magistrsko delo
David Majer (Author), Matjaž Finšgar (Mentor), Tanja Pečnik (Co-mentor)

Abstract

Magistrska naloga prikazuje razvoj in validacijo elektroanaliznih metod za določanje molekul epinefrina (EP), askorbinske kisline (AK) in sečne kisline (SK) z elektrodo iz steklastega ogljika in tehniko angl. square-wave voltametrije. Metode smo razvili in validirali kot nadomestek tekočinski kromatografiji visoke ločljivosti in plinski kromatografiji. Za študij difuzijsko kontrolirane reverzibilnosti sistema kalijevega heksacianoferata in določitev oksidacijsko redukcijskih potencialov analitov smo uporabili tehniko ciklične voltametrije. V sklopu validacije smo za vsak analit posamično preverjali mejo zaznavnosti, mejo določljivosti, linearnost, točnost in natančnost. Izmerjene podatke smo testirali za normalnost s Q-Q grafom in Kolmogorov-Smirnovim statističnim testom. Pri vsaki metodi smo preverjali homoscedastičnost ali heteroscedastičnost umeritvenih točk z analizo ostankov, Hartleyjevim testom, Bartlettovim testom in Cochranovim testom. Zaradi heteroscedastičnega obnašanja analiznih podatkov pri vseh analitih, smo uporabili uteženo linearno regresijo (angl. weighted linear regression) in s tem izboljšali kakovost analitskih rezultatov. Z dobljenim utežnim modelom smo nato preverjali točnost in natančnost metod. Razvite in validirane metode smo uspešno uporabili za analizo realnih vzorcev. Določevali smo vsebnost EP v zdravilu, vsebnost AK v prehranskem dopolnilu in vsebnost SK v človeškem urinu.

Keywords

epinefrin;askorbinska kislina;sečna kislina;elektrokemijske metode;elektroda iz steklastega ogljika;validacija metode;utežna regresija;magistrske naloge;

Data

Language: Slovenian
Year of publishing:
Typology: 2.09 - Master's Thesis
Organization: UM FKKT - Faculty of Chemistry and Chemical Engineering
Publisher: [D. Majer]
UDC: 543.55(043.2)
COBISS: 31805443 Link will open in a new window
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Downloads: 279
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Other data

Secondary language: English
Secondary title: Development and validation of electroanalytical methods for the determination of epinephrine, ascorbic acid, and uric acid
Secondary abstract: The master thesis presents the development and validation of electroanalytical methods for the determination of epinephrine (EP), ascorbic acid (AK), and uric acid (SK) using glassy carbon electrode and square-wave voltammetry. The methods were developed and validated as an alternative to the high performance liquid chromatography and gas chromatography. The technique of cyclic voltammetry was used to investigate the diffusion-controlled reversibility of the potassium hexacyanoferrate system and to determine the oxidation-reduction potentials of the analytes. During validation, the detection limit, limit of quantitation, linearity, accuracy, and precision were determined for each analyte individually. The measured data were checked for normality using the Q-Q plot and the Kolmogorov-Smirnov statistical tests. The analysis of the residuals, Hartley's test, Bartlett's test, and Cochran's test were used to check the homoscedasticity or heteroscedasticity of the data for the design of calibration plots. Due to the observed heteroscedastic behavior of the analytical data for all three analytes, a weighted linear regression was used, thus improving the quality of analytical results. The accuracy and precision of the methods were then verified using the resulting weighted model. The developed and validated methods were successfully used for the analysis of real samples by determining the concentrations of EP in a drug, AK in a dietary supplement, and SK in human urine.
Secondary keywords: epinephrine;ascorbic acid;uric acid;electrochemical methods;glassy carbon electrode;method validation;weighted regression;
Type (COBISS): Master's thesis/paper
Thesis comment: Univ. v Mariboru, Fak. za kemijo in kemijsko tehnologijo
Pages: XV, 76 str.
ID: 11938945