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An electroanalytical study for possible simultaneous detection of three naturally occurring isomers of vitamin E (α, γ, and δ-tocopherol) was performed. This research includes several optimization steps, such as selection of electrode material, composition of working medium, selection of electrochemical technique, and parameters of square-wave voltammetry (SWV), to reach a well-defined recognition of peaks. A glassy carbon electrode, 99.9% acetonitrile containing 0.1 mol L−1 lithium perchlorate, SWV at the potential step of 1 mV, potential amplitude of 25 mV, and frequency of 25 Hz were decided as the most suitable working conditions. Nevertheless, the corresponding anodic peaks were not sufficiently separated due to their overlapping. Thus, four standard evaluation methods (polynomial or linear baseline, zero base, and deconvolution) were compared, and the last-mentioned method was chosen as optimum. Similar linear ranges from 3.0 × 10−6 to 1.0 × 10−5 mol L−1 were obtained for α, γ, and δ-tocopherol, characterized by determination coefficient of 0.998, 0.985, and 0.994, quantification limits of 11.28, 2.70, and 3.67 × 10−6 mol L−1 and detection limits of 3.72, 0.89, and 1.21 × 10−6 mol L−1, respectively. A recovery from 72.0 to 128.5% for different concetration ratios of tocopherols has been achieved. This recovery range is in the accordance with values reported for liquid chromatography.

A new voltammetric method for the simultaneous determination of vitamin E and vitamin K present in different types of commercially available food supplements has been developed. This electroanalytical method is based on the ex situ adsorptive accumulation of these biologically active compounds onto the surface of a solid glassy carbon electrode (GCE) with subsequent electrochemical detection by square-wave adsorptive stripping voltammetry in 0.01-mol L−1 HNO3 containing 0.1-mol L−1 KCl at pH 2.08. Due to reversible electrochemical reactions of phylloquinone, a subsequent voltammetric detection of both vitamins in anodic mode can be performed. Since individual forms of vitamins E and K usually exhibit nearly identical electrochemical behavior, it is therefore impossible to distinguish individual forms (quinones and tocopherols) and determine their molar concentrations in this way. Thus, the values of vitamin content were expressed as mass equivalent of phylloquinone and α-tocopherol as they are the most biologically active forms. Despite the high sensitivity, relatively short linear ranges were obtained due to the interaction (competition) of both vitamins during adsorption onto the freshly polished surface of the GCE from a 50% aqueous–acetonitrile mixture. The obtained results showed that the voltammetric approach is a very simple and low-cost analytical method that can be used in analyses of food supplements.