A compreensão do mecanismo de redução de compostos nitroheterocíclicos pode ser um parâmetro importante para correlacionar estudos entre a transferência eletrônica e a atividade biológica. O nitrofural (NF), fármaco pertencente ao grupo químico dos 5-nitro- heterocíclicos é ativo contra o Trypanosoma cruzi, agente etiológico da doença de Chagas, mas sua toxicidade impede o seu uso no tratamento desta parasitose. Desta forma, realizaram-se estudos do comportamento eletroquímico de três bioisósteros de NF, com substituição ora no heteroátomo do anel (O e S) ora na carbonila (O e S). As técnicas eletroquímicas de voltametria cíclica (VC), voltametria de pulso diferencial (VPD) e cronoamperometria (CRO) em meio aquoso e empregando eletrodo de carbono vítreo (ECV) como eletrodo de trabalho. A finalidade deste estudo foi compreender a influência do efeito estrutural sobre a atividade redox dos bioisósteros, pois os respectivos comportamentos eletroquímicos podem estar correlacionados com a ação biológica. Todos os processos de redução foram controlados por difusão, com a formação de único pico de redução (Ecp,1), sendo os análogos NT e NTS reduzidos em potencial ligeiramente mais negativo. A comparação dos resultados voltamétricos de NF com os obtidos para cada análogo demonstraram que todos os compostos apresentaram mecanismo de redução similar, envolvendo quatro elétrons, sendo em meio ácido o derivado hidroxilmina (RNHOH) o principal produto formado. Os dados obtidos por VPD e CRO corroboraram com estes resultados. Em meio alcalino e com prévio tratamento do eletrodo de carbono vítreo, constatou-se a formação de um pico de redução reversível, com envolvimento de um elétron para todos os compostos. Este pico refere-se à formação do nitro radical aniônico (R-NO2•-), mostrando-se estável na escala de tempo de medida da técnica de VC. Ademais, realizou-se estudo comparativo do efeito do polimento mecânico no ECV, com diamante e alumina, onde os dois procedimentos não apresentaram efeitos significativos diferentes sobre o comportamento voltamétrico dos análogos estudados. O nitro radical gerado eletroquimicamente em meio aquoso sofre reação de desproporcionamento com cinética de segunda-ordem, seguindo mecanismo ErCi (reação eletroquímica reversível seguida de uma reação química irreversível). Os valores da constante de velocidade k2 desta reação mostraram-se dependentes do pH, confirmando que o nitro radical aniônico é mais facilmente estabilizado em meio alcalino, uma vez que com a diminuição da acidez do meio, a protonação do radical torna-se mais difícil. O composto com a inclusão de dois átomos de enxofre (NTS) apresentou os menores valores de k2 indicando uma cinética de reação de desproporcionamento mais lenta praticamente em toda faixa de pH, com exceção em pH 8, com o qual os valores de k2 não apresentaram diferenças significativas. Portanto, os resultados obtidos neste estudo indicaram claramente a possibilidade de geração e detecção do nitro radical em meio aquoso a partir de compostos nitro-heterocíclicos, distinguindo-se de dados reportados na literatura em que se realizam estes estudos predominantemente em meio não aquoso ou misto. / The comprehension of the reduction mechanism of nitroheterocyclic compounds is an important study to know the parameters which can establish the correlation between electron transfer and biological activity. Nitrofural (NF), a drug containing the 5-nitro-heterocyclic moiety, is active against Trypanosoma cruzi, which is the etiologic agent of Chagas disease. Unfortunately, as NF toxicity prevents its use for the treatment against this illness, studies on the electrochemical behavior of three NF bioisosteres were performed. These bioisosteres contained substitutions (O and S) on either the heterocyclic atom or the carbonyl group. The electrochemical techniques herein used were cyclic voltammetry (CV), differential pulse voltammetry (DPV) and chronoamperometry (CRO) in aqueous medium employing a glassy carbon (GCE) as the working electrode. The purpose of this study was to understand the structural influence on the redox activity of these bioisosteres and to suggest the correlation possibilities between the electrochemical behavior and the biological activity. The reduction processes were all diffusion controlled in acidic medium, with the formation of a single peak reduction (Ecp,1), being the NT and NTS analogue reduced at a slightly less negative potential. The comparison between the NF voltammetric results and those obtained with each analogue showed that all compounds presented a similar reduction mechanism, involving four electrons, being the hydroxylamine derivative the main product formed. The obtained data by DPV and CRO corroborated these results. Additionally, in alkaline medium and with previous GCE treatment by polishing a reversible reduction peak formation was observed with the involvement of one electron for all compounds. This peak refers to the nitro-radical anion formation ((R-NO2•-), being stable in the CV time scale. Moreover, a comparative study was carried out on the mechanical effect in the GCE by polishing with diamond and