This paper reports the results obtained from the determination of ascorbic acid with platinum-based voltammetric sensors modified with potassium hexacyanoferrate-doped polypyrrole. The preparation of the modified electrodes was carried out by electrochemical polymerization of pyrrole from aqueous solutions, using chronoamperometry. Polypyrrole films were deposited on the surface of the platinum electrode, by applying a constant potential of 0.8 V for 30 s. The thickness of the polymer film was calculated from the chronoamperometric data, and the value was 0.163 μm. Cyclic voltammetry was the method used for the Pt/PPy-FeCN electrode electrochemical characterization in several types of solution, including KCl, potassium ferrocyanide, and ascorbic acid. The thin doped polymer layer showed excellent sensitivity for ascorbic acid detection. From the voltammetric studies carried out in solutions of different concentrations of ascorbic acid, ranging from 1 to 100 × 10−6 M, a detection limit of 2.5 × 10−7 M was obtained. Validation of the analyses was performed using pharmaceutical products with different concentrations of ascorbic acid, from different manufacturers and presented in various pharmaceutical forms, i.e., intravascular administration ampoules, chewable tablets, and powder for oral suspension.
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