Search Results (10)

This paper presents the development of a cheap and rapid electrochemical sensor for ascorbic acid detection. In particular, the graphite ink working electrode of screen-printed cells was covered by a film of elecrosynthesized molecularly imprinted polypyrrole (e-MIP); differential pulse voltammetry (DPV) was the selected method for the analyte detection. The ascorbic acid molecules were successfully entrapped in the polypyrrole film, creating the recognition sites. The best results were obtained after polypyrrole overoxidation and performing the measurements in phosphate buffer solution 0.05 M/KCl 0.1 M at pH 7.5. A comparison with the bare and the not-imprinted polypyrrole-modified electrodes showed that the e-MIP-based sensor had the highest selectivity and reproducibility. The developed method was applied to assess ascorbic acid in farmaceutical products, obtaining values not significantly different from the declared content. Full article

To protect consumers from risks related to overexposure to sulfadiazine, total residues of this antibacterial agent in animal-origin foodstuffs not exceed international regulations. To this end, a new electrochemical sensor based on a molecularly imprinted polymer nanocomposite using overoxidized polypyrrole and copper nanoparticles for the detection of sulfadiazine is elaborated. After optimization of the preparation of the electrochemical sensors, their differential pulse voltammetric signal exhibits an excellent stability and reproducibility at 1.05 V, with a large linear range between 10⁻⁹ and 10⁻⁵ mol L⁻¹ and a low detection limit of 3.1 × 10⁻¹⁰ mol L⁻¹. The produced sulfadiazine sensor was successfully tested in real milk samples. The combination of the properties of the electrical conduction of copper nanoparticles with the properties of the preconcentration of the molecularly imprinted overoxidized polypyrrole allows for the highly sensitive detection of sulfadiazine, even in real milk samples. This strategy is new and leads to the lowest detection limit yet achieved, compared to those of the previously published sulfadiazine electrochemical sensors. Full article

Polypyrrole (PPy) is an interesting conducting polymer due to its good environmental stability, high conductivity, and biocompatibility. The association between PPy and metallic nanoparticles has been widely studied since it enhances electrochemical properties. In this context, gold ions are reduced to gold nanoparticles (AuNPs) directly on the polymer surface as PPy can be oxidized to an overoxidized state. This work proposes the PPy electrochemical synthesis followed by the direct reduction of gold on its surface in a fast reaction. The modified electrodes were characterized by electronic microscopic and infrared spectroscopy. The effect of reduction time on the electrochemical properties was evaluated by the electrocatalytic properties of the obtained material from the oxidation of ascorbic acid (AA) and electrochemical impedance spectroscopy studies. The presence of AuNPs improved the AA electrocatalysis by reducing oxidation potential and lowering charge transfer resistance. EIS data were fitted using a transmission line model. The results indicated an increase in the electronic transport of the polymeric film in the presence of AuNPs. However, PPy overoxidation occurs when the AuNPs’ deposition is higher than 30 s. In PPy/AuNPs 15 s, smaller and less agglomerated particles were formed with fewer PPy overoxidized, confirming the observed electrocatalytic behavior. Full article

Choline (Ch) and phosphocholine (PCh) levels in tissues are associated to tissue growth and so to carcinogenesis. Till now, only highly sophisticated and expensive techniques like those based on NMR spectroscopy or GC/LC- high resolution mass spectrometry permitted Ch and PCh analysis but very few of them were capable of a simultaneous determination of these analytes. Thus, a never reported before amperometric biosensor for PCh analysis based on choline oxidase and alkaline phosphatase co-immobilized onto a Pt electrode by co-crosslinking has been developed. Coupling the developed biosensor with a parallel sensor but specific to Ch, a crosstalk-free dual electrode biosensor was also developed, permitting the simultaneous determination of Ch and PCh in flow injection analysis. This novel sensing device performed remarkably in terms of sensitivity, linear range, and limit of detection so to exceed in most cases the more complex analytical instrumentations. Further, electrode modification by overoxidized polypyrrole permitted the development of a fouling- and interferent-free dual electrode biosensor which appeared promising for the simultaneous determination of Ch and PCh in a real sample. Full article

