Britton-Robinson Research Articles

Validation and application of the square wave voltammetry method for the electrochemical determination of eszopiclone in pharmaceutical formulations and human biological fluids using glassy carbon electrode

A buffer solution of Britton-Robinson (B-R) pH 6.5 was utilized to validate and apply a square wave voltammetry (SWV) method for the electrochemical determination of Eszopiclone (ESP) in pharmaceuticals and biological samples. The cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods were employed in the initial study of the voltammetric behavior of the ESP compound. The rotating glassy carbon (GC) indicator electrode (2.0 mm2), Pt auxiliary electrode, and Ag/AgCl reference electrode were used for ESP determination. ESP was analyzed to produce a sharp reduction peak at a potential of −750 mV. The best shape and high sensitivity of SWV cathodic current for ESP, were observed using GC electrode, B-R, pH 6.5, accumulation time (tacc) of 60-second, accumulation potential (Eacc) of - 0.1 V, amplitude voltage of 150 mV, frequency of 15 Hz, scan rate of 150 mV s−1, and stirrer rate of 1000 round per minute (rpm). The electroanalytical performance of the SWV method was evaluated through study of repeatability, stability, calibration curve, recovery, and limits of detection and quantification (LOD,LOQ). Under the optimal conditions, the SWV response was linear in the range from 3 × 10−6 to 5 × 10−5 mol/L (n = 10). The SWV method achieved a LOD of 1.9 × 10-8 mol/L (7.5 ppb), and a LOQ of 6.41 × 10−8 mol L−1 (24.93 ppb). The validated SWV method was appeared the good repeatability, sensitivity and stability for the determination of ESP. It was given a very stable SWV current for 90 min, with a 0.141 % relative standard deviation (RSD%). The SWV method was applied to the determination of ESP in pharmaceutical tablets and biological samples.

Unlocking the electrochemical signature of Naringenin: Implications for screening in pharmaceutical formulations

Naringenin (NAR) is a versatile herbal flavonoid known for its broad pharmacological benefits, including antioxidant, anti-inflammatory, and anticancer properties. These properties underscore its potential and necessity for industrial applications within the pharmaceutical sector, making its detection and quantification crucial for ensuring the quality and efficacy of pharmaceutical products. Addressing the imperative for a sensitive and sustainable screening approach, this research leverages electrochemical analysis techniques including electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and differential pulse voltammetry (DPV). Complementary to experimental investigations, the electronic structure of NAR was probed using B3LYP/Def2-TZVPPD calculations alongside Fukui and dual descriptor analyses. Our findings delineate the dissociation kinetics of the hydroxyl groups within NAR, with particular emphasis on the phenolic group’s proton as the primary dissociation site, elucidating pivotal insights into the oxidation mechanism of NAR. Noteworthy is the irreversibility of the electrochemical oxidation process observed on both non-modified glassy carbon electrode (GCE) and gold electrode (GE), indicating a one-electron-one-proton mechanism. Utilizing the external calibration method and GCE, a linear range from 1.36 to 19.1 mg L-1 in Britton-Robinson (BR) supporting electrolyte was established, exhibiting a limit of detection (LOD) of 0.11 mg L-1 (R2 = 0.9945). For GE, the standard addition calibration approach revealed one linear range, from 0.27 to 0.48 mg L-1 (LOD of 0.04 mg L-1, R2 = 0.9960). Importantly, the proposed methodologies demonstrate satisfactory selectivity against potential interferences, with intra- and inter-day precision exhibiting low relative standard deviation (RSD) values. This study introduces a simple, sensitive, stable, selective, and sustainable electroanalytical method for the detection of NAR in pharmaceutical formulations, harnessing the advantages of unmodified electrodes and rigorous experimental validation.

