| Abstract | Potrošnja vode zadnjih desetljeća uslijed rastućeg broja stanovništva, nekontrolirane urbanizacije i industrijalizacije znatno se povećala i danas predstavlja visokovrijedno dobro. Održivi razvoj u budućnosti u svom načelu mora kontrolirati i detektirati onečišćivala svih sirovina a poglavito vode. Stoga razvoj i validacija metoda za određivanje pseudopostojanih onečišćivala u vodama, ima veliki značaj u procesu očuvanja životne sredine.
U pseudopostojana onečišćivala ubrajaju se svi spojevi koji se ne bi trebali nalaziti u okolišu, a u njega dospijevaju antropološkim putem. Razvoj i validacija metoda za pseudopostojana onečišćivala je nužna kako bi ih se moglo redovito pratiti u okolišu, ali i u otpadnim i pitkim vodama. Potpuna validacija metoda zahtijeva ispitivanje svih izvedbenih karakteristika metode, a one su: specifičnost/selektivnost, linearnost, točnost, istinitost, preciznost, granica detekcije i kvantifikacije, radno područje i robusnost. Najbolje metode za njihovo praćenje su kromatografske metode vezane na spektrometar masa kojima se omogućuje istovremena detekcija, identifikacija i kvantifikacija ispitivanih analita. Cilj ovog rada je bio validirati metodu za određivanje antibiotika, antiparazita, antireumatika i antivirotika (klozantel, gentamicin, baricitinib i ivermektin) te ispitati karakteristike i na temelju rezultata zaključiti zadovoljava li analitička metoda kriterije prihvatljivosti. Razvoj metode prvo je proveden na HPLC-DAD kromatografskom sustavu pri čemu su određivani sljedeći validacijski parametri: specifičnost/selektivnost, linearnost, osjetljivost, preciznost, iskoristivost, granica detekcije i kvantifikacija. Nakon toga metoda je transverirana na HPLC-MS/MS uređaj. |
| Abstract (english) | Water consumption has increased significantly in recent decades due to the growing population, uncontrolled urbanization and industrialization, and today it represents a highvalue commodity. In principle, sustainable development in the future must control and detect pollutants in all raw materials, especially water. Therefore, the development and validation of methods for the determination of pseudo-persistent pollutants in water is of great importance in the process of environmental protection. Pseudo-persistent pollutants include all compounds that should not be found in the environment, but which reach it through anthropological means. The development and validation of methods for
pseudo-persistent pollutants is necessary so that they can be regularly monitored in the environment, but also in waste and drinking water. Full method validation requires examination of all performance characteristics of the method, namely: specificity/selectivity, linearity, accuracy, truthfulness, precision, limit of detection and quantification, working area and robustness. The best methods for their monitoring are chromatographic methods connected to a mass spectrometer, which enable simultaneous detection, identification and quantification of the analyzed analytes. The aim of this work was to validate the method for determining antibiotics, antiparasitics, antirheumatics and antivirals (clozantel, gentamicin, baricitinib and ivermectin) and to examine the characteristics and based on the results to conclude whether the analytical method meets the acceptance criteria. The development of the method was first carried out on the HPLC-DAD chromatographic system, where the following validation parameters were determined: specificity/selectivity, linearity, sensitivity, precision, usability, detection limit and quantification. After that, the method was transferred to the HPLC-MS/MS device. |
