A new modified ion-selective electrode with membranes of LaF3 single crystals with different internal contacts (solid steel or electrolyte) and with FexOy nanoparticles as loading was developed. The best response characteristic with linear potential change was found in the fluoride concentration range from 10−1 to 3.98 × 10−7 M. The detection limit for the electrolyte contact was determined at 7.41 × 10−8 M with a regression coefficient of 0.9932, while the regression coefficient for the solid contact was 0.9969. The potential change per concentration decade ranged from 50.3 to 62.4 mV, depending on whether the contact was solid or electrolytic. The prepared modified electrode has a long lifetime, as well as the possibility of application in different positions (solid contact), and it can also be used for the determination of iron ions. The electrode characterization was performed with scanning electron microscopy and elemental analysis with the technique of electron-dispersive X-ray spectroscopy.
Carbon nanotubes (CNTs) are widely used in electrochemical sensors due to their significant impact on the electroanalytical signal. However, there remain significant doubts regarding the origin of the improved electroanalytical response observed in CNT-based sensors, particularly concerning the precise role of CNTs in these systems. In particular, the origin of the electrochemical response is controversial, as it may be due to either electrocatalytic or non-electrocatalytic processes. The latter implies that the electroanalytical response is mainly governed by the mass transport phenomena within the porous CNT layer. This article briefly reviews the several comprehensive models based on the role of porosity (diffusion in a ‘thin-layer’) on the electrochemical behavior as well as on the electrocatalytic properties of CNTs to resolve conflicts arising from misinterpretations of the electroanalytical response of CNT-based sensors. However, even though there are some explanations and conclusions on this topic, they seem to be valuable for specific electroactive species, the type of CNTs and/or electrode architecture, the electrode surface, etc. Accordingly, general theories and conclusions are not yet defined, so different approaches to this topic are still needed, since the main phenomenological effects responsible for the nature of the electrochemical response of the electrodes modified with CNTs need to be determined in a rational way.
A novel promising carbon paste electrode with excellent potentiometric properties was prepared for the analysis of trihexyphenidyl hydrochloride (THP), the acetylcholine receptor and an anticholinergic drug in real samples. It contains 10.2% trihexyphenidy-tetraphenylborate ionic pair as the electroactive material, with the addition of 3.9% reduced graphene oxide and 0.3% of anionic additive into the paste, which consists of 45.0% dibutylphthalate as the solvent mediator and 40.6% graphite. Under the optimized experimental conditions, the electrode showed a Nernstian slope of 58.9 ± 0.2 mV/decade with a regression coefficient of 0.9992. It exhibited high selectivity and reproducibility as well as a fast and linear dynamic response range from 4.0 × 10−7 to 1.0 × 10−2 M. The electrode remained usable for up to 19 days. Analytical applications showed excellent recoveries ranging from 96.8 to 101.7%, LOD was 2.5 × 10−7 M. The electrode was successfully used for THP analysis of pharmaceutical and biological samples.
The emergence of antimicrobial resistance due to antibiotics in the environment presents significant public health, economic, and societal risks. This study addresses the need for effective strategies to reduce antibiotic residues, focusing on ciprofloxacin degradation. Magnetic iron oxide nanoparticles (IO NPs), approximately 13 nm in size, were synthesized and functionalized with branched polyethyleneimine (bPEI) to obtain a positive charge. These IO-bPEI NPs were combined with negatively charged titanium dioxide NPs (TiO2@CA) to form magnetically photocatalytic IO-TiO2 nanocomposites. Characterization techniques, including X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), infrared spectroscopy (IR), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), electrokinetic measurements, and a vibrating sample magnetometer (VSM), confirmed the successful formation and properties of the nanocomposites. The nanocomposites exhibited a high specific surface area, reduced mobility of photogenerated charge carriers, and enhanced photocatalytic properties. Testing the photocatalytic potential of IO-TiO2 with ciprofloxacin in water under UV-B light achieved up to 70% degradation in 150 min, with a degradation rate of 0.0063 min−1. The nanocomposite was magnetically removed after photocatalysis and successfully regenerated for reuse. These findings highlight the potential of IO-TiO2 nanocomposites for reducing ciprofloxacin levels in wastewater, helping curb antibiotic resistance.
A simple, sensitive, cost effective, and reliable enzymatic glucose biosensor was developed and tested. Nitrogen-doped heat-treated graphene oxide nanoribbons (N-htGONR) were used for modification of commercially available screen-printed carbon electrodes (SPCEs), together with MnO2 and glucose oxidase. The resulting sensors were optimized and used to detect glucose in a wide linear range (0.05–5.0 mM) by a simple amperometric method, where the limit of detection was determined to be 0.008 mM. (lifetime), and reproducibility studies were also carried out and yielded favorable results. The sensor was then tested against potential interfering species present in food and beverage samples before its application to real matrix. Spiked beer samples were analyzed (with glucose recovery between 93.5 and 103.5%) to demonstrate the suitability of the developed sensor towards real food and beverage sample applications.
Potentiometry with membrane selective electrodes is preferable for measuring the various constituents of pharmaceuticals. In this work, carbon paste electrodes (CPE) were prepared, modified, and tested for the determination of maprotiline hydrochloride, which acts as an antidepressant. The proposed CPE was based on an ionic association complex of maprotiline-tetraphenylborate, 2-nitrophenyloctyl as a binder, and sodium tetraphenylborate as an ionic lipophilic additive. The optimized composition improved potentiometric properties up to theoretical Nernst response values of −59.5 ± 0.8 mV dec−1, in the concentration range of maprotiline from 1.6 × 10−7 to 1.0 × 10−2 mol L−1, and a detection limit of 1.1 × 10−7 mol L−1. The CPE provides excellent reversibility and reproducibility, exhibits a fast response time, and is applicable over a wide pH range. No significant effect was observed in several interfering species tested. The proposed electrode was used for the precise determination of maprotiline in pure solutions, urine samples, and a real sample—the drug Ludiomil.