alumina, showing that both procedures had no significant effect on the voltammetric behavior of the compounds. The nitro-radical electrochemically generated in aqueous medium undergoes disproportionation reaction with second-order kinetics, following the ErCi mechanism (reversible electrochemical reaction followed by an irreversible chemical reaction). The constant rate values (k2) for this reaction proved to be pH dependent, confirming that the nitro-radical anion is more easily stabilized in alkaline medium, since the decreasing acidity of the medium hinders the radical protonation. Complementarily, NTS compound showed the lowest values of k2, indicating a slower disproportionation reaction in almost all pH values, except at pH 8, in which the k2 values had no significant difference among all bioisosteres. Therefore, the obtained results in this study clearly showed that nitro-radical anion can be detected and formed in aqueous solution in contrast to what is reported in literature, in which it is predominantly stabilized in non-aqueous solution or in solvent mixture.

A compreensão do mecanismo de redução de compostos nitroheterocíclicos pode ser um parâmetro importante para correlacionar estudos entre a transferência eletrônica e a atividade biológica. O nitrofural (NF), fármaco pertencente ao grupo químico dos 5-nitro- heterocíclicos é ativo contra o Trypanosoma cruzi, agente etiológico da doença de Chagas, mas sua toxicidade impede o seu uso no tratamento desta parasitose. Desta forma, realizaram-se estudos do comportamento eletroquímico de três bioisósteros de NF, com substituição ora no heteroátomo do anel (O e S) ora na carbonila (O e S). As técnicas eletroquímicas de voltametria cíclica (VC), voltametria de pulso diferencial (VPD) e cronoamperometria (CRO) em meio aquoso e empregando eletrodo de carbono vítreo (ECV) como eletrodo de trabalho. A finalidade deste estudo foi compreender a influência do efeito estrutural sobre a atividade redox dos bioisósteros, pois os respectivos comportamentos eletroquímicos podem estar correlacionados com a ação biológica. Todos os processos de redução foram controlados por difusão, com a formação de único pico de redução (Ecp,1), sendo os análogos NT e NTS reduzidos em potencial ligeiramente mais negativo. A comparação dos resultados voltamétricos de NF com os obtidos para cada análogo demonstraram que todos os compostos apresentaram mecanismo de redução similar, envolvendo quatro elétrons, sendo em meio ácido o derivado hidroxilmina (RNHOH) o principal produto formado. Os dados obtidos por VPD e CRO corroboraram com estes resultados. Em meio alcalino e com prévio tratamento do eletrodo de carbono vítreo, constatou-se a formação de um pico de redução reversível, com envolvimento de um elétron para todos os compostos. Este pico refere-se à formação do nitro radical aniônico (R-NO2•-), mostrando-se estável na escala de tempo de medida da técnica de VC. Ademais, realizou-se estudo comparativo do efeito do polimento mecânico no ECV, com diamante e alumina, onde os dois procedimentos não apresentaram efeitos significativos diferentes sobre o comportamento voltamétrico dos análogos estudados. O nitro radical gerado eletroquimicamente em meio aquoso sofre reação de desproporcionamento com cinética de segunda-ordem, seguindo mecanismo ErCi (reação eletroquímica reversível seguida de uma reação química irreversível). Os valores da constante de velocidade k2 desta reação mostraram-se dependentes do pH, confirmando que o nitro radical aniônico é mais facilmente estabilizado em meio alcalino, uma vez que com a diminuição da acidez do meio, a protonação do radical torna-se mais difícil. O composto com a inclusão de dois átomos de enxofre (NTS) apresentou os menores valores de k2 indicando uma cinética de reação de desproporcionamento mais lenta praticamente em toda faixa de pH, com exceção em pH 8, com o qual os valores de k2 não apresentaram diferenças significativas. Portanto, os resultados obtidos neste estudo indicaram claramente a possibilidade de geração e detecção do nitro radical em meio aquoso a partir de compostos nitro-heterocíclicos, distinguindo-se de dados reportados na literatura em que se realizam estes estudos predominantemente em meio não aquoso ou misto. / The comprehension of the reduction mechanism of nitroheterocyclic compounds is an important study to know the parameters which can establish the correlation between electron transfer and biological activity. Nitrofural (NF), a drug containing the 5-nitro-heterocyclic moiety, is active against Trypanosoma cruzi, which is the etiologic agent of Chagas disease. Unfortunately, as NF toxicity prevents its use for the treatment against this illness, studies on the electrochemical behavior of three NF bioisosteres were performed. These bioisosteres contained substitutions (O and S) on either the heterocyclic atom or the carbonyl group. The electrochemical techniques herein used were cyclic voltammetry (CV), differential pulse voltammetry (DPV) and chronoamperometry (CRO) in aqueous medium employing a glassy carbon (GCE) as the working electrode. The purpose of this study was to understand the structural