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Authenticity of cereals and pseudocereals -development of new methods for the analysis of flour and final bakery products

dc.contributor.advisorAčanski, Marijana
dc.contributor.otherKravić, Snežana
dc.contributor.otherKondić-Špika, Ankica
dc.contributor.otherAčanski, Marijana
dc.creatorPastor, Kristian
dc.date.accessioned2018-03-19T13:27:03Z
dc.date.available2018-03-19T13:27:03Z
dc.date.issued2018-03-05
dc.identifier.urihttps://www.cris.uns.ac.rs/DownloadFileServlet/Disertacija151436895213038.pdf?controlNumber=(BISIS)106920&fileName=151436895213038.pdf&id=10848&source=NaRDuS&language=srsr
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dc.identifier.urihttps://www.cris.uns.ac.rs/DownloadFileServlet/IzvestajKomisije151436902793964.pdf?controlNumber=(BISIS)106920&fileName=151436902793964.pdf&id=10849&source=NaRDuS&language=srsr
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dc.identifier.urihttp://nardus.mpn.gov.rs/123456789/9225
dc.description.abstractU ovoj doktorskoj disertaciji analizirano je brašno strnih žita (pšenice, spelte, ječma, raži, tritikalea, ovsa), prosolikog žita (kukuruza) i pseudocerealija (heljde i amarantusa) primenom gasne hromatografije sa masenom spektrometrijom (GC-MS) u kombinaciji sa multivarijantnom analizom, u cilju ispitivanja mogućnosti za određivanje autentičnosti navedenih biljnih vrsta. U tu svrhu, iz brašna navedenih cerealija i pseudocerealija ekstrahovani su mali molekuli (lipidi i šećeri). Lipidne komponente brašna ekstrahovane su heksanom. Nakon višestrukog obezmašćivanja istih uzoraka brašna heksanom i sušenja, usledila je ekstrakcija šećernih komponenata 96%-tnim etanolom. Dobijeni heksanski i etanolni ekstrakti derivatizovani su odgovarajućim reagensima. Za derivatizacaju lipidnih komponenata korišćen je rastvor TMSH (trimetilsulfonijum hidroksida, 0,2 M u metanolu). Time se masne kiseline prevode u odgovarajuće metil-estre. Za derivatizaciju šećernih komponenata korišćen je etanolni rastvor natrijum-hidroksida i hidroksilamin-hidrohlorida u kombinaciji sa BSTFA (bis-(trimetilsilil-trifluoroacetamidom). Na taj način su prosti šećeri prevedeni u odgovarujuće trimetilsilil-oksime. Ovako pripremljeni ekstrakti uzoraka brašna su analizirani na GC–MS uređaju. Dobijeni hromatogrami međusobno pokazuju veliku sličnost, a naročito u okviru uzoraka iste botaničke vrste. U obradi hromatograma i masenih spektara, korišćen je MSD Productivity ChemStation program uz primenu Wiley 275 biblioteke masenih spektara. Dobijeni podaci analizirani su na tri načina. Prvi način podrazumeva kreiranje numeričkih matrica u modu ukupne jonske struje (TIC). Drugi postupak podrazumeva kreiranje numeričkih matrica izolovanjem karakterističnih fragmentnih jona sa hromatograma (kod lipida 74 m/z, a kod šećera 73 m/z u kombinaciji sa bar jednim od sledećih jona: 204 m/z, 217 m/z, i 361 m/z). Kod trećeg načina obrade podataka, analiza je urađena kreiranjem matrica primenom binarnog sistema (1/0), gde „1“ označava prisustvo određene komponente, a „0“ označava njeno odsustvo u posmatranom uzorku. Tako dobijeni podaci podvrgnuti su multivarijantnoj analizi primenom statističkih programa – PAST i STATISTICA. U sva tri slučaja ispitivani uzorci grupisani su u međusobno jasno odvojene grupe, prema odgovarajućoj biljnoj vrsti. Uočeno je jasno razlikovanje pseudocerealija (heljde i amarantusa) i prosolikog žita (kukuruza) od grupe strnih žita (pšenice, spelte, ječma, raži, tritikalea i ovsa). Primenjenim metodama postiže se manje selektivna klasifikacija biljnih vrsta u okviru strnih žita, sa izuzetkom uzoraka ovsa i spelte. Ovi rezultati pokazuju da je novim navedenim postupcima moguće utvrditi autentičnost brašna različitih botaničkih vrsta cerealija i pseudocerealija. Na isti način tretirani su i uzorci proizvedenog hleba (kore i sredine) u kojima je pšenično brašno supstituisano sa 0, 20, 40, 50, 60, 80 i 100% heljdinog brašna. Multivarijantnom analizom GC-MS podataka dobijaju se jasno odvojeni klasteri u skladu sa porastom udela brašna heljde u kori i sredini hleba. Najbolji rezultati postignuti su koreliranjem sastava i sadržaja ugljenohidratnih komponenata u kori hleba. Krajnji ishod razvoja ovih novih originalnih metoda je mogućnost njihove praktične primene u cilju rutinskih kontrola kvaliteta brašna i gotovih pekarskih proizvoda u laboratorijama, proizvodnim pogonima i inspekcijskim službama. Posebna pogodnost primene predloženih metoda je to što su one semi-kvalitativnog i semi-kvantitativnog karaktera, pa se mogu izvoditi bez tačne identifikacije eluirajućih malih molekulasr