A novel electrochemical method to assay phospholipase D (PLD) activity is proposed based on the employment of a choline biosensor realized by immobilizing choline oxidase through co-crosslinking on an overoxidized polypyrrole film previously deposited on a platinum electrode. To perform the assay, an aliquot of a PLD standard solution is typically added to borate buffer containing phosphatidylcholine at a certain concentration and the oxidation current of hydrogen peroxide is then measured at the rotating modified electrode by applying a detection potential of +0.7 V vs. SCE. Various experimental parameters influencing the assay were studied and optimized. The employment of 0.75% (v/v) Triton X-100, 0.2 mM calcium chloride, 5 mM phosphatidylcholine, and borate buffer at pH 8.0, ionic strength (I) 0.05 M allowed to achieve considerable current responses. In order to assure a controlled mass transport and, at the same time, high sensitivity, an electrode rotation rate of 200 rpm was selected. The proposed method showed a sensitivity of 24 (nA/s)⋅(IU/mL)⁻¹, a wide linear range up to 0.33 IU/mL, fast response time and appreciable long-term stability. The limit of detection, evaluated from the linear calibration curve, was 0.005 IU/mL (S/N = 3). Finally, due to the presence of overoxidized polypyrrole film characterized by notable rejection properties towards electroactive compounds, a practical application to real sample analysis can be envisaged. Full article

Smart textiles for wearable devices require flexibility and a lightweight, so in this study, a soft polypyrrole (PPy) electrode system was integrated into a piezoelectric polyvinylidenefluoride (PVDF) energy harvester. The PVDF energy harvester integrated with a PPy electrode had the piezoelectric output voltage of 4.24–4.56 V, while the PVDF energy harvester with an additional aluminum-foil electrode exhibited 2.57 V. Alkaline treatment and chemical vapor deposition with n-dodecyltrimethoxysilane (DTMS) were employed to improve the adhesion between the PVDF and PPy and the resistance to over-oxidation in aqueous solutions. The PVDF film modified by an alkaline treatment could have the improved adhesion via the introduction of polar functional groups to its surface, which was confirmed by the ultrasonication. The surface hydrophobicity of the PPy electrode was enhanced by the DTMS coating, resulting in the improvement of the resistance to over-oxidation with a water contact angle of 111°. Even with the hydrophobic coating, the electrodes remained electroconductive and continued to transfer an electric charge, maintaining the piezoelectricity of the PVDF film. The developed electrode-integrated energy harvester is expected to be applied to smart textiles because it offers the advantages of efficient piezoelectric generation, flexibility, and durability. Full article

In this study, a miniaturized biosensor based on permselective polymer layers (overoxidized polypyrrole (Ppy) and Nafion^®) modified and enzyme (glutamate oxidase (GlutOx)) immobilized micro-platinum wire electrode for the detection of alanine aminotransferase (ALT) was fabricated. The proposed ALT biosensor was measured electrochemically by constant potential amperometry at +0.7 V vs. Ag/AgCl. The ALT biosensor provides fast response time (~5 s) and superior selectivity towards ALT against both negatively and positively charged species (e.g., ascorbic acid (AA) and dopamine (DA), respectively). The detection range of the ALT biosensor is found to be 10–900 U/L which covers the range of normal ALT levels presented in the serum and the detection limit and sensitivity are found to be 8.48 U/L and 0.059 nA/(U/L·mm²) (N = 10), respectively. We also found that one-day storage of the ALT biosensor at ?20 °C right after the sensor being fabricated can enhance the sensor sensitivity (1.74 times higher than that of the sensor stored at 4 °C). The ALT biosensor is stable after eight weeks of storage at ?20 °C. The sensor was tested in spiked ALT samples (ALT activities: 20, 200, 400, and 900 U/L) and reasonable recoveries (70%~107%) were obtained. Full article

