Project description:The present study described the fabrication and electroanalytical performance of planar screen-printed disposable sensors based on copper oxide nanoparticles (CuONPs/SPEs) for the voltammetric determination of tapentadol (TAP) in its marketed pharmaceutical products and biological fluids. CuONPs exhibited electrochemical activity against the electrooxidation of TAP with an anodic peak at 0.84 V in the BR buffer at pH 5. The electroanalytical investigations and molecular orbital calculations pointed out the oxidation of the tertiary amine group within the TAP moiety with the transfer of two electrons and protons during the oxidation of the TAP molecule at the CuONPs/SPEs surface. Linear calibration graphs were constructed covering the TAP concentration ranging from 0.83 to 738 ng mL-1 with a limit of detection (LOD) value up to 0.24 ng mL-1. The disposable printed sensor based on CuONPs offered high measurement and fabrication reproducibility with a prolonged lifetime of 6 months. Improved performance toward TAP was recorded without noticeable interference from degradation products, additives, excipients, uric acid, and ascorbic acid. Moreover, tapentadol and paracetamol (PC) can be simultaneously quantified. The CuONPs/SPEs were applied for monitoring TAP residues and in vitro dissolution studies of TAP in commercial pharmaceutical formulations.
Project description:Herein, the fabrication and full characterization of a novel atomoxetine (ATX) voltammetric carbon paste electrode (CPE) fortified with iron oxide nanoparticles (FeONPs) is demonstrated. Modification of the carbon paste matrix with the metallic oxide nanostructure provides proper electrocatalytic activity against the oxidation of ATX molecules at the carbon paste surface, resulting in a noticeable improvement in the performance of the sensor. At the recommended pH value, ATX recorded an irreversible anodic peak at 1.17 V, following a diffusion-controlled reaction mechanism. Differential pulse voltammograms exhibited peak heights linearly correlated to the ATX content within a wide concentration range from 45 to 8680 ng mL-1, with the limit of detection reaching 11.55 ng mL-1. The electrooxidation mechanism of the ATX molecule was proposed to be the oxidation of the terminal amino group accompanied by the transfer of two electrons and two protons. The fabricated FeONPs/CPE sensors exhibited enhanced selectivity and sensitivity and therefore can be introduced for voltammetric assaying of atomoxetine-indifferent pharmaceutical and biological samples in the presence of its degradation products and metabolites.
Project description:The present study introduced a novel disposable screen-printed carbon electrodes (SPCEs) modified with copper oxide/zeolite nanostructures for eco-friendly selective differential pulse voltammetric quantification of tetrahydrozoline (THZ) in eyedrop samples and biological fluids. Modification of the electrode matrix with copper oxide nanoparticles/zeolite nanostructures (CuONPs/ZY) with their effective and synergistic electrocatalytic activity enhanced the electrode performance against electrooxidation of THZ at 0.960 V in BR at pH 9.0 with a diffusion-controlled reaction mechanism. The tentative oxidation mechanism based on molecular orbital calculations postulates the oxidation of THZ molecules through oxidation of a nitrogen atom five-membered ring and the participation of two electrons/protons in the electrode reaction. Linear calibration curves were illustrated within a wide THZ concentration range from 0.24 to 57.2 μg mL-1 recording a limit of detection (LOD) value of 0.0799 μg mL-1. The CuONPs/ZY/SPEs exhibited improved performance compared with the sole reported THZ sensor-based gold film-plated carbon paste electrodes, in addition to their high reproducibility of fabrication and measurement and prolonged shelf lifetime. Tetrahydrozoline was successfully assayed in the presence of excipients, degradation products, and chloramphenicol. The presented voltammetric sensor can be considered as an eco-friendly and reliable analytical approach for monitoring THZ residues in eye drop samples and biological fluids with high recovery compared with the official pharmacopeial analytical protocol. The presented sensors were assessed according to an EcoScale tool and also compared with the reported THZ sensor.
Project description:In this work, a voltammetric method based on a metal organic framework (Ca-MOF)-modified carbon paste electrode for lead determination was developed. The MOF-based electrode was packed in a new type of 3D-printed syringe-type integrated device, which was entirely fabricated by a dual extruder 3D printer. After optimization of the operational parameters, a limit of detection of 0.26 µg L-1 Pb(II) was achieved, which is lower than that of existing MOF-based lead sensors. The device was used for Pb(II) determination in fish feed and bottled water samples with high accuracy and reliability. The proposed sensor is suitable for on-site analyses and provides a low-cost integrated transducer for the ultrasensitive routine detection of lead in practical applications.
Project description:A completely new direct voltammetric method has been developed for determination of acetaminophen (APAP), known as popular analgesic drug. The present electroanalytical method is based on anodic oxidation of APAP at the glassy carbon paste electrode modified with reduced graphene oxide (RGO). Key experimental conditions were studied, resulting in a set of optimal conditions: acetate buffer (pH 5.0) as working medium electrolyte, content of RGO, parameters of squarewave voltammetry including the potential step of 5 mV, potential amplitude of 50 mV, and frequency of 40 Hz. If peak area is used for evaluation, a linear range from 1.2 × 10-6 to 2.2 × 10-4 mol L-1 characterized by determination coefficient of 0.9971, limits of quantification and detection, 9.3 × 10-7 mol L-1 and 3.1 × 10-7 mol L-1, respectively, will be obtained. Under validation, the precision was described by relative standard deviation of 2.9% for the model sample analysis. Finally, the developed voltammetric method was compared with a reference high-performance liquid chromatography method in the analysis of commercially available pharmaceutical preparation and human urine collected from five healthy volunteers.
