A novel voltammetric sensor based on CeO2·Fe2O3 nanoparticles (NPs) has been developed for the determination of lipoic acid, playing an essential role in aerobic metabolism in the living organism. Sensor surface modification provides a 5.6-fold increase of the lipoic acid oxidation currents and a 20 mV anodic shift of the oxidation potential. The best voltammetric parameters have been obtained for the 0.5 mg mL−1 dispersion of CeO2·Fe2O3 NPs. Scanning electron microscopy (SEM) confirms the presence of spherical NPs of 25–60 nm, and their aggregates evenly distributed on the electrode surface and formed porous coverage. This leads to the 4.4-fold increase of the effective surface area vs. bare glassy carbon electrode (GCE). The sensor shows a significantly higher electron transfer rate. Electrooxidation of lipoic acid on CeO2·Fe2O3 NPs modified GCE is an irreversible diffusion-controlled pH-independent process occurring with the participation of two electrons. The sensor gives a linear response to lipoic acid in the ranges of 0.075–7.5 and 7.5–100 μM with the detection limit of 0.053 μM. The sensor is selective towards lipoic acid in the presence of inorganic ions, ascorbic acid, saccharides, and other S-containing compounds. The sensor developed has been tested on the pharmaceutical dosage forms of lipoic acid.
Tartrazine and brilliant blue FCF are synthetic dyes used in the food, cosmetic and pharmaceutical industries. The individual and/or simultaneous control of their concentrations is required due to dose-dependent negative health effects. Therefore, the paper presents experimental results related to the development of a sensing platform for the electrochemical detection of tartrazine and brilliant blue FCF based on a glassy carbon electrode (GCE) modified with MnO2 nanorods, using anodic differential pulse voltammetry. Homogeneous and stable suspensions of MnO2 nanorods have been obtained involving cetylpyridinium bromide solution as a cationic surfactant. The MnO2 nanorods-modified electrode showed a 7.9-fold increase in the electroactive surface area and a 72-fold decrease in the electron transfer resistance. The developed sensor allowed the simultaneous quantification of dyes for two linear domains: in the ranges of 0.10–2.5 and 2.5–15 μM for tartrazine and 0.25–2.5 and 2.5–15 μM for brilliant blue FCF with detection limits of 43 and 41 nM, respectively. High selectivity of the sensor response in the presence of typical interference agents (inorganic ions, saccharides, ascorbic and sorbic acids), other food dyes (riboflavin, indigo carmine, and sunset yellow), and vanillin has been achieved. The sensor has been tested by analyzing soft and isotonic sports drinks and the determined concentrations were close to those obtained involving the chromatography technique.
Sulfur-containing antioxidants are an important part of the antioxidant defense systems in living organisms under the frame of a thiol–disulfide equilibrium. Among them, l-cysteine, l-homocysteine, l-methionine, glutathione, and α-lipoic acid are the most typical representatives. Their actions in living systems are briefly discussed. Being electroactive, sulfur-containing antioxidants are interesting analytes to be determined using various types of electrochemical sensors. Attention is paid to the chemically modified electrodes with various nanostructured coverages. The analytical capabilities of electrochemical sensors for sulfur-containing antioxidant quantification are summarized and discussed. The data are summarized and presented on the basis of the electrode surface modifier applied, i.e., carbon nanomaterials, metal and metal oxide nanoparticles (NPs) and nanostructures, organic mediators, polymeric coverage, and mixed modifiers. The combination of various types of nanomaterials provides a wider linear dynamic range, lower limits of detection, and higher selectivity in comparison to bare electrodes and sensors based on the one type of surface modifier. The perspective of the combination of chromatography with electrochemical detection providing the possibility for simultaneous determination of sulfur-containing antioxidants in a complex matrix has also been discussed.
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