A novel sensor based on a modification of glassy carbon electrode (GCE) with NH2-functionalized multi-walled carbon nano-tubes (NH2fMWCNTs) is reported and its applicability to the electrochemical sensing of Propafenone (PPF) demonstrated. The electrochemical catalytic activity was also utilized as a sensitive detection method for the investigation of the detailed redox mechanism of PFF using cyclic and and differential pulse voltammetry. The surface morphology of the sensor was investigated by SEM armed with EDX probe. Electrochemical impedance spectroscopy was employed as well to define the electron transfer capability of modified and bare electrodes. Key experimental and instrumental conditions related to electrochemical determination by cyclic, differential pulse, and square wave voltammetry, such as amount of modifier, pH, scan rate, accumulation time and potential were studied and optimized. The results have shown a significant enhancement of the peak current after modifying the electrode; the calibration curves of PPF offering good linearity from 0.1 to 10 μM, limit of quantification (LOQ) being 0.03 μM and limit of detection (LOD) 0.01 μM, both when using DPV technique. The proposed sensor was successfully applied to the determination of PFF in dosage form without any special purification, separation or pre-treatment steps. The results of analyses obtained with the proposed sensor were satisfactory and fully statistically relevant.
- MeSH
- Anti-Arrhythmia Agents MeSH
- Electrodes MeSH
- Technology, Pharmaceutical instrumentation methods MeSH
- Dielectric Spectroscopy MeSH
- Calibration MeSH
- Hydrogen-Ion Concentration MeSH
- Oxygen chemistry MeSH
- Dosage Forms * MeSH
- Limit of Detection MeSH
- Microscopy, Electron, Scanning MeSH
- Nanomedicine MeSH
- Nanotubes, Carbon chemistry MeSH
- Propafenone administration & dosage MeSH
- Carbon chemistry MeSH
- Publication type
- Journal Article MeSH
Voltammetric determination of Tartrazine (Tz) and Brilliant Blue FCF (BB) in their mixture using novel type of carbon black-polyethylene composite electrode (CBPCE) with renewable surface modified by carbon ink (CI) was developed. Electrochemical properties of the tested dyes were investigated in 0.1 mol L-1 Britton-Robinson (BR) buffer by cyclic voltammetry (CV) and linear scan voltammetry (LSV). Simultaneous determination of the dyes is based on the application of supporting electrolytes with different pH: 2.0 for Tz and 10.0 for BB. Under the optimum experimental conditions, linear concentration dependences in the concentration ranges from 0.037 to 1.38 μmol L-1 for Tz and from 0.025 to 2.52 μmol L-1 for BB were obtained by LSV in the first-order derivative mode. Limits of detection (LODs) for Tz and BB were 0.019 and 0.011 μmol L-1, respectively. The modified electrode showed good stability and reproducibility and was successfully applied for the determination of the mixture Tz and BB in a candy and soft drink products.
- Publication type
- Journal Article MeSH
In this report, voltammetry with linear scan and chronopotentiometric stripping (CPS) with constant current were used for the analysis of doxorubicin (DOX) at a hanging mercury drop electrode (HMDE). CPS was used for the study of DOX in situ electrochemical reduction in adsorbed state and for ex situ (adsorptive transfer) analysis of the drug. For the first time, CPS was used to study the reversible reduction of the DOX quinine moiety at –0.45 V (vs Ag|AgCl|3 M KCl) as well as electrode processes giving rise to an irreversible signal around –1.45 V at the HMDE in 0.2 M acetate or Britton–Robinson buffers at different pH values. The dependence of the latter signal on pH revealed involvement of protonation equilibria; however, neither CV nor CPS data confirmed the catalytic character of the electrode reaction previously suggested by other authors. The CPS method was also applied to monitor the DOX interaction with double- (ds) and single-stranded (ss) DNA. In the presence of dsDNA, more pronounced changes in DOX signal intensity were observed, in agreement with a strong intercalation of the DOX redox centre into the DNA double helix.
The mechanism of electrochemical oxidation of rutin on a glassy carbon electrode was studied at different pH by using several electrochemical techniques (cyclic, linear sweep, differential pulse and square-wave voltammetry) in order to give deeper insight into the mechanism of electrochemical oxidation of rutin and adsorption of its oxidation products on a glassy carbon electrode. It was determined that the rutin oxidation process on a glassy carbon electrode is reversible, pH dependent and includes the transfer of 2 e– and 2 H+. The products of electrochemical oxidation strongly adsorb on the electrode surface. Maximum surface coverage, ?max, decreased with increasing scan rate from 3.4 × 10–9 mol cm–2 at scan rate 20 mV s–1 to 1.5 × 10–9 mol cm–2 at scan rate 100 mV s–1 and adsorption equilibrium constant was log K = 4.57 ± 0.05. Antioxidant properties of rutin were investigated by a Trolox equivalent antioxidant capacity (TEAC) assay. It was found that the TEAC values of rutin depend on concentration and the EC50 value of rutin amounted 0.23.