dc.description.abstractIn this doctoral thesis various flour samples of small grains (wheat, spelt, barley, rye, triticale, oats), corn and pseudocereals (buckwheat and amaranth) were analyzed using gas chromatography - mass spectrometry (GC-MS) in combination with multivariate analysis, in order to examine the possibilities for determining the authenticity of the plant species listed. Small molecules (lipids and sugars) were extracted from flour samples of the above-mentioned cereals and pseudocereals. The lipid components of the flour were extracted with hexane. The extraction of sugar components from the same flour samples was performed with 96% ethanol solution, after multiple defatting with hexane and drying of the samples. The obtained hexane and ethanol extracts were derivatized with appropriate reagents. For the derivatization of the lipid components, a solution of TMSH (trimethylsulfonium hydroxide, 0.2 M in methanol) was used. Thus, the fatty acids were converted into the corresponding methyl esters. For the derivatization of the sugar components, an ethanol solution of sodium hydroxide and hydroxylamine hydrochloride combined with BSTFA (bis- (trimethylsilyl trifluoroacetamide) was used. Thus, the free sugars were converted into the corresponding trimethylsilyl oximes. The derivatized extracts prepared in this manner were analyzed on a GC -MS device. The obtained chromatograms were very similar, and especially within the samples of the same botanical species. In the processing of the chromatograms and mass spectra, MSD Productivity ChemStation program was used with the Wiley 275 Mass Spectra Library. The obtained data were processed in three ways. The first method involves the creation of numerical matrices in the total ion current mode (TIC). The second method involves the creation of numerical matrices by isolating characteristic ion fragments from the TIC chromatograms (74 m/z for the lipid components, and 73 m/z in combination with at least one of the following ions: 204 m/z, 217 m/z, and 361 m/z, for the sugar components). In the third way of data processing, the analysis was done by creating a matrix using a binary system (1/0), where “1” denotes the presence of a particular component, and “0” denotes its absence in the observed sample. The data thus obtained were subjected to multivariate analysis using statistical programs - PAST and STATISTICA. In all three cases, the analyzed samples were grouped in clearly separated groups according to the appropriate plant species. A clear distinction was observed between pseudocereals (buckwheat and amaranth), corn and the group of small grains (wheat, spelt, barley, rye, triticale, oats). The applied methods achieved a less selective classification of plant species within the group of small grains, with the exception of oats and spelt samples. These results show that it is possible to determine the authenticity of flour of various botanical species of cereals and pseudocereals, applying new methods described in this doctoral thesis. The samples of produced bread (crust and crumbs) in which wheat flour was substituted with 0, 20, 40, 50, 60, 80 and 100% of buckwheat flour were treated in the same way. Multivariate analysis of GC-MS data provided clearly separated clusters in accordance with the increase in the share of buckwheat flour in bread crusts and crumbs. The best results were achieved by correlating the composition and content of the carbohydrate components in bread crusts. The ultimate outcome of the development of these new original methods is the possibility of their practical application for the purpose of routine quality control of flour and bakery products in laboratories, production facilities and inspection services. A particular advantage of applying the proposed methods is that they are semiqualitative and semi-quantitative. Therefore, they can be performed without the exact identification of eluting small molecules (lipids and free sugars), nor their quantification using analytical standards.en
dc.languagesr (latin script)
dc.publisherУниверзитет у Новом Саду, Технолошки факултетsr
dc.relationinfo:eu-repo/grantAgreement/MESTD/Technological Development (TD or TR)/31066/RS//
dc.rightsAttribution
dc.sourceУниверзитет у Новом Садуsr
dc.subjectCerealijesr
dc.subjectCerealsen
dc.subjectpseudocerealijesr
dc.subjectbrašnosr
dc.subjecthlebsr
dc.subjectgasna hromatografijasr
dc.subjectmasena spektrometrijasr
dc.subjectmultivarijantna analizasr
dc.subjectautentičnostsr
dc.subjectpseudocerealsen
dc.subjectflouren
dc.subjectbreaden
dc.subjectgaschromatographyen
dc.subjectmass spectrometryen
dc.subjectmultivariate analysisen
dc.subjectauthenticityen
dc.titleAutentičnost cerealija i pseudocerealija – razvoj novih metoda analize brašna i gotovih pekarskih proizvodasr
dc.title.alternativeAuthenticity of cereals and pseudocereals -development of new methods for the analysis of flour and final bakery productsen
dc.typeDoktorska disertacijasr
dcterms.abstractAчански, Маријана; Кравић, Снежана; Кондић-Шпика, Aнкица; Aчански, Маријана; Пастор, Кристиан; Aутентичност цереалија и псеудоцереалија – развој нових метода анализе брашна и готових пекарских производа; Aутентичност цереалија и псеудоцереалија – развој нових метода анализе брашна и готових пекарских производа;


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