Project description:Alloxan (AL) is a toxic glucose analogue that acts as a potent diabetogenic inducer by selectively destroying the insulin-producing ?-cells of the pancreas. Hence, a sensitive and selective cetyl trimethylammonium bromide (CTAB)-immobilized carbon paste electrode was utilized for the analysis of AL in the existence of anthrone. The CTAB-modified carbon paste electrode in contrast with the bare carbon paste electrode showed a magnificent behavior for the electrocatalytic oxidation of AL by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods. CV studies reveal a quasi-reversible diffusion-controlled process in the potential window of -0.5 to 0.4 V at an optimum pH of 6.5 in 0.2 M phosphate buffer solution. The electrode materials were characterized by CV, field emission-scanning electron microscopy, and electrochemical impedance spectroscopy. Under optimized experimental conditions, low detection limits of 1.09 and 3.64 ?M were obtained in a linear dynamic range of 5-80 ?M and from 8 to 90 ?M by DPV and CV methods, respectively. The performance of the modified electrode is impressive in terms of least charge transfer resistance (R ct), surface concentration (?), and heterogeneous electron transfer rate constant (k 0). A 50-fold excess concentration of other potential interferants such as food additives and other organic species present in the human body does not significantly alter the peak potential and peak current of AL. The analytical application of the modified sensor was appraised by determining AL in the spiked refined flour sample. The modified sensor with a swift fabrication procedure exhibited enduring stability, adequate reproducibility, and acceptable repeatability.
Project description:In this work, a novel electrochemical assay for characterizing both lipases and lipase inhibitors as well as for the determination of lipase activity is described. It is based on a carbon paste electrode, modified with cobalt(II)phthalocyanine, and multi-walled carbon nanotubes (MWCNTs). As reaction media, a sodium borate buffer was used (0.1 M, pH 9). The measurements were carried out in a batch system using differential pulse voltammetry (DPV) and 1,3-dilinolein as standard substrate. The activity assay showed a linearity for porcine pancreas lipase activity in a range between 20 and 300 U L-1 (per min) with a limit of detection (LOD) of 7 U L-1 and a limit of quantification (LOQ) of 20 U L-1. The kinetic behavior of the lipase reaction was investigated, resulting in a KM value of 0.29 mM. The applicability of the activity assay could be shown by investigating the activity of lipases from Aspergillus oryzae and Candida rugosa, and the results were confirmed by a reference method. The inhibitory effects were characterized with Orlistat.
Project description:Glutamate is an important neurotransmitter due to its critical role in physiological and pathological processes. While enzymatic electrochemical sensors can selectively detect glutamate, enzymes cause instability of the sensors, thus necessitating the development of enzyme-free glutamate sensors. In this paper, we developed an ultrahigh sensitive nonenzymatic electrochemical glutamate sensor by synthesizing copper oxide (CuO) nanostructures and physically mixing them with multiwall carbon nanotubes (MWCNTs) onto a screen-printed carbon electrode. We comprehensively investigated the sensing mechanism of glutamate; the optimized sensor showed irreversible oxidation of glutamate involving one electron and one proton, and a linear response from 20 μM to 200 μM at pH 7. The limit of detection and sensitivity of the sensor were about 17.5 μM and 8500 μA·mM-1·cm-2, respectively. The enhanced sensing performance is attributed to the synergetic electrochemical activities of CuO nanostructures and MWCNTs. The sensor detected glutamate in whole blood and urine and had minimal interference with common interferents, suggesting its potential for healthcare applications.
Project description:The present work describes a novel, simple, and fast electroanalytical methodology for naproxen (NAP) determination in pharmaceutical formulations and biological fluids in the presence of its degradation products. Carbon paste electrodes (CPEs) modified with different carbon nanomaterials, namely, glassy carbon powder (GCE), multiwall carbon nanotubes (MWCNTs), single-walled carbon nanotubes (SWCNTs), graphene nanosheets (Gr), and graphene oxides (GO) were tested. Comprehensive studies were performed on the electrode matrix composition including the nature of the pasting liquids, pH, carbon nanomaterials, and mode of electrode modification. Two anodic oxidation peaks were recorded at 0.890 and 1.18 V in 1 × 10-1 mol·L-1 phosphate buffer solution at pH 6. Oxidation of naproxen (NAP) is an irreversible diffusion-controlled process. Calibration plots were rectilinear in the concentration ranging from 0.067 to 1.0 µg·mL-1 with correlation coefficient 0.9979. Photodegradation of NAP resulted in disappearance of the oxidation peak at 1.18 V, allowing simultaneous determination of NAP in presence of its degradation product. The achieved high sensitivity and selectivity suggest the application of the proposed protocol for naproxen determination in pharmaceutical preparations and human blood plasma.
Project description:This work describes the development and characterization of a modified carbon-fiber microelectrode sensor capable of measuring real-time physiological pH changes in biological microenvironments. The reagentless sensor was fabricated under ambient conditions from voltammetric reduction of the diazonium salt Fast Blue RR onto a carbon-fiber surface in aprotic media. Fast-scan cyclic voltammetry was used to probe redox activity of the p-quinone moiety of the surface-bound molecule as a function of pH. In vitro calibration of the sensor in solutions ranging from pH 6.5 to 8.0 resulted in a pH-dependent anodic peak potential response. Flow-injection analysis was used to characterize the modified microelectrode, revealing sensitivity to acidic and basic changes discernible to 0.005 pH units. Furthermore, the modified electrode was used to measure dynamic in vivo pH changes evoked during neurotransmitter release in the central nervous system of the microanalytical model organism Drosophila melanogaster.