| Sažetak | U posljednje se vrijeme sve češće raspravlja o štetnosti pojedinih farmaceutika odnosno antibiotika na okoliš, ali i na zdravlje ljudi. Zasad ne postoji zakon koji bi zabranio njihovu primjenu ili je barem smanjio. Dapače, njihova potrošnja se iz godine u godinu sve više povećava i gotovo ju je nemoguće spriječiti. U ovom radu razvijene su metode priprave uzoraka za analizu trinaest farmaceutski aktivnih tvari (albendazol, azitromicin, etodolak, febantel, imatinib, levamisol, linezolid, omeprazol, prazikvantel, sulfafurazol, sulfametazin, tiamulin, torasemid) u uzorcima vode i sedimenta i to ekstrakcija miješalom i ultrazvučna ekstrakcija. U svrhu određivanja optimalnih uvjeta ekstrakcije miješalom korištena su čista organska otapala pri različitim pH vrijednostima vode, uz različite volumene otapala za desorpciju, pri različitim vremenima trajanja ekstrakcije i desorpcije kao i pri različitim temperaturama ekstrakcije. Ultrazvučna ekstrakcija provedena je čistim organskim otapalima (kao i njihovim smjesama) te smjesama otapala s kiselinama i lužinama. Utvrđeno je da je za optimalne uvjete ekstrakcije farmaceutika iz vode (ekstrakcije miješalom) najbolje čisto organsko otapalo, metanol, volumena 5 mL pri temperaturi ekstrakcije i desorpcije 30 °C i pH vrijednosti vode 3,0. Isto tako, za optimalne uvjete ekstrakcije farmaceutika iz sedimenta ultrazvukom odabrano je čisto organsko otapalo, metanol, volumena 10 mL pri temperaturi ekstrakcije 25 °C. Učinkovitost ekstrakcije kvantitativno je određena tekućinskom kromatografijom ultra visoke djelotvornosti. Nakon provođenja postupka optimizacije, metoda je validirana i primijenjena na realnim uzorcima. |
| Sažetak (engleski) | In recent times, there has been increasing discussion about the harmful effects of certain pharmaceuticals, in other words antibiotics, on the environment, but also on human health. At present, there is no law forbidding or decreasing their use. In fact, their use is increasing year by year and the increase is almost impossible to stop. In this paper, methods of sample preparation are developed for analysis of thirteen pharmaceutically active compounds (albendazole, azithromycin, etodolac, febantel, imatinib, levamisole, linezolid, omeprazole, praziquantel, sulfafurazole, sulfamethazine, tiamulin, torasemide) in water and sediment samples – stir bar sorptive extraction and ultrasound extraction. In order to determine optimal conditions for stir bar sorptive extraction, pure organic solvents were used at different pH values of water, with differing volumes of solvents for desorption, at differing time intervals of extraction and desorption, as well as at differing temperatures of extraction. Ultrasound extraction was done by using pure organic solvents (and their mixtures) and mixtures of solvents with acids and bases. It was thenceforth determined that for optimal conditions of extraction of pharmaceuticals from water (stir bar sorptive extraction) pure organic solvent, methanol, volume 5 mL at extraction and desorption temperatures of 30°C and water pH value of 3.0 is best used. Furthermore, for optimal extraction conditions of pharmaceuticals from sediments using ultrasound extraction, a pure organic solvent, methanol, volume 10 mL, at extraction temperature of 25 °C was chosen. The efficacy of extraction was quantitatively determined by ultra high-performance liquid chromatography. After the optimization process, the method was validated and applied to real samples. |
