A new electrochemical sensor based on NiO/Ni@C and poly(isonicotinic
acid), PINA, is fabricated to determine an important chemotherapeutic
drug, methotrexate (MTX). At first, a bare glassy carbon electrode
(GCE) was modified by NiO/Ni@C; then, INA was electropolymerized at
its surface. FT-IR, XRD, FE-SEM, EDS, elemental mapping, TEM, AFM,
and BET techniques were used to characterize the nanomaterials. Following
that, parameters affecting the sensor response, such as pH, amount
of the electrocatalyst, electropolymerization cycles, and instrumental
parameters, were optimized using cyclic voltammetry (CV) and differential
pulse voltammetry (DPV). Under the optimized conditions, a linear
range was obtained from 0.02 to 2.5 μM with a detection limit
of 7.2 nM. Repeatability was obtained with a relative standard deviation
(RSD) of 2.4%, and reproducibility was obtained with an RSD of 6.2%.
Finally, the sensor was tested in the presence of potential interference
compounds and human blood plasma with acceptable responses.