In this paper, the detection protocols for the selective and simultaneous determination of diclofenac (DCF) and tetracycline (TC) in aqueous solutions were developed using a commercial boron-doped diamond electrode modified with graphene oxide and silver, as the Ag/GG/BDD electrode. This electrode presented the possibility to detect only DCF and TC selectively by applying amperometric techniques. However, the pulsed voltammetric techniques operated in optimized working conditions allowed the selective/simultaneous detection of DCF and TC characterized by the improvement of the performance parameters compared to CV. Following the research study related to the electrochemical detection application of the two emerging target pollutants (DCF and TC), the Ag/GR/BDD electrode presented good stability and reproducibility of the results obtained