Razvoj i validacija kromatografske metode za određivanje odabranih karboksilnih kiselina

master's thesis

• Title (english): Development and validation of a chromatographic method for the determination of selected carboxylic acids
• Author: Damjan Petrin
• Mentor: Sandra Babić (mentor)
• Committee member: Sandra Babić (predsjednik povjerenstva)
• Committee member: Kristina Tolić Čop (član povjerenstva)
• Committee member: Irena Škorić (član povjerenstva)
• Granter: University of Zagreb; Faculty of Chemical Engineering and Technology; Zagreb
• Defense date and country: 2023-09-08, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

Halooctene kiseline su dezinfekcijski nusprodukti koji nastaju kada se sirova voda dezinficira klorom. Djelovanje i štetnost halooctenih kiselina za ljudsko zdravlje još uvijek nije sasvim istraženo i stoga se neprestano razvijaju i optimiraju analitičke metode kojima se nadzire njihova koncentracija u obrađenim vodama. Kroz ovaj rad analizirane su kloroctena, trikloroctena i bromoctena kiselina na način da su derivatizacijom prevedene u estere, nakon čega su snimljeni NMR i UV-Vis spektri derivata, te su potom analizirane kromatografskom HPLC-DAD metodom. Dodatno je provedena i GC-MS analiza trikloroctene i bromoctene kiseline. NMR analizom potvrđena je uspješna derivatizacija trikloroctene i bromoctene kiseline te djelomična derivatizacija kloroctene kiseline. UV-Vis analizom ustanovljeni su apsorpcijski maksimumi dobivenih derivata. Uz kvalitativnu kromatografsku analizu, razvijena je i validirana HPLC-DAD metoda za kvantitativno određivanje trikloroctene i bromoctene kiseline. Sve ispitane izvedbene karakteristike validacije zadovoljene su obzirom na postavljene kriterije. GC-MS analizom uspješno su detektirane trikloroctena i bromoctena kiselina.

Abstract (english)

Haloacetic acids form as disinfection byproducts when raw water is disinfected with chlorine. Since the harmful and adverse effects of haloacetic acids on human health have not yet been fully investigated, analytical methods are constantly being developed and optimized to monitor their concentration levels in water. In this paper, chloroacetic, trichloroacetic and bromoacetic acids were analyzed in such a way that they were converted into esters by derivatization, after which the NMR and UV-Vis spectra of the derivatives were obtained, and then they were analyzed using the chromatographic HPLC-DAD method. Additionally, GC-MS analysis of trichloroacetic and bromoacetic acids was carried out. NMR analysis confirmed the successful derivatization of trichloroacetic and bromoacetic acids as well as the partial derivatization of chloroacetic acid. UV-Vis analysis was used to determine the absorption maxima of the derivatives. Along with the qualitative chromatographic analysis, a new method for quantitative analysis of trichloroacetic and bromoacetic acids was developed and validated. All validation characteristics that were examined have met the set criteria. Trichloroacetic and bromoacetic acid were successfully detected with GC-MS analysis.

• Keywords: dezinfekcijski nusprodukti; halooctene kiseline; derivatizacija; kromatografija; validacija metode
• Keywords (english): disinfection byproducts; haloacetic acids; derivatization; chromatography; method validation
• Language: croatian
• URN:NBN: urn:nbn:hr:149:954399
• Study programme: Title: Materials Science and Engineering - Graduate study; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra inženjer/inženjerka kemijskog inženjerstva (magistar/magistra inženjer/inženjerka kemijskog inženjerstva)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Open access
• Created on: 2023-09-14 13:46:14