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.
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.
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