Samuel B. Adeloju

The fabrication of a highly selective and ultrasensitive sulfite nanobiosensor based on a layered architectural fabrication aided by the encapsulation of sulfite oxidase (SOx) in Nafion (Naf) matrix on a multiwalled carbon nanotubes‐polypyrrole (MWCNTs‐PPy) composite decorated with platinum nanoparticles (PtNPs) is described. The MWCNTs are deposited in the inner layer on a Pt electrode during electropolymerization of pyrrole (Py), followed by decoration with a PtNPs layer and subsequent encapsulation of SOx with Naf in the third layer capped with a fourth thin PtNPs layer. Images obtained by field emission scanning electron microscopy (FESEM) reveal that high‐density PtNPs are deposited onto the 3D nanostructured inner MWCNTs‐PPy layer and the electrochemical behavior is investigated. A large surface area provided by the incorporation of MWCNTs in the composite and decoration with PtNPs enables increased SOx loading, SOx retention, and substantial improvement in sensing performance. The resulting layered PtNPs/SOx‐Naf/PtNPs/MWCNTs‐PPy nanobiosensor exhibits a fast response time (within 3 s), a linear calibration range of 20 n m m – 6 m with an excellent sensitivity of 71 µA m m −1 cm −2 and a detection limit of 5.4 n m . The nanobiosensor was effective in discriminating against common interferants and was successfully applied to sulfite determination in real samples.