Two novel, discrete lanthanide–macrocycle binary complexes for the detection of hydrogen sulfide are reported. The hydrogen sulfide sensing mechanism utilises the copper sequestration at a secondary binding site, with resulting bimetallic lanthanide(III)/copper(II) complexes (Ln = Eu³⁺ and Tb³⁺) exhibiting high selectivity, good sensitivity and excellent reversibility for aqueous hydrogen sulfide. The inclusion of the DO2A macrocycle and 4-(2-pyridyl)-1,2,3-triazole dipicolinic acid ligand, results in a complex with good solubility and stability. The europium(III) complex also displayed a low limit of detection (665 ppb) with a response time of 30 seconds with gaseous hydrogen sulfide. The improved water solubility and stability over a previous complex results in these sensors having the potential for use in environmental monitoring and biological studies for various functional settings.