A rapid and improved method for the determination of ethyl carbamate in foodstuffs of different matrices.

This work deals with the rapid and simple determination of the probable carcinogen ethyl carbamate (EC), which is naturally present in fermented food products. An undemanding, robust, and rapid pre-column derivatization utilizing a 9-xanthydrol reagent has been developed. The resulting derivative was subsequently analysed by reversed-phase high-performance liquid chromatography coupled with fluorescence detection. As a result of the thorough optimisation of the chromatographic conditions, the run was completed in just 5 minutes, considerably speeding up the usual time of EC separation (30-60 min). Thanks to the fast separation, satisfactory yields (around 90%), negligible matrix effects, no interfering peaks, very low detection limit, and simple sample pre-treatment (for the very first time, the derivatization was performed in the presence of light and without any extraction step), the proposed method represents a significant improvement of the EC determination protocol used so far. After method validation, a total of fifty food samples were subjected to analysis without any additional sample pre-treatment despite their diverse matrix. Due to its robustness, simplicity, and low time, cost, and manual demands, this method is suitable for rapid screening of EC in both final food products and during their production.

Targeted and Non-Targeted HPLC Analysis of Coffee-Based Products as Effective Tools for Evaluating the Coffee Authenticity.

Coffee is a very popular beverage worldwide. However, its composition and characteristics are affected by a number of factors, such as geographical and botanical origin, harvesting and roasting conditions, and brewing method used. As coffee consumption rises, the demands on its high quality and authenticity naturally grows as well. Unfortunately, at the same time, various tricks of coffee adulteration occur more frequently, with the intention of quick economic profit. Many analytical methods have already been developed to verify the coffee authenticity, in which the high-performance liquid chromatography (HPLC) plays a crucial role, especially thanks to its high selectivity and sensitivity. Thus, this review summarizes the results of targeted and non-targeted HPLC analysis of coffee-based products over the last 10 years as an effective tool for determining coffee composition, which can help to reveal potential forgeries and non-compliance with good manufacturing practice, and subsequently protects consumers from buying overpriced low-quality product. The advantages and drawbacks of the targeted analysis are specified and contrasted with those of the non-targeted HPLC fingerprints, which simply consider the chemical profile of the sample, regardless of the determination of individual compounds present.

Comparison of mononuclear and dinuclear copper(II) biomimetic complexes: spectroelectrochemical mechanistic study of their catalytic pathways.

Two catecholase-like biomimetic catalysts, namely, two dinuclear copper complexes [Cu2(L1)(OH)(H2O)(EtOH)][ClO4]2 (C1) and [Cu2Ac2O(L1)ClO4] (C2) with the 2,6-bis(4-methyl piperazin-1-yl-methyl)-4-formyl-phenoxy ligand (L1) together with the mononuclear complex Cu(ClO4)2(L2) (C3) containing ligand 1,2-(C5H4N-6-OCH3-2-CHN)2CH2CH2 (L2), were synthesized. Their catalytic pathways were investigated and compared. The evaluation of the catalytic activity of compound C1 (and C2, C3) using the Michaelis-Menten model was represented by values of KM = 272.93 (223.02; 1616) µmol L-1 and Vmax of 0.981 (1.617; 1.689) µmol L-1 s-1. The role of water content in the solvent is also discussed. The dinuclear complexes C1 and C2 were found to be more efficient catalysts than mononuclear complex C3. The mode of catalytic action was characterized via cyclic voltammetry, spectrophotometry, and UV-Vis spectroelectrochemistry. The catalytic mechanism of 3,5-di-tert butyl catechol oxidation in the presence of oxygen was proposed. The reaction circle was proved by the confirmation of the chemical reversibility of complex reduction. The advantage of the in situ spectroelectrochemical measurement enabled to control the reduction of quinone formed by the chemical reaction of catechol with oxygen in solution. At this step, the simultaneous change in the absorption spectrum indicated a change in the copper redox state of the catalyst.

Rapid analysis of phenyl isothiocyanate derivatives of amino acids present in Czech meads.

Amino acids (AAs) are minor compounds occurring in meads contributing to their final organoleptic properties. Determination of AAs profile and content can help to assess the mead authenticity, adulteration and thus its quality. This work deals with the optimization of rapid analysis of 21 AAs present in mead using reversed-phase high performance liquid chromatography with spectrophotometric detection after simple derivatization procedure with phenyl isothiocyanate agent without any sample pre-treatment. Optimized derivatization and separation conditions have been successfully applied to the quantification of AAs present in five Czech meads using the multiple point standard addition method. The total amino acid content was in the range of 134-828 mg/L. The content of proline was confirmed by Harmonised spectrophotometric method. Both chromatographic and spectrophotometric methods provided overlapping results in the range of 30-266 mg/L.

Voltammetric determination of taurine in energy drinks after o-phthalaldehyde-ethanethiol derivatization.

A completely new voltammetric method has been developed for quantitative determination of food additive Taurine (Tau) in energy drinks. This electroanalytical method is based on voltammetric oxidation of o-phthalaldehyde-ethanthiol derivative of Tau at glassy carbon electrode in 95% methanol containing 0.1 mol L-1 lithium perchlorate. Working conditions necessary for quantitative Tau derivatization reaction and electrochemical detection using square wave voltammetry were optimized. Linear range from 1.0 × 10-5 to 1.0 × 10-4 mol L-1 characterized by coefficient of determination 0.9998, limits of quantification 6.8 × 10-6 mol L-1 and detection 2.1 × 10-6 mol L-1 were obtained at pulse amplitude 50 mV and frequency 80 Hz. Analytical method of calibration curve was used for evaluation of Tau content in several commercially available energy drinks. The procedure was validated using standard reference high performance liquid chromatography (HPLC) method. Both methods showed nearly identical Tau content, around 0.35% (w/w). Besides its reliability to the Tau determination, that is totally comparable to reference method used, present voltammetric approach is more advantageous on the economic and simplicity basis. Finally, developed voltammetric method could find employment in food quality control.