Efficient rice-shaped polyaniline@bismuth oxide (PANI@Bi 2 O 3 ) nanocomposites were synthesized by in situ sol-gel method. The sol of polyaniline was added to the gel of Bi 2 O 3 in different mixing volume ratios of inorganic reactant and with a fixed mixing volume ratio, i.e., 1:1, of organic polymer. The physicochemical characterization was carried out by SEM, XRD, FTIR, UV-Vis and simultaneous TGA studies. PANI@Bi 2 O 3 were deposited on a silver electrode (AgE, surface area, 0.0216 cm 2 ) to give an efficient sensor with a fast response toward the toxic 3-methoxy phenol in liquid phase. The calibration plot is linear (r 2 = 0.9809) over the 0.09 nM to 0.09 mM 3-methoxy phenol concentration ranges. The sensitivity is *0.8796 lAcm -2 lM -1 , and the detection limit is 0.016 ± 0.002 nM (signal-to-noise ratio, at a SNR of 3), which leads to a promising future sensitive sensor development using organic-inorganic nanocomposites by reliable I-V method for the potential applications of hazardous phenolic compounds in environmental and healthcare fields.Graphical Abstract Schematic diagram for the synthesis of rice-shaped polyaniline@Bi 2 O 3 nanocomposite.