Gold nanoparticles decorated kaolinite mineral modified screen-printed electrode: Use for simple, sensitive determination of gallic acid in food samples

The current study offers the nanomolar quantification of gallic acid (GAL) based on gold nanoparticles (AuNps) and kaolinite minerals (KNT) modified on a screen-printed electrode (SPE). The electrochemical behavior of GAL was performed using differential pulse voltammetry (DPV) in Britton Robinson (BR) buffer solution at pH 2.0 as a supporting electrolyte. Under the optimized DPV mode parameters, the oxidation peak current of GAL (at 0.72 V vs Ag/AgCl) increased linearly in the range between 0.002 μmolL−1 and 40.0 μmolL−1 with a detection limit of 0.50 nmolL−1. The effect of common interfering agents was also investigated. Finally, the applicability of the proposed method was verified by quantification analysis of GAL in black tea and pomegranate juice samples.

A voltammetric method coupled with chemometrics for determination of a ternary antiparkinson mixture in its dosage form: greenness assessment

An electroanalytical methodology was developed by direct differential pulse voltammetric (DPV) measurement of Levodopa (LD), Carbidopa (CD) and Entacapone (ENT) mixture using bare glassy carbon electrode (GCE) in Britton Robinson (BR) buffer (pH = 2.0). A multivariate calibration model was then applied to the exported preprocessed voltammetric data using partial least square (PLS) as a chemometric tool. Additionally, the model was cross-validated and the number of latent variables (LVs) were determined to produce a reliable model for simultaneous quantitation of the three drugs either in their synthetic mixtures or in their marketed pharmaceutical formulation with high accuracy and precision. Data preprocessing was used to tackle the problem of lacking bi-linearity which is commonly found in electrochemical data. The proposed chemometric model was able to provide fast and reliable technique for quantitative determination of antiparkinson drugs in their dosage forms. This was successfully achieved by utilizing sixteen mixtures as calibration set and nine mixtures as validation set. The percent recoveries for LD, CD and ENT were found to be 100.05% ± 1.28%, 100.04% ± 0.53% and 99.99% ± 1.25%, respectively. The obtained results of the proposed method were statistically compared to those of a previously reported High Performance Liquid Chromatography (HPLC) methodology. Finally, the presented analytical method strongly supports green analytical chemistry regarding the minimization of potentially dangerous chemicals and solvents, as well as reducing energy utilization and waste generation.

Challenging electroanalytical method for the determination of mirabegron in biological samples and pharmaceutical formulations

A simple, economic, sensitive, and time-saving differential pulse voltammetric (DPV) procedure using nanostructured zinc oxide modified carbon paste electrode (nano ZnO-CPE) in conjunction with an anionic surfactant sodium dodecyl sulfate (SDS) was developed for ultra- sensitive detection of mirabegron (MIR), the most prescribed pharmaceutical drug in treatment of overactive bladder (OAB). The use of nanostructured zinc oxide CPE modifier increased the electrode active surface area as well as improved the process of electron transfer, also it was found that at optimal conditions MIR electrochemical process was both irreversible and diffusion-regulated. The morphological characterization of the fabricated electrode was performed using field emission scanning electron microscopy (FESEM) and energy-dispersive X-ray spectroscopy (EDX). MIR voltammetric behavior was investigated using Nano ZnO-CPE in different content and electrode compositions. Therefore, ultra-sensitive results were attained with a linearity range of (0.55 to 100.20 ng ml−1) and a low limit of detection (LOD) of 0.51 ng ml−1 and limit of quantification (LOQ) of 1.54 ng ml−1 in a 0.04 M Britton-Robinson (BR) buffer at an adjusted pH of 6.0 with scan rate 100 mV s−1. Furthermore, the proposed approach was successful in measuring MIR with acceptable percentage recoveries (99.81–100.11 %) in pharmaceutical dosage form and varying concentration ranges in biological samples (99.74–100.35 %). The proposed method has been validated using ICH criteria and proven to be accurate and repeatable.

