Two new macrocyclic ligands (3) and (4), containing nitrogen-sulfur donor atoms, were designed and synthesized in a multi-step reaction sequence. The macrocycles (3) and (4)were used in solvent extraction of metal picrates such as Ag(+), Hg(2+), Cd(2+), Zn(2+), Cu(2+), Ni(2+), Mn(2+), Co(2+), and Pb(2+) from aqueous phase to the organic phase. The metal picrate extractions were investigated at 25 +/- 0.1 degrees C by using UV-visible spectrometry. The extractability and selectivity of the mentioned metal picrates were evaluated according to the organic solvents. The values of the extraction constants (log K(ex)) and the complex compositions were determined for the extracted complexes. (C) 2008 Elsevier B.V. All rights reserved.