With respect to sensor application investigations, hollow mesoporous carbon sphere-based materials of the spinel type of cobalt oxide (Co 3 O 4 ) and heteroatom-doped materials are gaining popularity. In this contribution, dopamine hydrochloride (DA) and cobalt phthalocyanine (CoPc) precursors were employed to construct a highly homogeneous Co 3 O 4 -embedded N-doped hollow carbon sphere (Co 3 O 4 @NHCS) by a straightforward one-step polymerization procedure. The resulting Co 3 O 4 @ NHCS materials may effectively tune the surface area, defect sites, and doping amount of N and Co elements by altering the loading amount of CoPc. The relatively high surface area, greater spherical wall thickness, enriched defect sites, and better extent of N and Co sites are all visible in the best 200 mg loaded Co 3 O 4 @NHCS-2 material. This leads to significant improvement in pyridine and graphitic N site concentrations, which offers exceptional electrochemical performance. Electrochemical analysis was used to study the electrocatalytic activity of Co 3 O 4 @NHCSs towards the sensing of pharmacologically active significant compounds (acetaminophen). Excellent sensor properties include the linear range (0.001−0.2 and 1.0−8.0 mM), sensitivity, limit of detection (0.07 and 0.11 μM), and selectivity in the modified Co 3 O 4 @NHCSs/ GCE. The authentic sample (acetaminophen tablet) produces a satisfactory result when used practically.