A Facile Strategy for Construction of Sensor for Detection of Ondansetron and Investigation of its Redox Behavior and Thermodynamic Parameters

A sodium dodecylsulfate‐doped polypyrrole (SDS‐PPy) film was elaborated on glassy carbon electrode (GCE) by an electrodeposition method in phosphate buffer solution (pH 2.0) containing pyrrole (Py) and sodium dodecyl sulfate (SDS). SDS‐PPy/GCE was used for the construction of sensor, which showed excellent electrochemical response for the detection of ondansetron (OND) compared to conventional PPy. The application of the square wave (SW), with the adsorptive accumulation, indicates a maximum response at 1.33 V in H₂SO₄ (0.5 M). The influence of experimental parameters on determination of OND is discussed. The adsorptive stripping technique showed to be more sensitive, giving responses twice as big as those of non‐accumulated OND. The substantial improvement of response permits the development of an electroanalytical technique with a linear concentration in the range (1.0–80 μM), low detection (0.09 μM), and quantification limits (0.3 μM), and acceptable relative standard deviations of repeatability (0.59 %), and reproducibility (1.51 %). Consequently, this electrode is promising candidate for an accurate electroanalytical determination of OND in pharmaceutical samples with high sensitivity and selectivity, good accuracy and precision. The electrooxidation of OND at SDS‐PPy/GCE at various temperatures were studied by cyclic voltammetry to evaluate both the kinetic (k_s and E_a) and thermodynamic (ΔG*, ΔH* and ΔS*) parameters.     

Synthesis,X-ray crystal structure and DFT studies of cobalt(II) and vanadium(V) complexes with N,N,O-tridentate aroyl-hydrazone based ligand

A new aroyl-hydrazone, 2-pyridine carboxaldehyde-derived hydrazone ligand and its cobalt(II) (1) and vanadium(V) (2) complexes were prepared. The structures of these compounds were investigated using elemental analysis, spectral (IR, UV), and X-ray diffraction measurements. The electrochemical properties of the complexes were studied by cyclic voltammetry. The hydrazone ligand acted as tridentate and coordinated to vanadium and cobalt via N-imine, N-pyridine, and O-benzohydrazide atoms. The Co(II) complex crystallizes in the monoclinic system, space group P2₁/c, and has a binuclear structure. Chloride ions behave as the linking bridge and a tridentate hydrazine ligand HL and water as the terminal capping ligands. The central Co(II) ion has distorted octahedral geometry. The vanadium(V) complex crystallizes in the monoclinic crystal system, space group P2₁/n, and can be described as having highly distorted trigonal-bipyramidal coordination. The geometries and electronic properties of the complexes were also obtained using DFT and TD-DFT calculations.     

Simultaneous determination of amlodipine besylate and rosuvastatin calcium in binary mixtures by voltammetric and chromatographic techniques

Voltammetric and liquid chromatographic (LC) methods have been developed for the simultaneous determination of amlodipine besylate (AML) and rosuvastatin calcium (ROS) for the first time. Detailed electrochemical behavior and simultaneous voltammetric determination of AML and ROS were investigated in detail using glassy carbon electrode (GCE). High-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC) were also developed for the comparison. Voltammetric method exhibited linear dynamic responses for the simultaneous assay of AML and ROS in the concentration range between 0.006 and 2.85 μg/mL and between 0.01 and 5.00 μg/mL, with detection limits of 0.001 and 0.003 μg/mL, respectively. On the other hand, LC methods presented a wider linearity range than that of the SWV method between 0.5 and 100 μg/mL with the detection limits of 0.011 and 0.027 μg/mL for AML and 0.034 and 0.042 μg/mL for ROS by UPLC and HPLC techniques, respectively.     

