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Electrochemical determination of histamine

dc.contributor.advisorŠvarc-Gajić, Jaroslava
dc.contributor.otherMalbaša, Radomir
dc.contributor.otherRajaković, Ljubinka
dc.contributor.otherŠvarc-Gajić, Jaroslava
dc.creatorStojanović, Zorica
dc.date.accessioned2018-12-19T17:10:38Z
dc.date.available2018-12-19T17:10:38Z
dc.date.issued2011-09-23
dc.identifier.urihttps://www.cris.uns.ac.rs/DownloadFileServlet/Disertacijadisertacija.pdf?controlNumber=(BISIS)76992&fileName=disertacija.pdf&id=143&source=NaRDuS&language=srsr
dc.identifier.urihttps://www.cris.uns.ac.rs/record.jsf?recordId=76992&source=NaRDuS&language=srsr
dc.identifier.urihttps://www.cris.uns.ac.rs/DownloadFileServlet/IzvestajKomisije152413143517040.pdf?controlNumber=(BISIS)76992&fileName=152413143517040.pdf&id=11203&source=NaRDuS&language=srsr
dc.identifier.uri/DownloadFileServlet/IzvestajKomisije152413143517040.pdf?controlNumber=(BISIS)76992&fileName=152413143517040.pdf&id=11203
dc.identifier.urihttp://nardus.mpn.gov.rs/123456789/10369
dc.description.abstractU ovom radu su razvijene elektrohemijske metode za određivanje histamina. U svim elektrohemijskim ispitivanjima korišćena je hronopotenciometrija. Istraživanja su obuhvatila optimizaciju uslova elektroanalitičkih tehnika i upoređivanje mehanizama generisanja analitičkog signala primenom različitih radnih elektroda, razvoj odgovarajućeg postupka pripreme uzoraka za analizu i samo određivanje histamina u hrani i piću. Ispitana je mogućnost primene čvrste zlatne elektrode, tankoslojne živine i tankoslojne niklove elektrode za elektrohemijsko određivanje histamina. U slučaju elektrooksidacije histamina, razjašnjeni su mehanizmi generisanja signala na primenjenim elektrodama. Optimizacija uslova elektroanalitičkih tehnika obuhvatila je odabir odgovarajućeg pomoćnog elektrolita i njegove koncentracije, ispitivanje uticaja početnog potencijala i struje oksidacije na analitički signal analita. Pored toga, za svaki elektrohemijski sistem definisana su osetljivost i reproduktivnost, selektivnost, kao i opseg linearnosti. Primenom tankoslojne niklove elektrode uočena je pojava adsorpcionog koncentrovanja analita, te su u slučaju ovog elektrohemijskog sistema ispitani i uticaji vremena adsorpcije i temperature ispitivanog medijuma na analitički signal histamina. Na tankoslojnoj živinoj elektrodi analitički signal se generisao usled direktne oksidacije histamina primenom konstantne struje. Na ostale dve elektrode, pored elektrodnih reakcija odvijale su se i hemijske reakcije, tako da se oksidacija histamina u oba slučaja odigravala po ECE mehanizmu (elektrodna reakcija – hemijska reakcija – elektrodna reakcija). Na čvrstoj zlatnoj elektrodi, generisanje signala je bilo posledica oksidacije histamina elektrogenerisanim hlorom, dok se u slučaju tankoslojne niklove elektrode radilo o kombinovanoj katalitičko‐adsorpcionoj hronopotenciometriji. Tankoslojna živina elektroda je pokazala dobru selektivnost pri koncentracijama aminokiselina i histamina nižim od 5 mg/dm3, dok je pri višim koncentracijama dolazilo do preklapanja analitičkih signala. Ostali elektrohemijski sistemi nisu pokazali odgovarajuću selektivnost. Najveća osteljivost je ostvarena primenom tankoslojne niklove elektrode (LOD = 0,11 mg/dm3), zatim sledi čvrsta zlatna elektroda (LOD = 0,27 mg/dm3) i na kraju tankoslojna živina elektroda (LOD = 1,31 mg/dm3). U okviru definisanja postupka pripreme uzoraka, ispitana je efikasnost različitih ekstrakcionih tehnika i različitih ekstragenasa u pogledu izdvajanja histamina iz uzoraka. Pored toga razvijeni su odgovarajući postupci prečišćavanja ekstrakata primenom preparativnih hromatografskih tehnika, i to na tankom sloju i na stubu adsorbensa. Po definisanju optimalnih uslova elektrohemijskog određivanje histamina, kao i razvijanja postupka pripreme uzoraka, histamin je određen u različitoj hrani i piću.sr
