Voltammetric behavior and determination of the macrolide antibiotics azithromycin, clarithromycin and roxithromycin at a renewable silver – amalgam film electrode

[Display omitted] •Voltammetric characterization of AZI, CLA and ROX at Hg(Ag)FE was performed.•AZI, CLA and ROX were determined via optimized SWV and SW-AdSV procedures.•Protonated forms of AZI, CLA and ROX favored their adsorption on Hg(Ag)FE.•1H NMR chemical shift dependence of N-methyl proton si...

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Published in:Electrochimica acta 2017-03, Vol.229, p.334-344
Main Authors: Vajdle, Olga, Guzsvány, Valéria, Škorić, Dušan, Csanádi, János, Petković, Miloš, Avramov-Ivić, Milka, Kónya, Zoltán, Petrović, Slobodan, Bobrowski, Andrzej
Format: Article
Language:English
Subjects:
1H NMR
Adsorption
Adsorptivity
Antibiotics
Cathodic polarization
Electrodes
Linearity
Macrolide antibiotics
NMR
Nuclear magnetic resonance
Renewable silver-amalgam film electrode
Silver
Square wave adsorptive stripping voltammetry
Stripping
Voltammetry
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Summary:[Display omitted] •Voltammetric characterization of AZI, CLA and ROX at Hg(Ag)FE was performed.•AZI, CLA and ROX were determined via optimized SWV and SW-AdSV procedures.•Protonated forms of AZI, CLA and ROX favored their adsorption on Hg(Ag)FE.•1H NMR chemical shift dependence of N-methyl proton signals from pH.•Optimized SW-AdSV procedure was applied to determine ROX in Runac® tablet. The renewable silver-amalgam film electrode (Hg(Ag)FE) was applied for voltammetric characterization and determination of semi-synthetic macrolide antibiotics azithromycin (AZI), clarithromycin (CLA) and roxithromycin (ROX) in the Britton-Robinson buffer as supporting electrolyte ranging the pH from 4.0 to 11.9. All three macrolides showed reduction signals in fairly negative potential range. During direct cathodic square wave voltammetric (SWV) investigations conducted over the potential range from −0.75V to −2.00V vs SCE, either one or two reduction peaks were obtained in the potential range from −1.5 to −1.9V. The shapes and intensities of the signals depend on the applied pH values in wider pH ranges. For analytical purposes concerning the development of direct cathodic SWV and adsorptive stripping SWV (SW-AdSV) methods the neutral and slightly alkaline media were suitable as pH 7.2, pH 7.4 and pH 7.0 for AZI, CLA and ROX, respectively. Based on the cyclic voltammograms recorded at these pH values, adsorption-controlled electrode kinetics process can be proposed for all three macrolides. Furthermore, the water suppressed 1H NMR measurements in the pH range between 6.0 and 10.5 indicated that the macrolide molecules at the optimal analytical conditions are predominantly in protonated form via their tertiary amino groups which supported in all three cases their adsorption on the appropriately polarized Hg(Ag)FE electrode. The optimized direct cathodic SWV methods showed good linearity in concentration ranges 4.81–23.3μgmL−1, 1.96–28.6μgmL−1 and 1.48–25.9μgmL−1 for AZI, CLA and ROX, respectively. The development of the SW-AdSV methods resulted in the linear responses at lower concentration ranges as 1.0–2.46μgmL−1, 0.05–0.99μgmL−1 and 0.10–0.99μgmL−1, for AZI, CLA and ROX, respectively. The relative standard deviation for all developed methods was not higher than 1.0% except the SWV method for AZI with 4.7%. In the case of all three investigated macrolide antibiotics the protonated form of the tertiary amino group(s) at appropriate accumulation potential and time favored t
ISSN:0013-4686
1873-3859
DOI:10.1016/j.electacta.2017.01.146