Razvoj metode z ionsko-izmenjevalno ekstrakcijo na trdno fazo za izbrana okoljska onesnaževala

Štuhec, Barbara (avtor), Prosen, Helena (mentor)

Emergentna onesnaževala so snovi naravnega ali sintetičnega izvora, ki zaradi širjenja človeških dejavnosti vse pogosteje vstopajo v okolje. Zaradi njihovih potencialno negativnih učinkov na ekosistem ter zdravje ljudi in živali, je pomembno razviti zanesljive analizne metode za njihovo določanje. Ker se emergentna onesnaževala v okolju nahajajo v sledovih, s koncentracijami od ng/L do μg/L, je predobdelava vzorca ključni del analiznega postopka. Za ekstrakcijo okoljskih vodnih vzorcev se je v zadnjih letih uveljavila ekstrakcija na trdno fazo (SPE), ki je primerna za spojine z raznolikimi fizikalno-kemijskimi lastnostmi. V diplomskem delu sem razvijala metodo z ionsko-izmenjevalno ekstrakcijo na trdno fazo za 20 izbranih emergentnih onesnaževal, ki sodijo v skupine zdravil, pesticidov, kozmetičnih sredstev, prehranskih aditivov in industrijskih kemikalij. Z metodo UHPLC-DAD sem preverjala rezultate optimizacije SPE pri višjih koncentracijah analitov (nekaj μg/L) ter izbrala ustrezno ekstrakcijsko kolono za nadaljnjo optimizacijo, ki sem jo pri nižjih koncentracijah analitov (nekaj ng/L) izvedla z metodo UHPLC-MS/MS. Preverila sem vpliv pH vzorca, vpliv pH raztopine za spiranje ter vpliv koncentracije, pH in moči elucijskega topila. Z optimizirano metodo SPE v kombinaciji z UHPLC-MS/MS sem lahko določila 16 od 20 izbranih analitov, od tega jih je 13 imelo zadovoljive izkoristke ekstrakcije (višje od 40 %). Optimizirana metoda je bila za vseh 16 analitov linearna v območju med 5 μg/L in 35 μg/L (R2 ≥ 0,990), ponovljivost metode je bila zadovoljiva za 14 analitov (RSD < 20 %).

• Jezik: Slovenski jezik
• Ključne besede: emergentna onesnaževala, ionsko-izmenjevalna SPE, UHPLC-DAD, UHPLC-MS/MS
• Vrsta gradiva: Diplomsko delo/naloga
• Organizacija: FKKT - Fakulteta za kemijo in kemijsko tehnologijo
• Leto izida: 2024
• PID: 20.500.12556/RUL-160785-3e73a3f9-0d84-f87b-a91c-36e83f0cdbe1
• Datum objave v RUL: 04.09.2024

Sekundarni jezik

• Jezik: Angleški jezik
• Naslov: Development of method with ion-exchange solid phase extraction for selected environmental pollutants

Izvleček

Emerging pollutants are compounds of natural or synthetic origin that enter the environment with increasing frequency due to the spread of human activities. Because of their potentially negative effects on the ecosystem, human and animal health it is important to develop reliable analytical methods for their determination. Emerging pollutants are found in trace amounts in the environment, with concentrations from ng/L to μg/L, therefore sample pretreatment is a crucial part of the analytical procedure. In recent years, solid phase extraction (SPE), which is suitable for compounds with diverse physicochemical properties, has been widely utilized. I developed the method using ion-exchange solid phase extraction for 20 selected emerging pollutants that belong to the groups of pharmaceuticals, pesticides, cosmetics, food additives and industrial chemicals. UHPLC-DAD method was used to monitor the results of SPE optimization at higher analyte concentrations (μg/L) to select the most suitable extraction column for further optimization, which was performed with UHPLC-MS/MS method at lower analyte concentrations (ng/L). In this study, pH of the sample, pH and effect of washing solution, as well as concentration, pH and strength of the elution solvent were optimized. Using the optimized SPE method combined with UHPLC-MS/MS, I was able to determine 16 of 20 selected analytes and 13 of them had satisfactory recoveries (higher than 40%). The linear range of optimized method was for all 16 analytes between 5 μg/L and 35 μg/L (R2 ≥ 0.990) and the reproducibility of the method was satisfactory for 14 target compounds (RSD < 20%).

• Ključne besede: emerging pollutants, ion-exchange SPE, UHPLC-DAD, UHPLC-MS/MS