. This work proposes amethod based on formation of the Mn(III)-EDTA complex after oxidation of
theMn(II)-EDTA complex by PbO2 immobilized on cyanoacrylate spheres. A design of experiments (DOE) based
on the Doehlert matrix was used to determine the optimum conditions of the method, and the influence of the
variables was evaluated using a multiple linear regression (MLR) model. The optimized method presented a linear
response in the range from 0.77 to 100.0 μmol L−1, with analytical sensitivity of 7.7 × 103 L mol−1, a coefficient
of determination of 0.999, and a limit of detection of 0.23 μmol L−1. Themethodwas applied using samples
fortified at different concentration levels, and the recoveries achieved were between 97.0 and 104.9%.