dc.description.abstractIn this work, the electrochemical methods for the determination of histamine were developed. All electrochemical investigations were carried out by chronopotentiometry. The research included optimization of the experimental parameters of electroanalytical techniques and comparison of the mechanism of the analytical signal generation by using the different working electrodes. Upon the development of sample preparation procedure, histamine was determined in different food and beverages. The possibility of applying solid gold electrodes, thin film mercury electrode and thin film nickel electrode for electrochemical determination of histamine was examined. The mechanisms of histamine electrooxidation on different working electrodes were explained and elaborated. Optimization of the experimental parameters of electroanalytical techniques included the selection of appropriate supporting electrolyte and its concentration, and investigation of the influence of initial potential and oxidation current on histamine analytical signal. Beside this, for each electrochemical system sensitivity and reproducibility, selectivity as well as linearity range were defined. The use of thin nickel film electrode resulted in adsorptive accumulation, and in that case the effects of accumulation time and medium temperature on histamine analytical signal were defined. On thin film mercury electrode, histamine analytical signal was generated due to direct oxidation of histamine by a constant current. On other two electrodes, electrode reactions were coupled with chemical reaction, and histamine oxidation was by ECE mechanism (electrode reaction – chemical reaction – electrode reaction). On solid gold electrode histamine was oxidized indirectly by electrogenerated chlorine, while in the case of thin film nickel electrode combination of catalytic and adsorptive chronopotentiomety was responsible for signal generation. Thin film mercury electrode showed good selectivity for histamine and amino acids concentrations below 5 mg/dm3, but higher concentrations caused the overlapping of analytical signals. Other electrochemical systems did not show adequate selectivity. The best sensitivity was achived by thin film nickel electrode (LOD = 0.11 mg/dm3), followed by a solid gold electrode (LOD = 0.27 mg/dm3), and by thin film mercury electrode (LOD = 1.31 mg/dm3). In order to define adequate sample preparation procedure, the efficiency of different extraction techniques and different solvents were tested for histamine extraction from the samples. Appropriate procedures for purification of extracts were defined as well, by applying preparative thin layer and column chromatography. After optimization of the electrochemical methods for histamine determination, as well as the procedure of sample preparation, developed methods were applied for histamine determination in various food and beverages.en
dc.formatapplication/pdf
dc.languagesr (latin script)
dc.publisherУниверзитет у Новом Саду, Технолошки факултетsr
dc.rightsAttribution-NonCommercial
dc.sourceУниверзитет у Новом Садуsr
dc.subjectHistaminsr
dc.subjectHistamineen
dc.subjectelektrohemijsko određivanjesr
dc.subjecthronopotenciometrijasr
dc.subjecttankoslojna živina elektrodasr
dc.subjectčvrsta zlatna elektrodasr
dc.subjecttankoslojna niklova elektrodasr
dc.subjectprehrambeni proizvodisr
dc.subjectelectrochemical determinationen
dc.subjectchronopotentiometryen
dc.subjectthin film mercury electrodeen
dc.subjectsolid gold electrodeen
dc.subjectthin film nickel electrodeen
dc.subjectfoodstuffsen
dc.titleElektrohemijsko određivanje histaminasr
dc.title.alternativeElectrochemical determination of histamineen
dc.typeDoktorska disertacijasr


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