<p>U okviru doktorske disertacije optimizovani su uslovi određivanja<br />metilestara masnih kiselina, uključujući i trans izomere, primenom<br />kapilarne gasne hromatografije–masene spektrometrije, na<br />kapilarnoj koloni SP-2560 (dužina x unutrašnji prečnik: 100 m x<br />0,25 mm, debljina sloja stacionarne likvidne faze 0,20 μm,<br />biscijanopropil polisiloksan). Korišćenjem standarnih rastvora<br />metilestara masnih kiselina optimizovani su temperaturni program,<br />odnos razdeljivanja i uslovi akvizicije podataka SCAN tehnikom.<br />Razvijena je metoda za pripremu uzoraka u cilju određivanja sastava<br />masnih kiselina u prehrambenim proizvodima gasnom<br />hromatografijom–masenom spektrometrijom zasnovana na<br />istovremenoj mikrotalasnoj ekstrakciji i esterifikaciji (SMEE).<br />Validacija metode je izvedena poređenjem sa rezultatima dobijenim<br />gasnom hromatografijom–masenom spektrometrijom nakon<br />ekstracije po Soxhlet-u i derivatizacije masnih kiselina u metilestre<br />masnih kiselina. Rezultati dobijeni primenom razvijene i referentne<br />metode bili su statistički isti, kako u pogledu sastava masnih<br />kiselina, tako i efikasnosti ekstrakcije. Rezultati su pokazali da su<br />prednosti SMEE u odnosu na konvencionalnu metodu: kratko vreme<br />pripreme uzoraka i samim tim manja potrošnja energije, kao i<br />upotreba malih količina skupih organskih rastvarača. Dobro slaganje<br />rezultata dobijenih primenom referentne i metode zasnovane na<br />istovremenoj mikrotalasnoj ekstrakciji i esterifikaciji pokazuje da bi<br />se SMEE mogla primeniti kao rutinska metoda za pripremu uzoraka<br />prehrambenih proizvoda u cilju određivanja trans masnih kiselina<br />(TFA). Određen je sastav masnih kiselina, sa posebnim akcentom na<br />trans masne kiseline, u 273 uzoraka prikupljenih sa našeg tržišta u<br />periodu od juna 2006. do juna 2009. godine. Sadržaj trans masnih<br />kiselina u analiziranim uzorcima prehrambenih proizvoda, sirovina i<br />međuproizvoda koji se koriste u pekarskoj i konditorskoj industriji,<br />kretao se u veoma širokom intervalu, od 0,0% do čak 48,7%.<br />Prosečan sadržaj trans masnih kiselina iznosio je 0,2% u uljima,<br />6,5% u jestivim margarinima, 19,9% u margarinima za domaćinstvo,<br />9,8% u industrijskim margarinima, 24,3% u namenskim mastima,<br />10,8% u masnim punjenjima, 1,6% u mlečnim proizvodima, 10,9%<br />u slanom trajnom pecivu, 10,2% u čajnom pecivu, 6,3% u tvrdom<br />keksu, 11,0% u vafel proizvodima, 10,6% u čokoladnim<br />proizvodima i 9,2% u karamelama. Od ukupno 124 analizirana<br />uzorka, koja se ne koriste za direktnu upotrebu u ishrani (namenske<br />masti, masna punjenja, industrijski i margarini za domaćinstvo) 86<br />uzoraka (69,3%) sadrži više od 5% trans masnih kiselina, 25<br />(20,2%) sadrži manje od 5% TFA, dok u 13 uzoraka (10,5%) nije<br />detektovano prisustvo trans izomera. Od ukupno 140 analiziranih<br />uzoraka, koji se koriste za direktnu upotrebu u ishrani 74 uzoraka<br />(52,8%) sadrži više od 2% trans masnih kiselina, 20 (14,3%) sadrži<br />manje od 2% TFA, dok u 46 uzoraka (32,9%) nije detektovano<br />prisustvo trans izomera.</p> / <p>In this thesis, operating conditions for fatty acids determination,<br />including trans isomers, by capillary gas chromatography–mass<br />spectrometry, on capillary column SP-2560 (100 m x 0.25 mm, with<br />a 0.20 μm film thickness of biscyanopropyl polysiloxane liquid<br />phase) were optimized. Temperature program, split ratio and<br />condition of data acquisition by SCAN technique were optimized<br />using standard solutions of fatty acid methyl esters. A sample<br />preparation method based on simultaneous microwave assisted<br />extraction–esterification (SMEE) was developed for the<br />determination of the fatty acid composition of foodstuffs by gas<br />chromatography–mass spectrometry. The proposed sample<br />preparation method was validated by comparison with the reference<br />Soxhlet extraction method followed by derivatisation by methyl<br />ester formation and the same determination step. The fatty acid<br />compositions, as well as extraction efficiencies obtained by the use<br />of the proposed SMEE method and reference method were<br />statistically similar. The results showed that compared to the<br />conventional method, SMEE method offer the advantages of short<br />sample preparation time, low consumption of expensive organic<br />solvents and less energy consumption. This good agreement between<br />results provided, both by the SMEE and reference method,<br />demonstrates the usefulness of the former as the routine method for<br />the treatment of food samples prior to trans fatty acid analysis. The<br />fatty acid composition, and trans fatty acid content of 273 samples<br />collected from June 2006 to June 2009 year were determined. Trans<br />fatty acid content in the analysed samples of food products, raw<br />materials and intermediate products used in bakery and<br />confectionery industry was ranged in a very wide interval, from<br />0.0% to 48.7%. The average contents of trans fatty acids were 0.2%<br />in oils, 6.5% in the edible margarines, 19.9% in cooking margarines,<br />9.8% in industrial margarines, 24.3% in shortenings, 10.8 % in fat<br />fillings, 1.6% in dairy products, 10.9% in crackers, 10.2% in tea<br />cookies, 6.3% in biscuits, 11.0% in wafer products, 10.6% in<br />chocolate products and 9.2% in the caramels. From the total of 124<br />analysed samples, which are not used for direct human consumption<br />(shortenings, fat fillings, industrial and cooking margarines) 86<br />samples (69.3%) contained more than 5% trans fatty acids, 25 (20.2<br />%) contained less than 5% TFA, while 13 samples (10.5%) had an<br />undetectable levels of trans isomers. From a total of 140 analysed<br />samples, which are used for direct human consumption 74 food<br />samples (52.8%) contained more than 2% trans fatty acids, 20<br />(14.3%) contained less than 2% TFA, while 46 samples (32.9%) had<br />an undetectable levels of trans isomers.</p>
| Identifer | oai:union.ndltd.org:uns.ac.rs/oai:CRISUNS:(BISIS)82631 |
| Date | 04 October 2010 |
| Creators | Kravić Snežana |
| Contributors | Suturović Zvonimir, Abramović Biljana, Pucarević Mira, Švarc-Gajić Jaroslava |
| Publisher | Univerzitet u Novom Sadu, Tehnološki fakultet Novi Sad, University of Novi Sad, Faculty of Technology at Novi Sad |
| Source Sets | University of Novi Sad |
| Language | Serbian |
| Detected Language | Unknown |
| Type | PhD thesis |
| Format | application/pdf |
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