Investigating the Influence of Column Depth on the Treatment of Textile Wastewater Using Natural Zeolite

Textile industry production processes generate one of the most highly polluted wastewaters in the world. Unfortunately, the field is also challenged by the availability of relatively cheap and highly effective technologies for wastewater purification. The application of natural zeolite as a depth filter offers an alternative and potential approach for textile wastewater treatment. The performance of a depth filter treatment system can be deeply affected by the column depth and the characteristics of the wastewater to be treated. Regrettably, the information on the potential of these filter materials for the purification of textile wastewater is still scarce. Therefore, this study investigated the potential applicability of natural zeolite in terms of column depth for the treatment of textile wastewater. From the analysis results, it was observed that the filtration efficiencies were relatively low (6.1 to 13.7%) for some parameters such as total dissolved solids, electrical conductivity, chemical oxygen demand, and sodium chloride when the wastewater samples were subjected to the 0.5 m column depth. Relatively high efficiency of 82 and 93.8% was observed from color and total suspended solids, respectively, when the wastewater samples were subjected to the 0.5 m column depth. Generally, the 0.75 m column depth achieved removal efficiencies ranging from 52.3% to 97.5%, whereas the 1 m column depth achieved removal efficiencies ranging from 86.9% to 99.4%. The highest removal efficiency was achieved with a combination of total suspended solids and 1 m column depth (99.4%). In summary, the treatment approach was observed to be highly effective for the removal of total suspended solids, with a 93.8% removal efficiency when the wastewater was subjected to the 0.5 m column depth, 97.5% for 0.75 m column depth, and 99.4% for 1 m column depth. Moreover, up to 218.233 mg of color per g of the filter material was captured. The results derived in this study provide useful information towards the potential applicability of natural zeolite in the textile wastewater treatment field.     

Determination of the Anticancer Drug Sorafenib in Serum by Adsorptive Stripping Differential Pulse Voltammetry Using a Chitosan/Multiwall Carbon Nanotube Modified Glassy Carbon Electrode

Adsorptive stripping differential pulse voltammetry (AdSDPV) was applied to the assay of sorafenib in human serum sample. Cyclic voltammetry at a carbon based screen printed electrode (SPE) permitted to detect the irreversible oxidation of SOR with formation of a new compound reversibly oxidized at a lower potential. Quantitative assays were realized using a chitosan/carboxylic acid functionalized multiwalled carbon nanotube modified glassy carbon electrode in 0.1 M phosphate buffer pH 7.0 in the presence of 50 % methanol. The AdSDPV method provided two linear responses within the concentration ranges 1×10^?8–8×10^?8 M and 1×10^?7–8×10^?7 M in serum with LOQ and LOD of 3.2×10^?9 and 9.6×10^?10 of lower linear range, respectively. The recovery of sorafenib in spiked serum was 97.5 %.     

Ionic‐liquid‐assisted desorption of DNA from polyamidoamine‐grafted silica nanoparticles surface by a low‐salt solution

We studied the influences of imidazolium‐based ionic liquids as additives in low ionic strength phosphate solution on releasing DNA from polyamidoamine dendrimer‐grafted silica nanoparticle surfaces. The effects of the side‐chain length of the imidazolium group, the anion and the concentration of the ionic liquid, the generation of the dendrimer, and the pH and the concentration of the release solution were investigated. It was found that addition of 4 mM 1‐hexyl‐3‐methylimidazolium bromide to 5 mM phosphate at pH 11 could markedly promote the desorption of DNA fragments, with a desorption efficiency of 99.0%. Compared with the conventional strategies employing high‐salt solutions or elevated temperature for acceptable recoveries, the method described here enabled quick release of DNA fragments that permitted direct, accurate analysis, and further treatment without desalting.     

Simultaneous Estimation of Ceftazidime and Ceftizoxime in Pharmaceutical Formulations by HPLC Method

The aim of the present study was to develop a fast, sensitive and reliable method for rapid screening of cephalosporin injectable dosage forms namely ceftazidime and ceftizoxime to the detection of counterfeit and substandard drugs that might be illegally commercialized. Ceftazidime, ceftizoxime and cefixime (IS) were separated in a X-Terra RP-18 column (250 × 4.60 mm ID × 5 ??) and DAD detector set at 290 and 260 nm. The mobile phase consisted of a mixture of methanol:water 20:80 (v/v) at a flow rate of 1.0 mL min^?1. Additionally, in order to find the optimum pH value of separation the pK _a values of studied compounds were determined by using two different methodologies. Aqueous pK _a values of studied compounds have been determined by UV-spectrophotometry and liquid chromatography were used for the determination and direct characterization of the dissociation constants by using the dependence of the capacity factor on the pH of the mobile phase in 20% (v/v) methanol?Cwater binary mixture in which separation was performed. The pH of the mobile phase was adjusted with 25 mM H₃PO₄ to 3.2. The method was shown to be linear, sensible, accurate, and reproducible over the range of analysis and it can be used to pharmaceutical formulations containing a single active ingredient within a short analysis time.     