influence on the redox activity of these bioisosteres and to suggest the correlation possibilities between the electrochemical behavior and the biological activity. The reduction processes were all diffusion controlled in acidic medium, with the formation of a single peak reduction (Ecp,1), being the NT and NTS analogue reduced at a slightly less negative potential. The comparison between the NF voltammetric results and those obtained with each analogue showed that all compounds presented a similar reduction mechanism, involving four electrons, being the hydroxylamine derivative the main product formed. The obtained data by DPV and CRO corroborated these results. Additionally, in alkaline medium and with previous GCE treatment by polishing a reversible reduction peak formation was observed with the involvement of one electron for all compounds. This peak refers to the nitro-radical anion formation ((R-NO2•-), being stable in the CV time scale. Moreover, a comparative study was carried out on the mechanical effect in the GCE by polishing with diamond and alumina, showing that both procedures had no significant effect on the voltammetric behavior of the compounds. The nitro-radical electrochemically generated in aqueous medium undergoes disproportionation reaction with second-order kinetics, following the ErCi mechanism (reversible electrochemical reaction followed by an irreversible chemical reaction). The constant rate values (k2) for this reaction proved to be pH dependent, confirming that the nitro-radical anion is more easily stabilized in alkaline medium, since the decreasing acidity of the medium hinders the radical protonation. Complementarily, NTS compound showed the lowest values of k2, indicating a slower disproportionation reaction in almost all pH values, except at pH 8, in which the k2 values had no significant difference among all bioisosteres. Therefore, the obtained results in this study clearly showed that nitro-radical anion can be detected and formed in aqueous solution in contrast to what is reported in literature, in which it is predominantly stabilized in non-aqueous solution or in solvent mixture.

This Thesis deals with the construction of an electrochemical cell with two types of integrated composite electrodes based on carbon films. Using these electrodes, the voltammetric behavior of environmental pollutant triclosan (5-chlor-2-(2,4- dichlorophenoxy)phenol) was studied. For the construction of composite electrodes, graphite and glassy carbon were used as conductive microparticles. Several types of polymers served as the nonconductive binder. For the measurements, combinations of graphite with polystyrene and graphite with polycarbonate were selected as optimum materials. From the dependence of peak heights on solution composition, a mixture of a buffer of pH 7 and methanol (1:9, V/V) was selected as the optimum medium. In this medium, concentration dependences were measured; calculated triclosan detection limit were 0,49 µmol dm-3 for carbon polystyrene composite electrode and 0,25 µmol dm-3 for carbon polycarbonate composite electrode, respectively. The possibility of further increasing the sensitivity of the determination by the accumulation step was studied. Accumulation of triclosan on carbon polystyrene composite electrode was observed, but the increase in response was connected with the loss of repeatability. Accumulation of triclosan on carbon polycarbonate composite electrode was...

<p>Cilj&nbsp; ove&nbsp; doktorske&nbsp; disertacije&nbsp; je&nbsp; bio&nbsp; razvoj&nbsp; brzih&nbsp; i&nbsp; pouzdanih&nbsp; voltametrijskih&nbsp; metoda zasnovanih na primeni jednostavnih i savremenih elektroda/senzora na bazi ugljeničnih materijala (ugljenične&nbsp; paste&nbsp; napravljene&nbsp; od&nbsp; grafitnog&nbsp; praha&nbsp; i&nbsp; parafinskog&nbsp; ulja&nbsp; i&nbsp; &scaron;tampanih&nbsp; ugljeničnih elektroda)&nbsp; za&nbsp; određivanje&nbsp; H ₂O₂u&nbsp; odabranim&nbsp; složenim&nbsp; model&nbsp; i&nbsp; realnim&nbsp; uzorcima.&nbsp; U&nbsp; tu&nbsp; svrhu, ispitana je primenljivost različitih radnih elektroda. Amperometrijska&nbsp; metoda&nbsp; zasnovana&nbsp; na&nbsp; elektrodi&nbsp; od&nbsp; ugljenične&nbsp; paste&nbsp; (CPE)&nbsp; zapreminski modifikovane&nbsp; sa&nbsp; 5%&nbsp; (m:m)&nbsp; MnO2 je,&nbsp; pri&nbsp; optimizovanim&nbsp; uslovima&nbsp; i&nbsp; pri&nbsp; radnom&nbsp; potencijalu&nbsp; od 0,40 V&nbsp; u&nbsp; odnosu&nbsp; na&nbsp; zasićenu&nbsp; kalomelovu&nbsp; elektrodu&nbsp; (ZKE)&nbsp; u&nbsp; fosfatnom&nbsp; puferu&nbsp; pH&nbsp; 7,50&nbsp; kao pomoćnom elektrolitu, omogućila kvantifikaciju H ₂O₂ u opsegu koncentracija od 1,4 do 65 &micro;g mL -1 sa&nbsp; relativnom&nbsp; standardnom&nbsp; devijacijom&nbsp; (RSD)&nbsp; manjom&nbsp; od&nbsp; 10%.&nbsp; Ova&nbsp; metoda&nbsp; je&nbsp; primenjena&nbsp; za određivanje sadržaja H ₂O₂u uzorcima podzemne vode iz centralnog Banata (Pokrajina Vojvodina, Srbija)&nbsp; tretirane&nbsp; Fentonovim&nbsp; (Fe²⁺ i&nbsp; H ₂O₂ )&nbsp; i&nbsp; Fentonu-sličnim&nbsp; (Fe ³⁺ i&nbsp; H ₂O₂ )&nbsp; reagensima&nbsp; u&nbsp; cilju uklanjanja&nbsp; prirodnih&nbsp; organskih&nbsp; materija&nbsp; (POM)&nbsp; pri&nbsp; čemu&nbsp; su&nbsp; kori&scaron;ćene&nbsp; različite&nbsp; početne koncentracije&nbsp; gvožđa&nbsp; i&nbsp; različiti&nbsp; odnosi&nbsp; molarnih&nbsp; koncentracija&nbsp; gvožđa&nbsp; i&nbsp; H ₂O₂ .