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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.

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Simple and rapid voltammetric method for simultaneous determination of all‐trans‐retinyl acetate (RAc) or all‐trans‐retinyl palmitate (RPa) and α‐tocopheryl acetate (α‐TOAc) has been proposed. The respective method was based on the anodic oxidation of the compounds of interest by square‐wave voltammetry in acetone with 0.1 mol L−1 LiClO4 at the glassy carbon electrode. The procedure was also beneficial with respect to simple dissolution of sample directly in the supporting electrolyte. The all‐trans‐retinyl acetate could be quantified in two linear ranges (3.1–140 μmol L−1 and 140–400 μmol L−1) and α‐tocopheryl acetate in linear range 5.3–400 μmol L−1 with detection limits of 0.9 μmol L−1 RAc (or 0.8 μmol L−1 RPa) and of 1.6 μmol L−1 α‐TOAc. Selected commercial cosmetic products were analysed achieving satisfactory recoveries.