Voltammetric determination of genotoxic 4‐nitroindane at a mercury meniscus modified silver solid amalgam electrode

AbstractA silver solid amalgam electrode modified with mercury meniscus (m‐AgSAE) was used as a non‐toxic replacement of mercury electrodes in the voltammetric determination of genotoxic environmental pollutant 4‐nitroindane (4‐NI). The m‐AgSAE was used to characterize of the overall electrode process during the 4‐NI conversion using cyclic voltammetry (CV), and it was shown that the electrochemical reduction of 4‐NI is an irreversible process controlled by both diffusion and adsorption. Techniques of direct current voltammetry (DCV) and differential pulse voltammetry (DPV) at the m‐AgSAE were optimized for the development of a method for the sensitive determination of 4‐NI. The application of the more convenient DPV method was proven on authentic drinking and river water samples. Limits of quantification (LQs) obtained under the following optimal conditions were 0.1 μmol L−1 for DCV at the m‐AgSAE (Britton‐Robinson (BR) buffer pH 5.0–methanol (1 : 1); regeneration potentials E1,reg=−200 mV, E2,reg=−1100 mV) and 0.1 μmol L−1 for DPV at the m‐AgSAE (BR buffer pH 9.0–methanol (1 : 1); regeneration potentials E1,reg=−300 mV, E2,reg=−1300 mV). An attempt to decrease the LQ of the 4‐NI determination by differential pulse adsorptive stripping voltammetry at the m‐AgSAE was not successful. The LQs for DPV at the m‐AgSAE in authentic samples of drinking and river water were 1.0 μmol L−1 and 2.0 μmol L−1 (BR buffer pH 9.0–drinking or river water (1 : 9); regeneration potentials E1,reg=−300 mV, E2,reg=−1300 mV), respectively.

Voltammetric behavior of solifenacin succinate on gold, glassy carbon and boron-doped diamond electrodes: Stability testing and determination

The anticholinergic drug, solifenacin, is frequently used for the treatment of the urological tract for urinary incontinence, and urinary frequency. The development of reliable and effective solifenacin electrochemical sensors is of great importance for the pharmaceutical industry and clinical practice. In this work, the electrochemical behavior of solifenacin succinate (SOL) was studied using three different working electrodes: gold (Au), glassy carbon (GCE) and boron-doped diamond electrode (BDDE). The cyclic voltammetric (CV) measurements performed in 0.05 M NaHCO3 indicated that the SOL oxidation process is irreversible and diffusion-controlled at all investigated working electrodes. Afterwards, the testing of SOL electrochemical stability and the possibility of its electrochemical degradation was performed at the Au electrode by the cycling of the potential during 3 h and continuously to 6 h. It was shown that the SOL was electrochemically transformed into another electroactive species and its degradation was excluded. For electroanalytical application, the anodically pretreated BDDE (+2.0 V; 30 s) was selected. Various experimental parameters were optimized, including the pH of the aqueous Britton-Robinson (B-R) buffer as a supporting electrolyte (from pH 2.0 to 11.98) and the most intensive peak of the target analyte was at pH 11.0, so this pH value was chosen as the optimum for further measurements. Based on the correlation of the SOL peak intensity and different concentrations, the developed differential pulse voltammetric (DPV) method was characterized by a linear concentration range from 0.041 to 2.50 µM, with a correlation coefficient of 0.999, and a relative standard deviation of 0.3 %. Taking into account the sensitivity of the developed DPV method towards the electrochemical oxidation of SOL, a very low detection limit of 0.012 µM in the model system was achieved. The BDDE showed adequate selectivity for SOL in the presence of the investigated interferents. The obtained results indicate that the BDDE with an optimized DPV method could be applied for the trace-level electroanalytical determination of SOL in human urine sample with excellent recovery and reproducibility.