&nbsp; Utvrđeno&nbsp; je&nbsp; da oksidaciono&nbsp; stanje&nbsp; gvožđe&nbsp; (Fe²⁺ ili&nbsp; Fe ³⁺)&nbsp; i&nbsp; molarni&nbsp; odnos&nbsp; jona&nbsp; Fe&nbsp; i&nbsp; H₂O₂ utiču&nbsp; na&nbsp; stepen potro&scaron;nje/razgradnje&nbsp; H₂O₂<br />u&nbsp; podzemnoj&nbsp; vodi&nbsp; sa&nbsp; visokim&nbsp; sadržajem&nbsp; POM.&nbsp; Takođe,&nbsp; u&nbsp; slučaju Fentonu-sličnog&nbsp; procesa,&nbsp; za&nbsp; sve&nbsp; početne&nbsp; koncentracije&nbsp; Fe ³⁺ i&nbsp; H ₂O_{2 ,}&nbsp; signifikantna&nbsp; količina&nbsp; H ₂O₂ostaje&nbsp; neiskori&scaron;ćena,&nbsp; &scaron;to&nbsp; ukazuje&nbsp; na&nbsp; nižu&nbsp; efikasnost&nbsp; ovakvog&nbsp; sistema u&nbsp; poređenju&nbsp; sa&nbsp; Fentonovim procesom.&Scaron;tampana&nbsp; ugljenična&nbsp; elektroda&nbsp; (SPCE)&nbsp; zapreminski&nbsp; modifikovana&nbsp; sa&nbsp; MnO 2 kao medijatorom&nbsp; je&nbsp; primenjena&nbsp; za&nbsp; određivanje&nbsp; sadržaja&nbsp; H₂O₂ u&nbsp; toku&nbsp; Fentonovog&nbsp; (Fe ²⁺ ,&nbsp; H₂O₂ )&nbsp; i vidljivom&nbsp; svetlo&scaron;ću&nbsp; potpomognutog&nbsp; foto-Fentonovog&nbsp; (Fe²⁺,&nbsp; H ₂O₂,&nbsp; h&nu;)&nbsp; procesa&nbsp; uklanjanja neonikotinoidnog&nbsp; insekticida&nbsp; acetamiprida&nbsp; (ACT).&nbsp; Pri&nbsp; optimizovanim&nbsp; uslovima&nbsp; (radni&nbsp; potencijal 0,40&nbsp; V&nbsp; u&nbsp; odnosu&nbsp; na&nbsp; ZKE,&nbsp; fosfatni&nbsp; pufer&nbsp; pH&nbsp; 7,50&nbsp; kao&nbsp; pomoćni&nbsp; elektrolit)&nbsp; amperometrijskog određivanja&nbsp; H ₂O₂ ,&nbsp; postignuta&nbsp; je&nbsp; linearnost&nbsp; u&nbsp; opsegu&nbsp; koncentracija&nbsp; 0,01&ndash;1,24&nbsp; mmol&nbsp; L-1(0,34&ndash; 42,2 &micro;g mL -1<br />) i vrednost RSD nije prelazila 4,2%. U ispitivanimuzorcima (nakon odgovarajućeg<br />pode&scaron;avanja pH vrednosti od 2,8 do 7,5 odmah nakon&nbsp; uzorkovanja radi stopiranja ili maksimalnog usporavanja&nbsp; procesa&nbsp; oksidacije,&nbsp; filtriranja,&nbsp; zamrzavanja&nbsp; i&nbsp; odmrzavanja&nbsp; neposredno&nbsp; pre&nbsp; merenja) sadržaj&nbsp; H ₂O₂ je&nbsp; određen&nbsp; metodom&nbsp; standardnog&nbsp; dodatka&nbsp; analiziranjem&nbsp; odgovarajućih amperometrijskih&nbsp; krivi.&nbsp; Paralelna&nbsp; HPLC-DAD&nbsp; merenja&nbsp; su&nbsp; vr&scaron;ena&nbsp; u&nbsp; cilju&nbsp; praćenja koncentracije/uklanjanja ACT. U slučaju foto-Fentonovog procesa (početne koncentracije 0,31; 2,0 i 3,0 mmol L -1 (70,0; 111,7 i 102,1 &micro;g mL -1 ) za ACT, Fe<br />²⁺ i H ₂O₂, redom) nakon 10 min H ₂O₂je izreagovao, a može se smatrati da je ACT uklonjen nakon 5 min. U toku Fentonovog procesa ACT je&nbsp; uklonjen&nbsp; nakon&nbsp; 20&nbsp; min&nbsp; tretmana&nbsp; i&nbsp; oko&nbsp; 10%&nbsp; početne&nbsp; koncentracije&nbsp; H ₂O₂ je&nbsp; ostalo&nbsp; u&nbsp; sistemu<br />neiskori&scaron;ćeno.CPE&nbsp; je&nbsp; povr&scaron;inski&nbsp; modifikovane&nbsp; kompozitom&nbsp; na&nbsp; bazi&nbsp; nanočestica&nbsp; Pt&nbsp; (&lt;&nbsp; 5&nbsp; nm)&nbsp; i grafitizovanog&nbsp; ugljenika&nbsp; (Pt-C,&nbsp; 10%&nbsp; Pt&nbsp; na&nbsp; Vulkanu&nbsp; XC72)&nbsp;&nbsp; etodom&nbsp; nano&scaron;enja&nbsp; kapi. Nemodifikovana&nbsp; CPE&nbsp; i&nbsp; modifikovana&nbsp; (Pt-C/CPE)&nbsp; su&nbsp;&nbsp; okarakterisane&nbsp; primenom&nbsp; SEM/EDS&nbsp; i&nbsp; CV merenja.&nbsp; Pt-C/CPE&nbsp; je&nbsp; pokazala&nbsp; izuzetne&nbsp; elektrokatalitičke&nbsp; osobine&nbsp; u&nbsp; pogledu&nbsp; elektrohemijskeredoks&nbsp; reakcije&nbsp; H<br />₂O₂ u&nbsp; poređenju&nbsp; sa&nbsp; nemodifikovanom&nbsp; CPE&nbsp; u&nbsp; fosfatnom&nbsp; puferu&nbsp; (0,1 mol&nbsp; L -1 ;<br />pH 7,50),&nbsp; a&nbsp; takođe&nbsp; i&nbsp; u&nbsp; acetatnom&nbsp; puferu&nbsp; (0,1&nbsp; mol&nbsp; L -1 ;&nbsp; pH&nbsp; 4,50)&nbsp; kao&nbsp;&nbsp; pomoćnim&nbsp; elektrolitima. Prilikom&nbsp; amperometrijskog&nbsp; određivanja&nbsp; H ₂O₂ primenom&nbsp; Pt-C/CPE&nbsp; u&nbsp; model&nbsp; sistemima, zadovoljavajuća linearnost je postignuta u koncentracionom opseguH₂O₂od 0,15 do 1,45 &micro;g mL -1 ,dok su vrednosti GO iznosile 0,06 &micro;g mL -1 (pH 7,50, radni potencijal 0,20 V) i 0,10 &micro;g mL -1 (pH<br />4,50,&nbsp; radni&nbsp; potencijal&nbsp; 0,50&nbsp; V).&nbsp; Optimizovane&nbsp; analitičke&nbsp; metode&nbsp; su&nbsp; primenjene&nbsp; za&nbsp; određivanje sadržaja H ₂O₂ u komercijalno dostupnim proizvodima za ličnu negu: rastvoru za dezinfekciju (pH 7,50)&nbsp; i&nbsp; rastvoru&nbsp; za&nbsp; či&scaron;ćenje&nbsp; kontaktnih&nbsp; sočiva&nbsp; (pH&nbsp; 4,50).&nbsp; Amperometrijski&nbsp; dobijeni&nbsp; rezultati&nbsp; su&nbsp; u dobrom&nbsp; slaganju&nbsp; sa&nbsp; rezultatima&nbsp; dobijenim&nbsp; primenom&nbsp; tradicionalne&nbsp; spektrofotometrijske&nbsp; metode bazirane&nbsp; na&nbsp; titanijum-sulfatu&nbsp; kao&nbsp; reagensu&nbsp; sa&nbsp; određenim&nbsp; koncentracijama&nbsp; 2,91%&nbsp; i&nbsp; 2,94%&nbsp; za<br />dezinfekcioni rastvor i 3,04% i 3,17% za rastvor zakontaktna sočiva, redom. RSD je bila manja od 2%.