Dual
heteroatom-doped carbon hollow spheres have attracted attention
for their intriguing properties, including high surface areas, mesoporosity,
sphere wall thicknesses, edge plane defect sites, catalytic active
sites, and fast heterogeneous electron-transfer rates. Understandably,
the material finds widespread attention in the field of electrochemical
sensors. In this work, we have successfully synthesized nitrogen (N)
and phosphorus (P) dual doped hollow mesoporous carbon spheres (NPHMCS)
by a simple self-polymerization process. The effect of loading a P
precursor, namely, phytic acid (PA), on the electrochemical sensing
of bioanalytes is investigated in detail. The investigation revealed
that 0.6 g loading of PA (NPHMCS-0.6) resulted in an enhanced surface
area of 940 m2 g–1, a higher pore volume
of 0.40 cm3 g–1, enriched defect sites
of 0.99, pyridinic sites of 24.90%, and moderate P–C + P–N
sites of 74.65%. The synergistic effect of nitrogen and phosphorous
doping along with the abovementioned properties is taken advantage
in the fabrication of electrochemical sensors for the simultaneous
determination of ascorbic acid (AA), dopamine (DA), uric acid (UA),
and acetaminophen (AC). The fabricated sensors displayed a wide linear
range of sensing over a concentration from 5 to 6000 μM for
AA, 0.5 to 2000 μM for DA, 0.5 to 5000 μM for UA, and
5 to 1200 μM for AC. Based on the calibration plot, the limits
of detection (LOD) were calculated to be 0.032, 0.002, 0.005, and
0.020 μM for AA, DA, UA, and AC, respectively. The electroanalytical
performance of the fabricated sensor was successfully validated for
the analysis of target species in real samples. The developed methodology
offers prospective advantages in clinical diagnostics for the simultaneous
analysis of small biomolecules and drugs.