Određivanje metilnih estera masnih kiselina GC - FID metodom

master's thesis

• Title (english): Determination of fatty acid methyl esters by GC - FID method
• Author: Goran Filipović
• Mentor: Lidija Furač (mentor)
• Committee member: Lidija Furač (predsjednik povjerenstva)
• Committee member: Matija Cvetnić (član povjerenstva)
• Committee member: Dajana Kučić Grgić (član povjerenstva)
• Granter: University of Zagreb; Faculty of Chemical Engineering and Technology; Zagreb
• Defense date and country: 2022-09-27, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

Metilni esteri masnih kiselina (engl. fatty acid methyl esters, FAME) su spojevi koji nastaju reakcijom transesterifikacije. To je postupak u kojem dolazi do modifikacije estera, a temelji se na njihovoj reakciji s alkoholom metanolom u prisutnosti baznog katalizatora. Kako su masti i ulja po kemijskom sastavu esteri, podložni su ovakvoj vrsti reakcije. Razlog zbog kojeg se prevode u metilne estere je radi uspješnijeg određivanja profila masnih kiselina u željenim uzorcima metodom koja se u tu svrhu najčešće koristi, a to je plinska kromatografija. U ovome radu provedena je validacija analitičke metode za određivanje metilnih estera masnih kiselina plinskom kromatografijom s detektorom plamene ionizacije (engl. gas chromatography with a flame ionization detector, GC–FID). Određivale su se odabrane izvedbene karakteristike validacije: selektivnost, linearnost, granica detekcije i granica kvantifikacije, točnost i preciznost. Analiza je provedena i na uzorku ricinusovog ulja, slijepoj probi i realnom uzorku, čime se provela i djelomična validacija postupka metilacije te postupka pripreme uzorka gdje su se odredile izvedbene karakteristike točnosti i preciznosti. Validacija predstavlja postupak kojim se utvrđuje da je odabrana metoda prikladna za namijenjenu svrhu. S obzirom da dobiveni rezultati zadovoljavaju zadane kriterije prihvatljivosti, zaključuje se da odabrana GC–FID metoda odgovara određivanju metilnih estera masnih kiselina.

Abstract (english)

Fatty acid methyl esters (FAME) are compounds that are formed by the transesterification reaction. It is a process in which esters are modified and it is based on their reaction with alcohol methanol in the presence of a base catalyst. As fats and oils are chemically esters, they are subject to this type of reaction. The reason why they are converted into methyl esters is to determine the profile of fatty acids more successfully in the desired samples by the method that is most often used for this purpose, which is gas chromatography. In this paper, the validation of the analytical method for the determination of fatty acid methyl esters by gas chromatography with a flame ionization detector (GC–FID) was performed. Selected performance characteristics of the validation were determined: selectivity, linearity, limit of detection and limit of quantification, accuracy and precision. The analysis was carried out on a sample of castor oil, a blank test and a real sample, where a partial validation of the methylation procedure and the sample preparation procedure was carried out and the performance characteristics of accuracy and precision were determined. Validation is a procedure that determines that the chosen method is suitable for the intended purpose. Given that the results obtained meet the set acceptability criteria, it is concluded that the selected GC–FID method corresponds to the determination of fatty acid methyl esters.

• Keywords: masne kiseline; metilni esteri masnih kiselina; plinska kromatografija; validacija; ricinusovo ulje
• Keywords (english): fatty acids; fatty acid methyl esters; gas chromatography; validation; castor oil
• Language: croatian
• URN:NBN: urn:nbn:hr:149:309268
• Study programme: Title: Applied Chemistry - Graduate study; specializations in: Environmental chemistry and green technologies, Advanced materials and technologies, Applied organic chemistry; Course: Environmental chemistry and green technologies; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra primijenjene kemije (magistar/magistra primijenjene kemije)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Closed access
• Created on: 2023-03-23 14:04:08