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1.
Anal Methods ; 15(38): 5071-5077, 2023 10 05.
Artigo em Inglês | MEDLINE | ID: mdl-37743796

RESUMO

This works presents a novel screen-printed carbon electrode modified with nickel hydroxide nanoparticles and chitosan (Ni(OH)2/CS/SPCE) for the non-enzymatic flow injection amperometric detection of glucose. The electrode was modified by drop-casting a suspension of the synthesised nanocomposite onto the screen-printed electrode and dried for 1 hour at room temperature. EDX analysis was used to investigate the chemical composition of the electrode before and after modifying. The electrochemical response of the unmodified SPCE and modified electrode was initially investigated by cyclic voltammetry (CV) using 0.1 M NaOH as the supporting electrolyte. CVs showed catalytic activity for glucose oxidation using the Ni(OH)2/CS/SPCE at 0.55 V. During flow injection analysis (FIA), 0.60 V and 1.5 mL min-1 were identified as the optimal potential and flow rate, respectively. A wide linear range of detection was observed (0.2 to 10.0 mM) with a sensitivity and limit of detection of 913 µA mM-1 cm-2 and 0.0174 mM, respectively. The modified electrode also displayed excellent repeatability (RSD = 0.47%, n = 20) and good reproducibility (RSD = 2.52%, n = 6). The modified electrode was shown to be very selectivity for glucose over other interferences commonly found in human blood samples. The practicality of the developed flow injection-amperometric system (FIA-Amp) was validated by the quantification of glucose in real serum samples, where results were in close agreement with those obtained from the local hospital.


Assuntos
Quitosana , Humanos , Níquel/química , Análise de Injeção de Fluxo , Reprodutibilidade dos Testes , Glucose/análise , Hidróxidos , Eletrodos
2.
J Phys Chem A ; 127(23): 5039-5047, 2023 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-37257064

RESUMO

Many recent research studies have reported indirect methods for the detection and quantification of OH radicals generated during photocatalysis. The short lifespan and high reactivity of these radicals make indirect detection using probes such as coumarin a more viable quantification method. Hydroxyl radical production is commonly monitored using fluorescence spectroscopy to determine the concentration of the compound 7-hydroxycoumarin, which is formed from hydroxyl radical attack on coumarin. There are, however, a number of additional hydroxylated coumarins generated during this process, which are less amenable to detection by fluorescence spectroscopy. Consequently, limitations and inaccuracies of this method have previously been reported in the literature. As an alternative approach to those previously reported, this work has developed an electrochemical screening method using coumarin as a OH radical trap, that is capable of in situ monitoring of not only 7-hydroxycoumarin, but all the main mono-hydroxylated products formed. As a result, this technique is a more representative and comprehensive method for the quantification of OH radicals produced by photocatalysts using coumarin as a probe molecule. Moreover, the electroanalytical method provides a portable, rapid, sensitive, and accurate in situ method for the monitoring of OH radical formation without the need for sample preparation.

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