Vesicular exocytosis is ubiquitous, but it is difficult to detect within the cells’ communication mechanism. For this purpose, a 2 µm ultramicrodic carbon fiber electrode was fabricated in this work based on electrodeposition with over-oxidized polypyrrole nanoparticle (PPyox-CFE), which was applied successfully for real-time monitoring of quantal exocytosis from individual pheochromocytoma (PC12) cells. PPyox-CFE was evaluated by dopamine (DA) solutions through cyclic voltammetry and amperometry electrochemical methods, and results revealed that PPyox-CFE improved the detection limit of DA. In particular, the sensitivity of DA was improved to 24.55 µA·µM^?1·µm^?2 using the PPyox-CFE. The ultramicrodic electrode combined with the patch-clamp system was used to detect vesicular exocytosis of DA from individual PC12 cells with 60 mM K⁺ stimulation. A total of 287 spikes released from 7 PC12 cells were statistically analyzed. The current amplitude (I_max) and the released charge (Q) of the amperometric spikes from the DA release by a stimulated PC12 cell is 45.1 ± 12.5 pA and 0.18 ± 0.04 pC, respectively. Furthermore, on average ~562,000 molecules were released in each vesicular exocytosis. PPyox-CFE, with its capability of detecting vesicular exocytosis, has potential application in neuron communication research. Full article

A novel electrochemical sensor for the detection of anthracene was prepared by modifying a glassy carbon electrode (GCE) with over-oxidized polypyrrole (PPyox) and Ag-Au (1:3) bimetallic nanoparticles (Ag-AuNPs). The composite electrode (PPyox/Ag-AuNPs/GCE) was prepared by potentiodynamic polymerization of pyrrole on GCE followed by its overoxidation in 0.1 M NaOH. Ag-Au bimetallic nanoparticles were chemically prepared by the reduction of AgNO₃ and HAuCl₄ using C₆H₅O₇Na₃ as the reducing agent as well as the capping agent and then immobilized on the surface of the PPyox/GCE. The nanoparticles were characterized by UV-visible spectroscopy technique which confirmed the homogeneous formation of the bimetallic alloy nanoparticles. Transmission electron microscopy showed that the synthesized bimetallic nanoparticles were in the range of 20–50 nm. The electrochemical behaviour of anthracene at the PPyox/Ag-AuNPs/GCE with Ag: Au atomic ratio 25:75 (1:3) exhibited a higher electrocatalytic effect compared to that observed when GCE was modified with each constituent of the composite (i.e., PPyox, Ag-AuNPs) and bare GCE. A linear relationship between anodic current and anthracene concentration was attained over the range of 3.0 × 10^?6 to 3.56 × 10^?4 M with a detection limit of 1.69 × 10^?7 M. The proposed method was simple, less time consuming and showed a high sensitivity. Full article

In this work, preparation of a molecularly imprinted polymer (MIP) film and its recognition properties for sulfamethoxazolewere investigated. The overoxidized polypyrrole (OPPy) film was prepared by the cyclic voltammetric deposition of pyrrole (Py) in the presence of supporting electrolyte (tetrabutylammonium perchlorate-TBAP) with and without a template molecule (sulfamethoxazole) on a pencil graphite electrode (PGE). The voltammetric behaviour of sulfamethoxazole on imprinted and non-imprinted (NIP) films was investigated by differential pulse voltammetry (DPV) in Britton-Robinson (BR) buffer solutions prepared in different ratio of acetonitrile-water binary mixture, between the pH 1.5 and 7.0. The effect of the acetonitrile-water ratio and pH, monomer and template concentrations, electropolymerization cycles on the performance of the MIP electrode was investigated and optimized. The MIP electrode exhibited the best reproducibility and highest sensitivity. The results showed that changing acetonitrile-water ratio and pH of BR buffer solution changes the oxidation peak current values. The highest anodic signal of sulfamethoxazole was obtained in BR buffer solution prepared in 50% (v/v) acetonitrile-water at pH 2.5. The calibration curve for sulfamethoxazole at MIP electrode has linear region for a concentration range of 25.10^-3 to 0.75 mM (R²=0.9993). The detection limit of sulfamethoxazole was found as 3.59.10^-4 mM (S/N=3). The same method was also applied to determination of sulfamethoxazole in commercial pharmaceutical samples. Method precision (RSD<1%) and recoveries (>87%) were satisfactory. The proposed method is simple and quick. The polypyrrole (PPy) electrodes have low response time, good mechanical stability and are disposable simple to construct. Full article