<p>The current work focusses on synthesis of electrocatalyst for electrochemical determination of metronidazole and water splitting applications. The f-MWCNT@CoCuMoO₄ NCs was developed and characterized systematically, where phase purity of samples was validated by XRD analysis, uniformly dispersed CoCuMoO₄ NPs on f-MWCNT was confirmed by SEM and TEM analysis, elemental composition was determined by EDX and surface area was determined by BET analysis, exhibited the surface area of 34.65 m²/g by facilitating improved active site exposure. Electrochemically investigation of GCE/10% f-MWCNT@CoCuMoO₄ electrode displayed remarkable catalytic efficiency for metronidazole detection, achieving limit of detection 0.31 µM and limit of quantification of 1.04 µM, with 1-850 µM of broad linear range with superior stability. The electrochemical evaluation detection was evaluated by using real samples such as cow and poultry feed, yielding recovery percentage from 95.47% to 103.7% and 90.59% to 105.45%. In this work, six different machine-learning models were tested for calibration of LSV data. Among all models, multivariate linear regression with full available potential range was consistently the best method for achieving highest predictive accuracy, yielding up to R² = 0.99 with lowest RMSE and MAE in all splits. Additionally, GCE/10% f-MWCNT@CoCuMoO₄ electrode had the excellent electrocatalytic activity towards water splitting processes by exhibiting favourable Tafel slope and achieved low overpotential values, 222 mV for HER reaction and 140 mV for OER reaction. These results validate long-term stability, rapid catalytic kinetics and efficient electron transfer. Thus, GCE/10% f-MWCNT@CoCuMoO₄ electrode as a promising dual functional electrocatalyst for electrochemical application including sustainable energy conversion and environmental monitoring.</p>