A macrobicyclic ligand and its mononuclear Ni(II) complex were studied as extractants for Pb2+, Cd2+, and Hg2+. The metal picrates were used for extraction experiments. The solutions of the ligands in chloroform and dichloromethane were used as organic phases. The most effective transport was observed for Cd2+ picrate among the tested metal picrates with dichloromethane. The effect of pH on the extraction efficiency was evaluated for both organic solvents. The cations were stripped from the organic phase with 0.75M nitric acid and the ligands were determined spectrophotometrically in the proper wavelength. The recovery% values of the ligands were calculated at pH 3.5.