&nbsp; Postignuti&nbsp; rezultati&nbsp; su&nbsp; u&nbsp; dobrom&nbsp; slaganju&nbsp; sa&nbsp; sadržajem&nbsp; H<br />₂O₂deklarisanim&nbsp; od&nbsp; strane proizvođača (3%) u oba ispitivana uzorka. Pt-C/CPE je takođe testirana za praćenje koncentracije H₂O₂ u rastvoru za kontaktna sočiva u toku procesa njegove neutralizacije/razgradnje. Nakon 6 h procesa neutralizacije, 24,68&nbsp; &micro;g mL -1 je bila određena koncentracija H ₂O_{2 ,} &scaron;to je ispod dozvoljene<br />H₂O₂koncentracije u rastvoru za kontaktna sočiva imajući u vidu granicu koja izaziva iritaciju oka. CPE&nbsp; je&nbsp; povr&scaron;inski&nbsp; modifikovana&nbsp; vi&scaron;ezidnim&nbsp; ugljeničnim&nbsp; nanocevima&nbsp; (MWCNT)&nbsp; i kompozitima MnO 2 -MWCNT ili Pt-MWCNT metodom nano&scaron;enja kapi radi pripreme jednostavnih, osetljivih i pouzdanih voltametrijskih senzora za&nbsp; određivanje H ₂O₂u odabranom uzorku. Rezultati SEM/EDS&nbsp; analize&nbsp; kompozitnih&nbsp; materijala&nbsp; su&nbsp; potvrdili da&nbsp; su&nbsp; medijatori,&nbsp; čestice&nbsp; MnO 2 i&nbsp; Pt, nasumično&nbsp; raspoređeni na povr&scaron;ini MWCNT i zastupljeni sa blizu 5% (m:m) u kompozitu izraženo<br />preko Mn i Pt. CV merenja su vr&scaron;ena sa pripremljenim radnim elektrodama u acetatnom (pH 4,50), fosfatnom&nbsp; (pH&nbsp; 7,50)&nbsp; i&nbsp; boratnom&nbsp; (pH&nbsp; 9,18)&nbsp; puferu&nbsp; kako&nbsp; bi&nbsp; se&nbsp; okarakterisalo&nbsp; osnovno elektrohemijsko&nbsp; pona&scaron;anje&nbsp; H ₂O₂i&nbsp; odabrali&nbsp; pogodni&nbsp; radni&nbsp; potencijali&nbsp; za&nbsp; amperometrijsko određivanje ovog ciljnog analita. Pt- WCNT/CPE je primenljiva za rad kako u fosfatnom puferu pH&nbsp; 7,50&nbsp; tako&nbsp; i&nbsp; u&nbsp; acetatnom&nbsp; puferu&nbsp; pH&nbsp; 4,50&nbsp; V&nbsp; kako&nbsp; pri&nbsp; negativnim&nbsp; tako&nbsp; i&nbsp; pri&nbsp; pozitivnim&nbsp; radnim<br />potencijalima, pri&nbsp; čemu su vrednosti RSD uglavnom ispod 2,5%. U slučaju MnO 2<br />-MWCNT/CPE, na&nbsp; potencijalu&nbsp; 0,30&nbsp; V&nbsp; i&nbsp; vi&scaron;im&nbsp; vrednostima,&nbsp; oksidacioni&nbsp; signali&nbsp; H<br />₂O₂ su&nbsp; signifikantni&nbsp; u&nbsp; blago alkalnoj sredini (pH 7,50), pri pH 4,50 ova elektroda pokazuje nezadovoljavajuće pona&scaron;anje, dok&nbsp; pri pH 9,18 ima prihvatljive performanse. Granice određivanja (GO) su bile u oblasti &micro;g mL -1 . H ₂O₂ je&nbsp; određen&nbsp; u&nbsp; spajkovanom&nbsp; uzorku&nbsp; mleka&nbsp; metodom&nbsp; standardnog&nbsp; dodatka&nbsp; nakon&nbsp; odgovarajuće pripreme&nbsp; uzorka&nbsp; (pH&nbsp; pode&scaron;avanje&nbsp; i&nbsp; centrifugiranje)&nbsp; i&nbsp; primenom&nbsp; optimizovane&nbsp; amperometrijske procedure (acetatni pufer pH 4,50, radni&nbsp; potencijal-0,75 V) koristeći Pt-MWCNT/CPE kao radnu elektrodu. RSD za tri&nbsp; ponovljena merenja je iznosila 2,5%, dok je prinos metode bio ne&scaron;to veći od 71%.<br />Kompozitni materijali koji se sastoje od MWCNT i&nbsp; čestica na bazi Pd (Pd-MWCNT) ili Pt (Pt-MWCNT) su primenjeni za pripremu zapreminski modifikovanih SPCE (Pd-MWCNT-SPCE i Pt-MWCNT-SPCE)&nbsp; i&nbsp; povr&scaron;inski&nbsp; modifikovane&nbsp; SPCE&nbsp; (Pd-MWCNT/SPCE).&nbsp; Ove&nbsp; elektrode,&nbsp; kao&nbsp; i nemodifikovana&nbsp; SPCE&nbsp; i&nbsp; MWCNT-SPCE,&nbsp; su&nbsp; okarakterisane primenom&nbsp; CV&nbsp; i&nbsp; amperometrije&nbsp; u fosfatnom puferu pH 7,50 radi određivanja H ₂O₂ . Pd-MWCNT-SPCE i Pd-MWCNT/SPCE su se pokazale&nbsp; pogodnim&nbsp; za&nbsp; određivanje&nbsp; H ₂O₂ na&nbsp; radnim&nbsp; potencijalima&nbsp; između&nbsp; -0,50&nbsp; i&nbsp; 0,50&nbsp; V,&nbsp; a&nbsp; PtMWCNT-SPCE na ispitivanim radnim potencijalima od -0,80 do 0,70 V. Ove&nbsp; elektrode su zatim modifikovane&nbsp; enzimom&nbsp; glukoza&nbsp; oksidazom&nbsp; (GOx)&nbsp; metodom&nbsp; nano&scaron;enja&nbsp; kapi&nbsp; rastvora&nbsp; GOx&nbsp; i Nafion &reg; -a&nbsp; na&nbsp; njihovu&nbsp; povr&scaron;inu,&nbsp; pri&nbsp; čemu&nbsp; je&nbsp; optimizovana&nbsp; količina&nbsp; nanetog&nbsp; biofilma.&nbsp; GOx/PdMWCNT-SPCE&nbsp; je&nbsp; pokazala&nbsp; bolje&nbsp; analitičke&nbsp; performanse&nbsp; za&nbsp; određivanje&nbsp; glukoze&nbsp; u&nbsp; poređenju&nbsp; sa GOx/Pd- WCNT/SPCE.&nbsp; Kao&nbsp; optimalan&nbsp; radni&nbsp; potencijal&nbsp; GOx/Pd-MWCNT-SPCE&nbsp; je&nbsp; odabrana<br />vrednost&nbsp; potencijala&nbsp; -0,40&nbsp; V&nbsp; u&nbsp; odnosu&nbsp; na&nbsp; ZKE,&nbsp; sa&nbsp; zadovoljavajućom&nbsp; linearno&scaron;ću&nbsp; u&nbsp; ispitivanom opsegu&nbsp; koncentracija&nbsp; glukoze&nbsp; od&nbsp; 0,16&nbsp; do&nbsp; 0,97&nbsp; mmol&nbsp; L -1 (od&nbsp; 29,1&nbsp; do&nbsp; 174&nbsp; &micro;g&nbsp; mL -1),&nbsp; dok&nbsp; je&nbsp; GO iznosila 0,14 mmol L -1 (25 &micro;g mL<br />-1 ). Optimizovana metoda zasnovana na GOx/Pd-MWCNT-SPCE je&nbsp; uspe&scaron;no&nbsp; primenjena&nbsp; za&nbsp; određivanje&nbsp; glukoze&nbsp; u&nbsp; uzorku&nbsp; livadskog&nbsp; meda.