New macrocyclic ester (L) was yielded through reaction of catechol with isophthaloylchloride and isolated as white solid, air stable at room temperature. L was characterized by melting point, mass spectra, FTIR and NMR ( 1 H, 13 C) spectroscopy. The molecular structure was determined by single-crystal X-ray diffraction. The macrocyclic compound was evaluated to determine ultra-trace concentrations of Pb (II) by anodic stripping voltammetry in the presence of Cd(II). The method is based on the formation of a complex between lead and the macrocyclic ester, immobilized on a vitreous carbon electrode, allowing the oxidation of lead by voltammetric scan, using square wave modulation method. Anodic peak current was observed at -0.20 V for Pb(II). Under the best experimental conditions (pH 4.0; L concentration 10.0 mmol L -1 ; accumulative potential (Eacc) -0.8 V and accumulative time (tacc) of 60 s) anodic peak current was proportional to the Pb (II) concentration up to 80.0 ?g L -1 , with a detection limit (3?) of 0.33 ?g L -1 . The proposed method was validated by determining Pb(II) in model solution with ultra-pure water with satisfactory results.