A new strategy for the determination of dinobuton fungicide by square wave stripping voltammetry on the multi-walled carbon nanotube electrode

Dinobuton is a fungicide with a dinitrophenol group pesticide, and its electrochemical behavior was investigated by cyclic voltammetry (CV) and square wave stripping voltammetry (SWSV) on a multi-walled carbon nanotube paste electrode (MWCNTPE). First of all, optimum parameters such as pH, step potential, frequency, puls amplitude, deposition time and, deposition potential were specified by using SWSV on the MWCNTPE. In the negative potential scans, two cathodic peaks appeared at nearly −480 mV and –760 mV due to the nitro groups on the molecule and the second sharp one appeared at −760 mV (versus Ag/AgCl) was used for analytical purposes. The linear working range was found to be within 3.74–25.8 μM on the MWCNTPE by SWSV in pH 7.0 Britton Robinson (BR) buffer solution. The limit of detection (LOD) and limit of quantification (LOQ) values were found to be 0.73 μM and 2.43 μM, respectively. The interference study was conducted in the presence of some pesticides such as triasulfuron, azinphos-methyl, bromoxynil-octanoate, dialifos, fipronil, vinclozolin, iprodione, procymidone, and some selected metal ions withal. Furthermore, the proposed method was also applied to apple juice, tap water, and grape juice, and percent recoveries (%) were detected as 105.9 ± 4.3; 98.3 ± 0.9; 103.7 ± 2.5% with relative standard deviations of 4.0, 1.0, and 2.4%, respectively. On the other hand, percent relative errors were calculated as 5.90, 1.65, and 3.74%, respectively. High recoveries and low relative standard deviations indicate that the applicability of the proposed method in both matrix and real samples is satisfying.

Wetting and swelling behaviour of N-acetylated thin chitosan coatings in aqueous media

Chitosan nanocoatings (thickness range of 120–540 nm) were produced on glass, zinc and silicon substrates with dip-coating and spin coating techniques to study their pH-dependent wetting and swelling behaviour. The coatings were N-acetylated with the methanolic solution of acetic anhydride to increase the degree of acetylation from 36 % to 100 % (according to ATR-FTIR studies). The measured contact angles of Britton–Robinson (BR) buffer solutions (pH 6.0, 7.4 and 9.0) were lower on the acetylated surfaces (ca. 50°), than that of their native counterparts (ca. 70°) and does not depend on the pH. Contrary, contact angles on the native coating deteriorated 10°-15° with increasing the pH. In addition, for native coatings, the decrease of the contact angles over time also showed a pH dependence: at pH 9.0 the contact angle decreased by 7° in 10 min, while at pH 6.0 it decreased by 13° and at a much faster rate. The constraint swelling of the coatings in BR puffer solutions was studied in situ by scanning angle reflectometry. The swelling degree of the native coatings increased significantly with decreasing pH (from 250 % to 500 %) due to the increased number of protonated amino groups, while the swelling degree of acetylated coatings was ca. 160 % regardless of the pH. The barrier properties of the coatings were studied by electrochemical tests on zinc substrates. The analysis of polarization curves showed the more permeable character of the acetylated coatings despite the non-polar character of the bulk coating matrix. It can be concluded that in the case of native coatings, 49 % of the absorbed water is in bound form, which does not assist ion transport, while in the case of acetylated coatings, this value is only 33 %.

New Au/chitosan nanocomposite modified carbon paste sensor for voltammetric detection of nicotine

A profoundly touchy voltammetric sensor for detection of nicotine (NIC) in urine and tobacco specimens has been developed in light of the boosted electrochemical response of NIC at gold and chitosan nanocomposite modified carbon paste electrode (ACMCPE). Material characterization techniques Scanning Electron Microscope and Energy Dispersive X-ray (SEM & EDX) were utilized to describe the ACMCPE surface material. The impedance spectroscopy technique (EIS), cyclic voltammetry (CV), chronoamperometry (CA), and differential pulse voltammetry (DPV) were employed to explore the electrochemical sensing of NIC at ACMCPE. The created sensor exhibits an exceptional electrochemical sensitivity to NIC in a universal Britton–Robinson (B-R) buffer solution with a pH range of 2.0 to 8.0. The sensor shows a linear response over NIC concentration ranges of 4.0–320.0 µM, with the detection limit (LOD) of 7.6 µM. The prepared sensor has been shown to be exceptionally viable in detecting NIC with amazing selectivity and reproducibility. We suggest it as a trustworthy and useful electrochemical sensor for NIC location.