Development of a Surfactant/Platinum Composite for Sensitive Cardio‐selective Beta Blocker Detection and their Theoretical Studies

An electrooxidative behavior of beta‐blocker drug esmolol was thoroughly investigated by using glassy carbon electrode modified with sodium dodecyl sulfate‐based platinum nanoparticles. The designed nanosensor exhibited remarkable electro‐catalytic effect by dramatically boosting the signal of the esmolol as compared to the bare electrode with detection limit up to picomolar. The effects of pH, scan rate, temperature, deposition potential, deposition time, effect of electrolyte and interfering agents were investigated to optimize conditions for getting intense signal of the analyte. Under optimized experimental conditions, a linear calibration plot for esmolol with a detection limit of 60 pM was obtained. The analyte sensing ability of the modified electrode was supported by the application of theoretical studies that showed favorable interaction between sodium dodecyl sulfate/platinum nanoparticles composite and esmolol. In this study, our aim was to developed a nanosensor for the sensitive detection of esmolol by electrochemical assay. We tried a lot of different modification style and modifiers for creating a sensitive nanosensor for esmolol. This nanosensor can be applied to the esmolol in serum sample without using any further separation, evaporation or precipitation steps. Application could apply in serum sample to test accuracy of our sensor and method. The high recovery results were observed in serum study.     

Electrochemical Determination and in silico Studies of Fludarabine on NH2 Functionalized Multiwalled Carbon Nanotube Modified Glassy Carbon Electrode

A sensitive voltammetric technique has been developed for the determination of Fludarabine using amine‐functionalized multi walled carbon nanotubes modified glassy carbon electrode (NH₂‐MWCNTs/GCE). Molecular dynamics simulations, an in silico technique, were employed to examine the properties including chemical differences of Fludarabine‐ functionalized MWCNT complexes. The redox behavior of Fludarabine was examined by cyclic, differential pulse and square wave voltammetry in a wide pH range. Cyclic voltammetric investigations emphasized that Fludarabine is irreversibly oxidized at the NH₂‐MWCNTs/GCE. The electrochemical behavior of Fludarabine was also studied by cyclic voltammetry to evaluate both the kinetic (k_s and E_a) and thermodynamic (ΔH, ΔG and ΔS) parameters on NH₂‐MWCNTs/GCE at several temperatures. The mixed diffusion‐adsorption controlled electrochemical oxidation of Fludarabine revealed by studies at different scan rates. The experimental parameters, such as pulse amplitude, frequency, deposition potential optimized for square‐wave voltammetry. Under optimum conditions in phosphate buffer (pH 2.0), a linear calibration curve was obtained in the range of 2×10^?7 M–4×10^?6 M solution using adsorptive stripping square wave voltammetry. The limit of detection and limit of quantification were calculated 2.9×10^?8 M and 9.68×10^?8 M, respectively. The developed method was applied to the simple and rapid determination of Fludarabine from pharmaceutical formulations.     

Effect of Catalytically Active Zinc Oxide−Carbon Nanotube Composite on Sensitive Assay of Desloratadine Metabolite

Desloratadine is one of the most effective second‐generation antihistamines and the electrochemical behavior of the active agent of desloratadine was investigated with a new nanosensor designed with the addition of zinc oxide and multiwalled carbon nanotube (ZnO : MWCNT) mixture on glassy carbon (GCE). By investigating and using cyclic, differential pulse and square wave voltammetry techniques with ZnO : MWCNT/GCE, it is planned to obtain information about quantification and mechanism of desloratadine. The efficiency of experimental parameters such as pH, scan rate, accumulation potential and time on the anodic response of desloratadine were studied. Differential pulse voltammetry was selected as assay method and under developed method and optimized conditions, the current showed linear dependence with concentration in the range between 2×10^?8 and 8×10^?6 M in pH 5.5 acetate buffer. The achieved limits of detection (LOD) and quantification (LOQ) are 0.769 nM and 2.56 nM respectively. Applicability of the methods was demonstrated by their implementation in pharmaceutical dosage forms of desloratadine and the accuracy, precision, selectivity, sensitivity, intra‐day and day‐to‐day reproducibility of the methods were clearly explored. Finally, this sensor was successfully applied on real sample as a selective, simple, reproducible, repeatable an electrochemical sensor.