&nbsp; Dobijeni&nbsp; rezultati&nbsp; su&nbsp; u dobroj&nbsp; saglasnosti&nbsp; sa&nbsp; onima&nbsp; dobijenim&nbsp; primenom&nbsp; komercijalno&nbsp; dostupnog&nbsp; aparata&nbsp; za&nbsp; merenje glukoze. Pogodan radni potencijal za GOx/Pt-MWCNT-SPCE je bio -0,50 V u odnosu na ZKE, pri čemu je zadovoljavajuća linearnost postignuta u ispitivanom opsegu koncentracija glukoze od 65,8 do 260,6 &micro;g mL -1 , sa GO 35 &micro;g mL -1 . Optimizovana metoda zasnovana na GOx/Pt-MWCNT-SPCE je&nbsp; uspe&scaron;no&nbsp; primenjena&nbsp; za&nbsp; određivanje&nbsp; glukoze&nbsp; u&nbsp; u&nbsp; uzorku&nbsp; belog&nbsp; grožđa&nbsp; i&nbsp; uzorku&nbsp; tableta (Traubenzucker-bonbons),&nbsp; pri&nbsp; čemu&nbsp; su&nbsp; dobijeni&nbsp; rezultati&nbsp; u&nbsp; dobroj&nbsp; saglasnosti&nbsp; sa&nbsp; rezultatima dobijenim primenom Accu-Chek aparata.<br />Na&nbsp; osnovu&nbsp; dobijenih&nbsp; rezultata&nbsp; može&nbsp; se&nbsp; zaključiti&nbsp; da&nbsp; su&nbsp; razvijene&nbsp; analitičke&nbsp; metode&nbsp; pre svega jednostavne, pouzdane i pogodne za dobijanje brzih informacija o sadržaju H ₂O₂ u različitim tipovima&nbsp; uzoraka.&nbsp; Svakako&nbsp; odabir&nbsp; pogodne&nbsp; radne&nbsp; elektrode,&nbsp; kao&nbsp; i&nbsp; optimizacija&nbsp; eksperimentalnih uslova su ključni faktori za uspe&scaron;no određivanje H ₂O₂</p> / null / <p>The aim of this doctoral dissertation was the development of fast and reliable voltammetric methods&nbsp; based&nbsp; on&nbsp; the&nbsp; application&nbsp; of&nbsp; simple&nbsp; and&nbsp; contemporary&nbsp; electrodes/sensors&nbsp; based&nbsp; on carbonaceous materials (carbon paste made of graphite powder and paraffin oil and screen printed carbon electrodes) for the determination of H <span id="cke_bm_571S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_571E" style="display: none;">&nbsp;</span>O₂ in the selected complex model and real samples.For this purpose, applicability of different working electrodes was investigated.The&nbsp; amperometric&nbsp; method&nbsp; based&nbsp; on&nbsp; carbon&nbsp; paste&nbsp; electrode&nbsp; (CPE)&nbsp; bulk- modified&nbsp; &nbsp;&nbsp; with 5% (m:m) MnO 2 , under optimized conditions, with a working potential of 0.40 V vs. the saturated calomel&nbsp; elect<span id="cke_bm_572E" style="display: none;">&nbsp;</span>rode&nbsp; (SCE)&nbsp; and&nbsp; a&nbsp; phosphate&nbsp; buffer&nbsp; solution&nbsp; (pH&nbsp; 7.50)&nbsp; as&nbsp; supporting&nbsp; electrolyte, enabled the quantitation of H <span id="cke_bm_577S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_577E" style="display: none;">&nbsp;</span>O₂in the concentration interval from 1.4 to 65 &micro;g mL &minus;1 with a relative standard deviation (RSD) of less than 10%. This meth<span id="cke_bm_578E" style="display: none;">&nbsp;</span>od was applied for the determination of the H<span id="cke_bm_583S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_583E" style="display: none;">&nbsp;</span>O₂consumption&nbsp; in&nbsp; samples&nbsp; of&nbsp; groundwater&nbsp; fro<span id="cke_bm_584E" style="display: none;">&nbsp;</span>m&nbsp; the&nbsp; Central&nbsp; Banat&nbsp; region&nbsp; (Province&nbsp; of Vojvodina, Serbia) treated by the Fenton (Fe ²⁺and H ₂O₂ ) and Fenton-&nbsp; like (Fe ³⁺and H ₂O₂ ) reagents to remove natural organic matter (NOM) at&nbsp; differentinitial concentrations of iron species, and of their molar ratios to the initial concentration of H₂O₂ . It was found that the form of Fe (Fe ²⁺ or Fe ³⁺ )and the molar&nbsp; ratio to H ₂O₂influenced the degree of the H₂O₂ decomposition in the groundwater with high NOM content. Besides, in the case of the Fenton-like process, for all initial doses of Fe ³⁺ and H<span id="cke_bm_604S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_604E" style="display: none;">&nbsp;</span>O₂, a sign<span id="cke_bm_605E" style="display: none;">&nbsp;</span>ificant amount of H<span id="cke_bm_610S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_610E" style="display: none;">&nbsp;</span>O₂ remained unused, whi<span id="cke_bm_611E" style="display: none;">&nbsp;</span>ch also indicates a lower efficiency of such system compared to the Fenton process. Screen&nbsp; printed&nbsp; carbon&nbsp; electrode&nbsp; (SPCE)&nbsp; bulk-modified&nbsp; with&nbsp; MnO&nbsp;₂ as&nbsp; a&nbsp; mediator&nbsp; was applied&nbsp; for&nbsp; amperometric&nbsp; determination&nbsp; of&nbsp; the&nbsp; H <span id="cke_bm_617S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_617E" style="display: none;">&nbsp;</span>O₂ content&nbsp; during&nbsp; the&nbsp; Fenton&nbsp; (Fe ²⁺ ,&nbsp; H <span id="cke_bm_624S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_624E" style="display: none;">&nbsp;</span>O₂)&nbsp; and <span id="cke_bm_625E" style="display: none;">&nbsp;</span>visible&nbsp; light-assisted<span id="cke_bm_618E" style="display: none;">&nbsp;</span>,&nbsp; photo-Fenton&nbsp; (Fe ^2+&nbsp; ,&nbsp; H <span id="cke_bm_631S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_631E" style="display: none;">&nbsp;</span>O₂ ,&nbsp; h&nu;)<span id="cke_bm_632E" style="display: none;">&nbsp;</span>&nbsp; based&nbsp; removal&nbsp; of&nbsp; neonicotinoid&nbsp; insecticide acetamiprid (ACT). Under&nbsp; optimized conditions (working potential of 0.40 V vs. SCE, phosphate buffer&nbsp; pH&nbsp; 7.50&nbsp; as&nbsp; supporting&nbsp; electrolyte)&nbsp; amperometric&nbsp; determination&nbsp; of&nbsp; H <span id="cke_bm_637S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_637E" style="display: none;">&nbsp;</span>O₂showed&nbsp; a&nbsp; linear dynamic range from 0.01 