A Prussian Blue (PB) zinc oxide carbon nanotube sensing composite was developed for the rapid assaying of H2O2 generated from BT20 and 4T1 breast cancer cells, important for elucidating mechanisms governing apoptosis of these cell lines. The combination of H2O2's transient nature along with matrix effects makes monitoring this molecule in biological samples a challenge. The standard addition method (SAM) was coupled with chronoamperometric sensing (CA) to overcome these obstacles. An electrocatalyst composite consisting of refluxed zinc oxide nanoparticles (NPs) tethered to carboxylic acid-functionalized multiwalled carbon nanotubes (ZnO/COOH-MWNTs) was electrostatically attached to PB for signal enhancement. Optimization of the sensor was achieved via adjusting solution pH and stirring time to optimize PB electrostatic attachment to ZnO/COOH-MWNTs prior to its deposition onto the working glassy carbon electrode (GCE) surface. CA SAM showed the ability to accurately measure H2O2 within the 1-21 μM range, suitable for monitoring cancer cell line apoptosis resistance scenarios and offering analytical advantages over standard enzyme-linked immunosorbent assays (ELISA) for rapid, matrix-effect-free analysis.