The stopped-flow technique was employed to measure chemiluminescent emission from the reaction of a mixture of oxalate and proline with a chemiluminescence reagent, tris(2,2'-bipyridine) ruthenium(III), or Ru(bpy)3(3+) is a versatile reagent and is often used in bioanalytical applications, including the detection of certain drugs and their metabolites, for example. Unfortunately, Ru(bpy)3(3+) has not yet been fully examined as a possible chemiluminescence reagent for simultaneous kinetic determinations. In this work, a differential reaction rate method, based on simple least squares regressions of the pseudo-first order decay data, was used to resolve two compounds, oxalate and proline, reacting simultaneously with Ru(bpy)3(3+). Our results indicate that stopped-flow analyses with Ru(bpy)3(3+) could provide a viable method for simultaneous determinations of unresolvable analytes of environmental and pharmaceutical importance.