Electrochemical Study of Sunset Yellow and its Determination in Soft Drink by Differential Pulse Adsorptive Stripping Voltammetry Using Ag-ErGO/GCE

The electrochemical behavior of sunset yellow on the glassy carbon electrode modified with silver and reduced graphene oxide has been investigated by cyclic and differential pulse adsorptive stripping voltammetry. The electrochemical behavior of sunset yellow was reversible and adsorptive on the working electrode. The optimal conditions were obtained as follows: Britton-Robinson (BR) buffer at pH 8.0; adsorption potential 0.4 V; adsorption time 50 s; sweep rate 50 mV/s; linearity range from 10-7 M to 10-6 M; the limits of detection and quantitation were 2.5 × 10­-8 M and 8.3 × 10­-8 M, respectively. The procedure was successfully applied to determine sunset yellow in soft drink samples.

Structure-Dependent Electrochemical Behavior of 2-Pyridone Derivatives: A Combined Experimental and Theoretical Study

In this work, the electrooxidation ability of nine pyridones was evaluated using cyclic (CV) and square-wave voltammetry (SWV) in Britton–Robinson (BR) aqueous buffer solutions on a glassy carbon electrode (GC). The dependence of electrochemical activity on pyridone structure was elucidated by means of experimentally obtained spectra and quantum chemical calculations. Firstly, it was shown that electrochemical activity is determined by the –OH group as a substituent in position 6 of the pyridone ring. By coupling the experimentally obtained UV-Vis spectra and DFT calculations, the most stable forms, both protonated and deprotonated, were defined. The calculated values are consistent with the electrochemical behavior observed, indicating that the deprotonated anionic form was the most electrochemically active. Moreover, the impact of the substituent in position 3 of the pyridone scaffold was discussed.

Caftaric acid oxidation in the presence of cell signaling regulator glutathione: Electrochemical and chromatographic analyses

New antioxidant materials in biomedical applications are an exciting research topic. However, the lack of understanding of the products/intermediates formed and the interaction between nucleophiles and these antioxidants will prevent commercial or industrial applications. To overcome this obstacle, chromatographic techniques, mass spectroscopy, and electrochemical analyses were combined to study the mechanism and products of the expected reaction between antioxidants and nucleophiles. Grape juice contains phenolic compounds such as 2-S-glutathionylcaftaric acid, which is formed as a result of oxidative action. Through UPLC and voltammetric analysis of caftaric acid (CFT) and its quinone with glutathione (GSH), the oxidation and subsequent reactions were monitored. Electrochemical techniques such as cyclic voltammetry (CV) and chronoamperometry (CA) have been used to investigate the electrochemical oxidation characteristics of the investigated CFT in a Britton-Robinson (B-R) buffer electrolyte. As a result of the analysis of ultra-high performance liquid chromatography-mass spectrometry (UHPLC-MS) results, the oxidation products were identified to suggest the optimal mechanism for the oxidation of CFTs both in the presence and absence of GSH. A reversible oxidation process is observed at pH 1.8 for CFT without glutathione (GSH) at E1/2 = 0.52 V against Ag/AgCl 3.0 M KCl) using cyclic voltammetry. During this electrochemical process, two electrons in the CFT molecule were oxidized along with two protons, forming o-quinone. In the presence of GSH, the formed quinone either reacts with glutathione to form mono- and bi-glutathione CFT conjugates or is reduced by GSH to its original state. As a result of the UPLC-MS analysis, the oxidation products of CFT were identified, and the reaction pathways were proposed.

