A porous silicon/palladium nanostructure was prepared and used as a new electrode material for the simultaneous determination of acetaminophen (ACT) and codeine(COD). Palladium nanoparticles were assembled on porous silicon(PSi) microparticles by a simple redox reaction between the Pd precursor
and P-Siinan aqueous solution of hydrofluoric acid.This novel nanostructure was characterized by different spectroscopic and electrochemical techniques in cluding scanning electronmicroscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, fourier transform infrared spectroscopy and cyclic
voltammetry. The high electrochemical activity, fast electron transfer rate, high surface area and good antifouling properties of this nanostructure enhanced the oxidation peak currents and reduced the peak potentials of ACT and COD at the surface of the proposed sensor. Simultaneous determination of ACT and
COD was explored using differential pulse voltammetry. A linear range of 1.0–700.0 nmol L
1 was achieved for ACT and COD with detection limits of 0.4 and 0.3 nmol L
1, respectively. Finally, the proposed method was used for the determination of ACT and COD in blood serum, urine and pharmaceutical compounds.