) 2017 Elsevier B.V. All rights reserved.