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A solid-phase extraction method followed by reverse phase high-performance liquid chromatography (RP-HPLC) was optimized and validated for the quantitative determination of tartaric, malic, shikimic, lactic, citric and succinic acids in wine. Solid-phase extraction was carried out with C18 cartridges and extraction recoveries for all acids ranging from 98.3 to 103% were obtained. HPLC separation was performed with isocratic elution on a LiChrosorb RP-18 column (250 × 4.6 mm I.D., 5 µm) protected with the appropriate guard column. The mobile phase was a 5 mM solution of H3PO4 with pH 2.1 at a flow rate of 1 ml/min. Detection of the organic acids was performed at 210 nm. The developed method was validated by checking its linearity, limit of detection (LOD), limit of quantification (LOQ), precision and recovery. The method was applied to the analysis of organic acids in Macedonian red and white wines.Keywords: wine; organic acids; separation; HPLC; validation ВАЛИДАЦИЈА И ПРИМЕНА НА HPLC ЗА АНАЛИЗА НА ОРГАНСКИ КИСЕЛИНИ ВО ВИНО ПО ЦВРСТО-ФАЗНА ЕКСТРАКЦИЈАОптимизиран и валидиран е метод за квантитативна анализа на винска, јаболкова, шикимска, млечна, лимонска и килибарна киселина во вино со цврсто-фазна екстракција следена со реверзно-фазна високо ефикасна течна хроматографија (RP-HPLC). Цврсто-фазната екстракција е изведена со колони C18 и добиениот аналитички принос за сите киселини се движи од 98,3 до 103%. Разделувањето со HPLC е извршено со изократско елуирање на LiChrosorb-ова колона RP-18 (250 × 4,6 mm I.D., 5 µm) користејќи соодветна претколона. Мобилната фаза којашто е употребена за елуирање е раствор од H3PO4 со концентрација 5 mM и pH 2,1 при проток од 1 ml/min. Детекцијата на органските киселини е извршена со следење на апсорбанцата на 210 nm. Развиениот метод е валидиран со проверка на неговата линеарност, осетливост, граница на детекција (LOD), граница на квантификација (LOQ), аналитички принос и прецизност. Методот потоа е применет за анализа на органски киселини во македонски црвени и бели вина.

The abundances of selected elements in different environmental compartments, namely soil, honey, and bee pollen, was determined in this study. For that purpose, sixteen soil and honey samples, and nine pollen samples were taken in the region of Mitrovica, Kosovo. The concentration of elements was measured by ICP-AES and ICP-MS. Pollution level concentrations of Pb, Zn, As, and Cd were observed in soil. The level of soil pollution was estimated by calculating pollution indices. Pb was also observed at high concentrations in honey, as was Cd and Pb in pollen. Pearson’s correlation coefficients revealed mostly weak and moderate correlations of the concentrations of the eight selected elements among the soil, honey, and pollen samples. Several groups of elements with geogenic and anthropogenic origin were identified by hierarchical cluster analysis. The concentrations of selected heavy metals for soil and honey were compared to those in neighboring countries, and those for pollen with samples from Turkey, Serbia, and Jordan.

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In this study, a fast, simple, and sensitive analytical method for direct determination of biogenic amines tryptamine, putrescine, histamine, phenylethylamine, tyramine, cadaverine, spermine, and spermidine in wine has been developed and validated. Detection of analytes was performed with ultra-performance liquid chromatography (UPLC) coupled to triple quadruple mass spectrometer (TQ/MS). The calibration curves of all amines were linear with correlation coefficients (R 2 ) ranging from 0.9906 for putrescine to 0.9998 for histamine and 2-phenyethylamine. The accuracy of the method was checked with a standard addition method, showing good accuracy, repeatability, and reproducibility (RSD < 10%). The limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.50 to 30 μg/L and 1.50 to 90 μg/L, respectively, for all amines. The validated method was applied to detect and quantify biogenic amines in Macedonian red and white wines. Higher concentration of amines was observed in red wines (5797 μg/L, on average) compared to the white wines (1485 μg/L, on average).

Elements atmospheric deposition was studied by mosses method in Kosovo. Mosses are a very useful tool for atmospheric deposition of elements monitoring, owing to their physiological and morphological characteristics. Moss samples were collected from 45 locations, they were cleaned from leaves, twigs and other materials, they were grinded, digested in a microwave system and analyzed by spectroscopy Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). A total of 25 elements concentration in collected moss samples was determined: Al, As, Ba, Ca, Cd, Co, Cr, Cu, Fe, Hg, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Sr, Ti, Tl, V and Zn. Extremely high concentrations of Pb and Zn were found in moss samples from the areas of Zveçan and Stanterg where the ore processing facilities are located, as well as the tailings landfill in Mitrovica which is nearby in the south, which reflects eminent air pollution. High concentrations of As and Cd were also measured in the same sampling points. The obtained results were processed by multivariate statistical analysis/factor analysis, which resulted in four factors, one anthropogenic and three geogenic or mixed geogenic-anthropogenic. The factor analysis revealed that the area with the highest atmospheric deposition of potentially toxic elements is the basin of Kosovo, from the north in Leposaviç to the south in Hani i Elezit because of the industrial plants laying in this line.

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