to 1.24 mmol L -1 (from 0.34 to 42.2 &micro;g mL -1) and the RSD did not exceed 4.2%. In the investigated samples (after appropriate pH adjustment from 2.8 to 7.5 instantly after the sampling<span id="cke_bm_638E" style="display: none;">&nbsp;</span> to stop or maximum decelerate the oxidation processes, filtering, and storage of the deep- frozen sample with defrosting immediately before the measurements) the H <span id="cke_bm_643S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_643E" style="display: none;">&nbsp;</span>O₂&nbsp; contents were determined by the standard addition method by analyzing the corresponding amperometric curves. Parallel HPLC-DAD measurements were performed to monito<span id="cke_bm_644E" style="display: none;">&nbsp;</span>r the concentration/removal of ACT. In the case of the photo- Fenton process (initial concentrations: 0.31; 2.0 and 3.0 mmol L -1 (70.0; 111.7 and 102.1 &micro;g mL -1 ) of ACT, Fe²⁺ and H <span id="cke_bm_650S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_650E" style="display: none;">&nbsp;</span>O₂, respec<span id="cke_bm_651E" style="display: none;">&nbsp;</span>tively) after 10 min of irradiation H <span id="cke_bm_656S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_656E" style="display: none;">&nbsp;</span>O₂ was&nbsp; consumed&nbsp; and&nbsp; it&nbsp; can&nbsp; be&nbsp; consi<span id="cke_bm_657E" style="display: none;">&nbsp;</span>dered&nbsp; that&nbsp; ACT&nbsp; was&nbsp; removed&nbsp; after&nbsp; 5&nbsp; min.&nbsp; During&nbsp; the&nbsp; Fenton process ACT was removed after 20 min of treatment and around 10% of the initial concentration of the H 2O2 remained still unused.<br />CPE&nbsp; was&nbsp; surface&nbsp; modified&nbsp; with&nbsp; a&nbsp; composite&nbsp; of&nbsp; Pt&nbsp; nanoparticles&nbsp; (&lt;&nbsp; 5&nbsp; nm)&nbsp; on&nbsp; graphitized carbon (Pt-C, 10% Pt on Vulcan XC72) by simply dropcoating method. The unmodified CPE and the&nbsp; modified&nbsp; one&nbsp; (Pt-C/CPE)&nbsp; were&nbsp; characterized&nbsp; by&nbsp;&nbsp; EM/EDS&nbsp; and&nbsp; CV&nbsp; measurements.&nbsp; The&nbsp; PtC/CPE showed remarkable electrocatalytic propertiestoward the electrochemical redox reaction of H<span id="cke_bm_662S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_662E" style="display: none;">&nbsp;</span>O₂ compared to&nbsp; modified CPE in phosphate buffer (0.1 mol L -1 ; pH 7.50), as well in acetatebuffer&nbsp; (0.1 mol&nbsp; L -1 ; pH .50) supporting&nbsp; electrolytes. Amperometry of&nbsp; H2O2 in the concentration range from 0.15 to 1.45 &micro;g mL -1 with the Pt-C/CPE showed acceptable linearity, while the obtained values of LOQs were 0.06 &micro;g mL -1&nbsp; (pH 7.50, working potential 0.20 V) and 0.10 &micro;g mL -1 (pH 4<span id="cke_bm_663E" style="display: none;">&nbsp;</span>.50, working potential 0.50 V). The proposed analytical&nbsp; methods were applied to the determination of the H 2O2 content in commercially available personal care products; i.e., disinfection (pH 7.50) and contact lens cleaning solutions (pH 4.50). The obtained amperometric results are in good agreement with those measured by traditional titanium sulfatereagent based spectrophotometric method with determined concentrations as 2.91% and 2.94%&nbsp; for the disinfection product, and 3.04% and 3.17% for the contact lens solution, respectively. RSD was lower than 2%. The obtained results are in a good agreement with the amounts of the H<span id="cke_bm_668S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_668E" style="display: none;">&nbsp;</span>O₂declared by producers (3%) in the both investigated samples. The Pt-C/CPE was also tested for monitoring of the H<span id="cke_bm_674S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_674E" style="display: none;">&nbsp;</span>O₂ residual concentration in contact lens&nbsp; solution&nbsp; during&nbsp; its&nbsp; neutralization/decomposition&nbsp; rocess.&nbsp; At&nbsp; 6&nbsp; h&nbsp; of<span id="cke_bm_675E" style="display: none;">&nbsp;</span>&nbsp; neutralization&nbsp; treatment 24.68 &micro;g mL -1 of the H <span id="cke_bm_680S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_680E" style="display: none;">&nbsp;</span>O₂was&nbsp; determined which is almost half of the allowedH2<span id="cke_bm_681E" style="display: none;">&nbsp;</span>O2 concentration in the case of the contact lens solution concerningthe limit of eye irritation. CPE&nbsp; was&nbsp; surface&nbsp;&nbsp; modified&nbsp; with&nbsp; multiwalled&nbsp; carbon&nbsp; nanotubes&nbsp; (MWCNT)&nbsp; and&nbsp; with composites of MnO₂-MWCNT or Pt-MWCNT by drop coating method to prepare simply, sensitive and reliable volta<span id="cke_bm_669E" style="display: none;">&nbsp;</span>mmetric sensors for the determination of H <span id="cke_bm_687S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_687E" style="display: none;">&nbsp;</span>O₂in selected sample. The results of the&nbsp; SEM/<span id="cke_bm_688E" style="display: none;">&nbsp;</span>EDS&nbsp; analysis&nbsp; of&nbsp; composite&nbsp; materials&nbsp; have&nbsp; confirmed&nbsp; that&nbsp; the&nbsp; mediators,&nbsp; MnO ₂ and&nbsp; Pt&nbsp; articles, are randomly distributed on the surface of MWCNT and represent nearly 5% (m:m) of the composite expressed as Mn and Pt. CV measurements were performed&nbsp; with prepared electrodes in acetate&nbsp; (pH&nbsp; 4.50),&nbsp; phosphate&nbsp; (pH&nbsp; 7.50)&nbsp; and&nbsp; borate&nbsp; (pH&nbsp; 9.18)&nbsp; buffers&nbsp; to&nbsp; characterize&nbsp; the&nbsp; basic electrochemical&nbsp; behavior&nbsp; of&nbsp; H <span id="cke_bm_694S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_694E" style="display: none;">&nbsp;</span>O₂ and&nbsp; to&nbsp; select&nbsp; the&nbsp; working&nbsp; potentials&nbsp; suitable&nbsp; for&nbsp; amperometric determination&nbsp; of&nbsp; this&nbsp; target&nbsp; analyte.