Effect of Magnesium Chloride in Supporting Electrolyte for Enhancing Sensitive and Selective Electrochemical Sensor: An Approach for Anti-Rheumatic Sulfasalazine Detection

In this work, an electroanalytical evaluation for voltammetric sensing of the anti-rheumatic sulfasalazine (SSZ) at an unmodified screen-printed graphene electrode (SPGE) is demonstrated. By using the differential pulse (DPV) technique, the SSZ produced a well-defined peak of around −0.3 V (vs Ag AgCl−1) in Britton-Robinson (BR) buffer pH 4. Supporting electrolytes, pH, and salts all significantly impact SSZ reduction. Therefore, their impact on the working solutions was assessed. We discovered that using a mixture of Britton–Robinson (BR) buffer with pH 4 and MgCl2 as a supporting electrolyte can enhance SSZ sensitivity by approximately 1.7 times while simultaneously increasing detection selectivity. Under optimal conditions, the proposed assay demonstrated the ultrasensitive determination of SSZ with a broad linear detection range from 0.01 to 100 μM and a low detection limit of 4.7 nM (S/N = 3). To demonstrate the impact of the proposed method, the sensor has been successfully applied for the quantitative determination of SSZ in pharmaceutical, urine, and artificial serum sample. Therefore, this approach could offer simplicity, and rapidity, and serve as an alternative to the SSZ detection in practical applications.

Determination of trace cobalt (II) in spices samples by ultrasonic assisted cloud point extraction with spectrophotometry

In this study, ultrasonic assisted cloud point extraction (UA-CPE) method was developed for the determination of Cobalt (II) (Co(II)) in spices. After extraction and preconcentration, the Co(II) contents of the samples were determined by UV–VIS. After complexing with Ponceau Xylidine (PX) and EDTA in the presence of cationic surfactant, CTAB at pH 4.0 with Britton–Robinson (BR) buffer, Co(II) ion was withdrawn the surfactant-rich phase of nonionic surfactant, Triton X-114 (TX-114). The concentrated surfactant-rich phase containing the analyte was diluted with ethanol to a volume of 1.0 mL and then analyzed by UV–VIS spectrophotometer. The various analytical parameters affecting the UA-CPE yield were investigated and optimized. Analytical data achieved after optimization: limits of detection (LOD) and: limits of quantification (LOQ) are 0.76 and 2.59 μg L−1, respectively; The calibration curve is rectilinear for Co(II) with changed calibration sensitivity in the range of 1–10 and 10-210 μg L−1. The precision (as RSD%) is 4.8. This optimized method was applied in the analysis of various spice samples.

Voltammetric quantitative analysis of vildagliptin in bulk form and spiked human serum at a modified electrode

The electrochemical behavior of Vildagliptin (VILD) was studied using the cyclic voltammetric technique in an aqueous Britton–Robinson (BR) universal buffer solution of various pH levels between 4.0 and 10 at a 5% calcium-montmorillonite clay modified with carbon paste electrode surface (5% Ca-MMT/CPE). The results exhibited an irreversible anodic peak at about 1.238 V versus Ag/AgCl, KCl (3 mol L−1). The anodic peak was found to be diffusion–adsorption controlled. The possible reaction mechanism is estimated taking into consideration of the calculated electrons and protons number transferred on the electrode/electrolyte interface using the cyclic voltammetric technique. VILD was found to adsorb onto the surface of 5% Ca-MMT/CPE in a monolayer surface coverage of 3.0 × 10−12 mol cm−2. A validated square wave voltammetry (SWV) technique for VILD determination was performed. The calibration curve of VILD onto the 5% Ca-MMT/CPE surface was linear in the concentration range of 1.0–110 nmol L−1 with the mean limits of detection and quantification was 0.285 and 0.950 nmol L−1, respectively, in the bulk form. The proposed procedure for the assay of VILD in bulk form, dosage form, and spiked human serum has the advantage of being simple, rapid, sensitive, and inexpensive compared to other analytical methods. The described method showed an excellent performance for the trace determination of VILD in its formulation without interference from excipients.Graphical abstract

Development of Micro-Column Preconcentration Method Using a Restricted-Access Poly(protoporphyrin-co-vinyl pyridine) Adsorbent for Copper Determination in Water and Milk Samples by FIA-FAAS

