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Ivana Sálusová, Kristína Cinková, Barbora Brtková, Marian Vojs, Marián Marton and Ľubomír Švorc
The electrochemical behavior and determination of ascorbic acid (AA) was investigated at a bare boron-doped diamond (BDD) electrode using cyclic and differential pulse voltammetry. The influence of pH of supporting electrolyte and scan rate on the current response of analyte was examined to select the suitable experimental conditions. It was found that AA provided one well-shaped irreversible and diffusioncontrolled oxidation peak at +0.87 V vs. Ag/AgCl in Britton-Robinson buffer pH 4.0. Applying differential pulse voltammetry, the peak current of AA was linearly proportional to its concentration from 5 × 10-6 to 2 × 10-4 mol L-1 (R2 = 0.999), with the limit of detection of 1.1 × 10-6 mol L-1 and the good repeatability (relative standard deviation of 2.3 %). The developed electroanalytical protocol was successfully applied to determine the content of AA in commercial pharmaceutical preparations, based on the standard additions method, with the obtained recovery of 122 %. The accomplished analytical performance indicates that BDD electrodes are promising electrochemical sensors for pharmaceutical analysis.
Elisabeta-Irina Geana, Andreea-Maria Iordache and Roxana Elena Ionete
Increased use of food, beverages or drugs containing synthetic sweeteners presents a real danger to health, which is why the EU Member States had to establish a system of regular surveys to monitor sweetener consumption. In case of wine industry, according to law no. 244/2002, Romania prohibits the addition of synthetic sweeteners in wine in order to obtain sweet wine. The official method for detection of adulterated sweet wines with synthetic sweeteners is TLC-Thin Layer Chromatography. However, quantitative methods of analysis are needed to measure levels of sweeteners in different food matrices and high performance liquid chromatography has proved to be a powerful tool for quantitative analysis of compounds at traces levels. In this paper, a high performance liquid chromatographic (HPLC) method for the simultaneous separation and determination of three of the most popular artificial sweeteners (acesulfame potassium, saccharine and aspartame) in a single injection was developed. The described method is rapid, accurate and highly sensitive. Detection limit were 4 mg/L for acesulfame K, 1 mg/L for saccharine and 9 mg/L for aspartame respectively. The precision of the method was about 2% and recovery ranged between 92.6% and 103.3%. There were analyzed commercial wine samples, in order to detect possible counterfeits-sweet and medium sweet wines. Therefore, of the 20 analyzed wine samples, only two samples consisting in wine sweet table, were counterfeited by adding saccharin.
An effective and practical method for the determination of macrolide antibiotics azithromycin, clarithromycin, erythromycin and roxithromycin in wastewater samples has been developed. The analytical method combines solid phase extraction followed by a chromatographic separation by hydrophilic interaction liquid chromatography (HILIC) coupled with an ion trap mass spectrometer utilizing the electrospray ionization technique. Detection of positively charged ions was performed in full scan mode from 500 to 900 m/z. The method detection limits and method quantification limits obtained were in the range of 2.03-7.59 ng L-1 and 6.08-23.84 ng L-1, respectively. Recoveries of solid phase extraction were obtained using SupelTM-Select HLB cartridges ranging from 85.76 % to 92.54 %. All target antibiotics were detected in 100 % of the collected raw influent samples with concentrations varying from 15 ng L-1 to 1849 ng L-1. Azithromycin, clarithromycin and erythromycin were also detected in 100 % of the treated water samples and roxithromycin was present in 96 % of the samples. The highest determined concentration in the treated water samples was 1404 ng L-1 of azithromycin. Based on the determined macrolide concentrations, removal efficiencies of individual wastewater treatment plants were calculated to range from 13 % to 100 %.
Miroslav Variny, Patrik Furda, Norbert Kováč and Otto Mierka
Propane-propylene mixture splitting by industrial conventional rectification incorporating a heat pump for energy intensity decrease was modeled in the Matlab environment. The constructed model was verified by comparing its results with operational data of a real C3 fraction splitting unit. As documented, increased product quality can be obtained at zero additional costs due to specific features of the system design. Process capacity and product purity limitations have to be considered in future C3 fraction production increase plans. Further compressor and its driving unit design features have to be incorporated in the calculation model to reliably assess the C3 fraction processing costs and provide a reliable tool for process operation optimization.
I.V. Tudose, M. Suchea, K. Siderakis, E. Thalassinakis and E. Koudoumas
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4. Siderakis, K