&nbsp; The&nbsp; Pt-MWCNT/CPE&nbsp; performs&nbsp; well&nbsp; in&nbsp; phosphate&nbsp; buffer pH .50 and acetate buffer solution pH 4.50 in the&nbsp; negative as well as in the positive polarization range with RSD mainly lower than 2.5%. In case of MnO₂-MWCNT/CPE at <span id="cke_bm_695E" style="display: none;">&nbsp;</span>0.30 V and above the H<span id="cke_bm_701S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_701E" style="display: none;">&nbsp;</span>O₂oxidation signal is rem<span id="cke_bm_702E" style="display: none;">&nbsp;</span>arkable in slightly alkaline media (pH 7.50), at pH 4.50 this electrode showed poor behavior and at pH 9.18 offered acceptable performance. LOQs were in the &micro;g mL -1 concentration&nbsp; range.&nbsp; H<span id="cke_bm_707S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_707E" style="display: none;">&nbsp;</span>O₂was&nbsp; determined&nbsp; in&nbsp; a&nbsp; spiked&nbsp; milk&nbsp; sample&nbsp; by&nbsp; standard addition&nbsp; method after&nbsp; appropriate&nbsp; sample&nbsp; preparation&nbsp; (pH&nbsp; adjustment and&nbsp; centrifugation)&nbsp; and&nbsp; using&nbsp; optimized amperometric p<span id="cke_bm_708E" style="display: none;">&nbsp;</span>rocedure (acetate buffer pH 4.50, working potential -0.75 V) by Pt-MWCNT/CPE as a working electrode. RSD for three repeated measurements was 2.5%, while the recovery of the method was a bit higher than 71%. The&nbsp; composite&nbsp; materials&nbsp; consisting&nbsp; of&nbsp; MWCNT&nbsp; and&nbsp; Pd&nbsp; (Pd-MWCNT)&nbsp; or&nbsp; Pt&nbsp; containing particles&nbsp; (Pt-WCNT)&nbsp; were&nbsp; applied&nbsp; to&nbsp; the&nbsp; preparation&nbsp; of&nbsp; bulk- modified&nbsp; SPCEs&nbsp; (Pd-MWCNTSPCE and Pt-MWCNT-SPCE) and surface modifiedSPCE (Pd- MWCNT/SPCE). These electrodes, as well as unmodified SPCE and MWCNT-SPCE,&nbsp; were characterized by CV and&nbsp; amperometry&nbsp; in phosphate&nbsp; buffer&nbsp; solution&nbsp; of&nbsp; pH&nbsp; 7.50&nbsp; for&nbsp; the&nbsp; H<span id="cke_bm_713S" style="display: none;">&nbsp;</span>₂<span id="cke_bm_713E" style="display: none;">&nbsp;</span>O₂determination.&nbsp; Pd-MWCNT-SPCE&nbsp; and&nbsp; PdMWCNT/SPCEare convenient for the etermination of H 2O2 at working potentials from -0.50 to 0.50 V, and Pt-MWCNT-SPCE at investigated working potentials in the range from -0.80 to 0.70 V. These electrodes were then modified with glucose&nbsp; oxidase (GOx) by drop coating a solution of GOxand Nafion &reg; on their surface, whereby the applied amount of biococktail was optimized. GOx/PdMWCNT-SPCE&nbsp; showed&nbsp; better&nbsp; analytical&nbsp; performance&nbsp; for&nbsp; glucose&nbsp; determination&nbsp; in&nbsp; comparison with&nbsp; GOx/Pd-MWCNT/SPCE.&nbsp; The&nbsp; optimal&nbsp; working&nbsp; potential&nbsp; for&nbsp; GOx/Pd-MWCNT- SPCE&nbsp; was -0.40 V vs. SCE and <span id="cke_bm_714E" style="display: none;">&nbsp;</span>satisfactory linearity was obtained in the investigated glucose concentration range from 0.16 to 0.97 mmol L -1 (from 29.1 to 174&nbsp; &micro;g mL -1 ), hile the LOQ was 0.14 mmol L -1 (25 &micro;g mL -1 ). The optimized method based on GOx/Pd-MWCNT-SPCE was successfully applied to the determination of glucose in multifloral honey sample.&nbsp; The results are in a good agreement with those&nbsp; obtained by commercially available equipment for determination of glucose. Optimal working potential&nbsp; for&nbsp; GOx/Pt-MWCNT-SPCE&nbsp; was&nbsp; -0.50&nbsp; V&nbsp; vs.&nbsp; SCE,&nbsp; and&nbsp; the&nbsp;&nbsp; satisfactory&nbsp; linearity&nbsp; was obtained in the investigated concentration range ofglucose from 65.8 to 260.6&nbsp; &micro;g mL -1 , with LOQ of 35&nbsp; &micro;g mL -1 . The optimized method based on GOx/Pt- MWCNT-SPCE was successfully applied for determination of glucose in white grape and glucose tablets (Traubenzucker-bonbons) samples, whereby&nbsp; the&nbsp; obtained&nbsp; results&nbsp; were&nbsp; in&nbsp; a&nbsp; good&nbsp; agreement&nbsp; with&nbsp; the&nbsp; results&nbsp; obtained&nbsp; by&nbsp; Accu-Chek device. Based on the results, the developed analytical methods are first of all simple, reliable and suitable&nbsp; for&nbsp; obtaining&nbsp; fast&nbsp; information&nbsp; about&nbsp; the&nbsp; content&nbsp; of&nbsp; H ₂O₂ in&nbsp; different&nbsp; types&nbsp; of&nbsp; samples. Certainly the selection of a suitable working electrode, as well as the optimization of experimental conditions are key factors for the successful determination of H₂O₂.</p>