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+, Hg2+, Cd2+, Zn2+, Cu2+, Ni2+, Mn2+, Co2+, and Pb2+ 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.