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Razvoj disperzivne mikroekstrakcije na trdno fazo za izbrana okoljska onesnaževala
ID Težak, Nina (Author), ID Prosen, Helena (Mentor) More about this mentor... This link opens in a new window

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Abstract
Emergentna onesnaževala so skupina naravnih in sintetičnih spojin, katerih prisotnost v okolju narašča kot posledica antropogenih dejavnosti in vsesplošne kemične obremenitve sodobne družbe. Zaradi pomanjkanja podatkov o njihovi toksičnosti in dolgoročnih učinkih na okolje, trenutno še niso vključena v okoljsko regulativo, zato je nujen razvoj občutljivih analiznih metod za njihovo določanje. V analitiki vodnih vzorcev se je kot korak priprave vzorca uveljavila predvsem ekstrakcija na trdno fazo (SPE) z uporabo SPE kolon, ki ji sledi instrumentalna analiza z LCMS/MS. Kljub temu pa se v zadnjih letih zaradi svoje vsestranskosti, hitrega postopka in manjše porabe organskih topil vse bolj uveljavlja disperzivna mikroekstrakcija na trdno fazo (DMSPE). Ena izmed njenih prednosti je tudi uporaba mešanic različnih sorbentov, kar poveča možnosti interakcij z večjim številom raznolikih analitov. V diplomskem delu sem s preizkušanjem različnih tipov sorbentov ter optimizacijo ekstrakcijskih in desorpcijskih pogojev razvila DMSPE metodo za ekstrakcijo dvajsetih onesnaževal z raznolikimi kemijsko-fizikalnimi lastnostmi iz vodne matrice. Ekstrakte sem analizirala z UHPLC-DAD oziroma UHPLC-MS/MS metodo s separacijo na reverznofazni kromatografski koloni. Končni določeni izkoristki spojin so znašali med 18 % in 110 % (od tega je 9 spojin doseglo zadovoljive izkoristke nad 50 %). S tem so bili doseženi predkoncentracijski faktorji med 5 in 29. Relativni standardni odkloni (RSD) izkoristkov ekstrakcije vseh spojin so bili manjši od 10 %.

Language:Slovenian
Keywords:DMSPE, emergentna onesnaževala, UHPLC-DAD, UHPLC-MS/MS
Work type:Bachelor thesis/paper
Typology:2.11 - Undergraduate Thesis
Organization:FKKT - Faculty of Chemistry and Chemical Technology
Year:2023
PID:20.500.12556/RUL-149537 This link opens in a new window
COBISS.SI-ID:163683075 This link opens in a new window
Publication date in RUL:07.09.2023
Views:485
Downloads:49
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Secondary language

Language:English
Title:Development of dispersive solid phase microextraction for selected environmental pollutants
Abstract:
Emerging pollutants represent a group of natural and synthetic compounds whose presence in the environment is increasing due to anthropogenic activities and the chemicalization of modern society. These compounds with unknown toxicities and long-term effects, have not yet been subject to environmental regulations. Therefore, the development of ultrasensitive multi-residue analytical methods for their determination is necessary. In water analysis, solid-phase extraction (SPE) using SPE cartridges has been widely utilized as a sample preparation step, followed by instrumental analysis using LC-MS/MS. However, in recent years, dispersive micro solid-phase extraction (DMSPE) has gained recognition for its versatility, rapid procedure, and reduced consumption of organic solvents. Notably, DMSPE allows for the use of mixtures of various sorbents, expanding the range of possible interactions with diverse analytes. In this study, various sorbent types were tested, and extraction and desorption conditions were optimized to develop a DMSPE method for the determination of twenty selected pollutants with diverse physicochemical properties from water samples. The extracts were analysed using UHPLC-DAD or UHPLC-MS/MS with separation on a reversephase chromatographic column. The achieved recovery rates for the target compounds ranged from 18% to 110% (with 9 compounds exhibiting satisfactory recoveries above 50%). This resulted in preconcentration factors ranging from 5 to 29. The relative standard deviation (RSD) for the extraction recoveries of all compounds was below 10%.

Keywords:DMSPE, emerging pollutants, UHPLC-DAD, UHPLC-MS/MS

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