The simultaneous detection of multiple biological small molecules is critical for human health evaluation and disease prevention. In this study, a nano-ZnS decorated hierarchically porous carbon (ZSHPC) electrocatalyst with multiple enzyme-like activities as a nanozyme sensing platform for simultaneous derivative voltametric detection of four important biological small molecules, dopamine (DA), uric acid (UA), guanine (G), and adenine (A), is successfully synthesized via an in situ hydrothermal reaction using leaves of Cinnamomum camphora (L.) after the extraction of essential oil as a carbon source, ZnCl₂ as both zinc source and an activator, sulfuric acid as a sulfur source, and silica gel as a hard template. Activator together with the introduction of silica gel is beneficial for tuning pore structure. The in situ synthesized ZnS nanoparticles and sulfur doping improve the conductivity and cycling stability of the material. The ZSHPC electrode with multiple enzyme-like activities and oxidase-like characteristics was employed for the simultaneous detection of multiple target molecules in linear ranges of 0.3–500 μM with detection limits of 0.12 μM for DA, 0.26 μM for UA, 0.07 μM for G, and 0.075 μM for A. A derivative technique was selected for enhancing the peak resolution of the partial overlapped voltammograms and eliminating human error. Both the coefficient of determination and residual prediction deviation were used to evaluate this technique.