In this paper, the d(GCGAAGC) heptamer and the closely related d(GCGAGC) hexamer are examined via electrochemical (cyclic voltammetry) and spectroscopic (circular dichroism) methods. Dramatic changes in the CD spectroscopic and CV electrochemical properties, induced by the loss of only one single nucleotide (A), are detected. The CD spectra and native polyacrylamide gel electrophoresis (PAGE) confirmed structural changes taking place in the relevant chain-like oligodeoxynucleotide assemblies. Dedicated studies suggest that the heptamer (Hp) possesses a hairpin structure, whereas the hexamer (Hx) appears to be rather a duplex. Both of the structures exhibited completely different adsorption behavior at the hanging mercury drop electrode, and this factor was readily confirmed by means of elimination voltammetry with linear scan (EVLS). We established that the Hp hairpin (~-1300 mV), compared to the Hx duplex (~-1360 mV), is the thermodynamically favored electron acceptor. The adsorption isotherms were constructed based on the voltammetric peak height values, reflecting the reduction of the adenine (A) and cytosine (C) moieties as well as the oxidation of the 7,8-dihydroguanine (7,8-DHG) moieties. Finally, as revealed by the spectroscopic and electrochemical results, Hx forms a bimolecular antiparallel homo-duplex carrying both Watson-Crick base pairs (CG or GC) and mismatched edge-to-edge base pairs (GA or AG).
The analytical performance of the clay paste electrode and graphene paste electrode was compared using square wave voltammetry (SWV) and cyclic voltammetry (CV). The comparison was made on the basis of a paracetamol (PA) determination on both working electrodes. The influence of pH and SWV parameters was investigated. The linear concentration ranges were found to be 6.0 × 10-7-3.0 × 10-5 and 2.0 × 10-6-8.0 × 10-5 mol L-1 for clay paste electrode (ClPE) and graphene paste electrode (GrPE), respectively. The detection and quantification limits were calculated as 1.4 × 10-7 and 4.7 ×10-7 mol L-1 for ClPE and 3.7 × 10-7 and 1.2 × 10-6 mol L-1 for GrPE, respectively. Developed methods were successfully applied to pharmaceutical formulations analyses. Scanning electron microscopy and energy-dispersive X-ray spectroscopy were used to characterize ClPE and GrPE surfaces. Clay composition was examined with wavelength dispersive X-ray (WDXRF).
- MeSH
- Electrochemical Techniques methods MeSH
- Electrodes MeSH
- Graphite * chemistry MeSH
- Clay MeSH
- Acetaminophen analysis MeSH
- Carbon chemistry MeSH
- Publication type
- Journal Article MeSH
New screen-printed sensor with a boron-doped diamond working electrode (SP/BDDE) was fabricated using a large-area linear antenna microwave chemical deposition vapor system (LA-MWCVD) with a novel precursor composition. It combines the advantages of disposable printed sensors, such as tailored design, low cost, and easy mass production, with excellent electrochemical properties of BDDE, including a wide available potential window, low background currents, chemical resistance, and resistance to passivation. The newly prepared SP/BDDEs were characterized by scanning electron microscopy (SEM) and Raman spectroscopy. Their electrochemical properties were investigated by cyclic voltammetry and electrochemical impedance spectroscopy using inner sphere ([Fe(CN)6]4-/3-) and outer sphere ([Ru(NH3)6]2+/3+) redox probes. Moreover, the applicability of these new sensors was verified by analysis of the anti-inflammatory drug lornoxicam in model and pharmaceutical samples. Using optimized differential pulse voltammetry in Britton-Robinson buffer of pH 3, detection limits for lornoxicam were 9 × 10-8 mol L-1. The oxidation mechanism of lornoxicam was investigated using bulk electrolysis and online electrochemical cell with mass spectrometry; nine distinct reaction steps and corresponding products and intermediates were identified.
- MeSH
- Boron * chemistry MeSH
- Electrodes MeSH
- Electrolysis * MeSH
- Oxidation-Reduction MeSH
- Spectrum Analysis, Raman MeSH
- Publication type
- Journal Article MeSH
Electric spark discharge was employed as a green, fast and extremely facile method to modify disposable graphite screen-printed electrodes (SPEs) with copper, nickel and mixed copper/nickel nanoparticles (NPs) in order to be used as nonenzymatic glucose sensors. Direct SPEs-to-metal (copper, nickel or copper/nickel alloys with 25/75, 50/50 and 75/25wt% compositions) sparking at 1.2kV was conducted in the absence of any solutions under ambient conditions. Morphological characterization of the sparked surfaces was performed by scanning electron microscopy, while the chemical composition of the sparked NPs was evaluated with energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy. The performance of the various sparked SPEs towards the electro oxidation of glucose in alkaline media and the critical role of hydroxyl ions were evaluated with cyclic voltammetry and kinetic studies. Results indicated a mixed charge transfer- and hyroxyl ion transport-limited process. Best performing sensors fabricated by Cu/Ni 50/50wt% alloy showed linear response over the concentration range 2-400μM glucose and they were successfully applied to the amperometric determination of glucose in blood. The detection limit (S/N 3) and the relative standard deviation of the method were 0.6µM and <6% (n=5, 2µM glucose), respectively. Newly devised sparked Cu/Ni graphite SPEs enable glucose sensing with distinct advantages over existing glucose chemical sensors in terms of cost, fabrication simplicity, disposability, and adaptation of green methods in sensor's development.
