Optimizacija i validacija HS SPME GC MS metode za određivanje alkohola, pirazina i furana u bezglutenskom kruhu

master's thesis

• Title (english): Optimization and validation of HS SPME GC MS method for the determination of alcohols, pyrazines and furans in gluten free bread
• Author: Anja-Matea Lovrić
• Mentor: Mirjana Hruškar (mentor)
• Granter: University of Zagreb; Faculty of Food Technology and Biotechnology; (Department of Food Quality Control); (Laboratory for Food Quality Control); Zagreb
• Defense date and country: 2016-09-30, Croatia
• Scientific / art field, discipline and subdiscipline: BIOTECHNICAL SCIENCES; Food Technology

Abstract

Cilj ovog istraživanja bilo je provesti optimizaciju i validaciju metode za određivanje spojeva iz skupine alkohola (17), pirazina (4) i furana (3) u uzorcima bezglutenskog kruha pomoću mikroekstrakcije na čvrstoj fazi (HS-SPME) i plinske kromatografije-masene spektrometrije (GC-MS). Optimizacija metode obuhvaćala je ispitivanje utjecaja temperature (40, 50 i 60 °C) i vremena ekstrakcije (30, 45 i 60 min) na količinu ekstrahiranih ciljanih spojeva. Validacija metode je provedena pri optimalnim uvjetima mikroekstrakcije, pri čemu su ključni parametri validacije bili selektivnost, linearnost, preciznost te granica detekcije i granica kvantifikacije. Temperatura 60 C i vrijeme 60 min pokazali su se optimalnim uvjetima za provođenje mikroekstrakcije ciljanih spojeva. Rezultati provedenih validacijskih eksperimenata dokazali su da je metoda selektivna, linearna unutar radnog područja, precizna i osjetljiva pri određivanju svih ciljanih spojeva. Budući da su zadovoljeni svi postavljeni kriteriji prihvatljivosti, može se zaključiti da je optimizirana HS-SPME/GC-MS metoda prikladna za određivanje alkohola, pirazina i furana u bezglutenskom kruhu.

Abstract (english)

The aim of this study was to optimize and validate the method for the determination of alcohols (17), pyrazines (4) and furans (3) in gluten-free bread using solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). Method optimization included determination of the influence of different temperatures (40, 50 and 60 °C) and extraction times (30, 45 i 60 min) on the amount of extracted compounds. Method was validated under optimal microextraction conditions, while key validation parameters were selectivity, linearity, and precision, limit of detection and limit of quantification. Temperature of 60 C and time 60 min showed to be optimal conditions for microextraction of target compounds. Results of validation experiments confirmed method's selectivity, linearity under working range, precision and sensitivity in determination of all target compounds. Since all validation citeria have been met, it can be concluded that optimized HS-SPME/GC-MS method is suitable for determination of alcohols, pyrazines and furans in gluten-free bread.

• Keywords: aromatski spojevi; bezglutenski kruh; HS-SPME/GC-MS; optimizacija; validacija
• Keywords (english): aroma compounds; gluten-free bread; HS-SPME/GC-MS; optimization; validation
• Language: croatian
• URN:NBN: urn:nbn:hr:159:504396
• Study programme: Title: Food Safety Management; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra inženjer/inženjerka upravljanja sigurnošću hrane (magistar/magistra inženjer/inženjerka upravljanja sigurnošću hrane)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Open access
• Created on: 2017-04-26 08:20:54