For years, researchers have focused on the determination of metal ions at trace levels in environmental and food samples using analytical methods that employ techniques with low cost acquisition and maintenance and without microwave-assisted acid digestion procedures or aggressive reagents. Therefore, the present study deals with the synthesis and application of a novel, restricted-access poly(protoporphyrin-co-vinyl pyridine) adsorbent to preconcentrate copper in water samples and bovine milk that have only been subjected to pH adjusting (pH 6.0) and filtration using posterior on-line determination by FAAS. Regarding macromolecules, the restricted-access property of the adsorbent was achieved using the hydrophilic compound 2-hydroxyethyl methacrylate (HEMA). This method is based on the preconcentration of Cu2+ ions using a flow-injection system which is buffered with 0.05 mol L−1 of Britton–Robinson (BR) at a pH of 6.0 and has a flow rate of 14.0 mL min−1 through a mini-column packed with 50.0 mg of adsorbent. The elution was carried out using 0.40 mol L−1 of HCl toward the FAAS detector. The developed method provided a preconcentration factor of 44.7-fold, low limits of detection (LOD) (0.90 µg L−1) and quantification (LOQ) (2.90 µg L−1), tolerance to interfering ions (95.0 and 103.0%), and intra-day and inter-day precision assessed as the RSD (percentage of relative standard deviation), which ranged from 3.08 to 4.80%. The restricted-access poly(protoporphyrin-co-vinyl pyridine) adsorbent demonstrated outstanding features to exclude macromolecules, bovine serum albumin (BSA), and humic acid (HA) from an aqueous medium. Lake water and bovine milk samples were analyzed by the proposed preconcentration method with minimal sample pretreatment (which was based mainly on pH adjusting and filtration using an analytical curve with external calibration), yielding recovery values from addition and recovery tests ranging from 91.7 to 101.9%. The developed method shows great advantages over previously published methods, avoiding the time-consuming use of concentrated acids in a microwave-assisted acid digestion procedure.

Voltammetric determination of anti-malarial drug amodiaquine at a boron-doped diamond electrode surface in an anionic surfactant media

In this study, the electrochemical determination of the amodiaquine (ADQ) drug was evaluated using an electrochemically pretreated boron-doped diamond (BDD) electrode due to the enhanced surface activity. The cyclic voltammogram results of ADQ were given as single reversible and diffusion-controlled peaks at +0.48 V for the oxidation peak and +0.05 V for the reduction peak (vs. Ag/AgCl) in Britton-Robinson (BR) buffer at pH 8.0. The peak potential and current signals of ADQ were evaluated at the surface of the BDD electrode using instrumental parameters to develop a simple method for ADQ detection. Also, the effect of an anionic surfactant, sodium dodecyl sulfate (SDS), on the adsorption applicability of the BDD electrode significantly increased the stripping voltammetric determination of ADQ. Under the optimal conditions chosen and employing square-wave adsorptive stripping voltammetry at the BDD electrode, ADQ was determined at + 0.34 V (vs. Ag/AgCl) at the open-circuit condition in BR buffer at pH 8.0 in the presence of 2·10–4 mol l–1 SDS. Furthermore, analytical parameters showed the linear relationship for ADQ determination in the concentration range of 0.1–20.0 μg ml–1 (2.2·10–7 – 4.3·10–5 mol l–1), with a detection limit of 0.03 μg ml–1 (6.5·10–8 mol l–1). The proposed approach can be applied to determine ADQ in water samples.

A Novel Carbon Paste Electrode Modified with N1-Hydroxy-N1,N2-Diphenylbenzamidine for the Electrochemical Determination of Cadmium(II) in Environmental Samples.

The present study introduces a novel electrode for rapid, highly sensitive, and selective electrochemical sensor for cadmium(II) using 5% N1-hydroxy-N1,N2-diphenylbenzamidine (HDPBA) modified carbon paste electrode (CPE) (HDPBA‒CPE). Surface characterizations and structural analysis of the proposed HDPBA‒CPE were performed using several analytical techniques. The voltammetric measurements of Cd(II) were conducted by cyclic voltammetry (CV) and square wave anodic stripping voltammetry (SWASV). Several experimental conditions such as composition and pH of buffer solutions, HDPBA composition, accumulation potential and time, and other voltammetric conditions were optimized. Cd(II) was preconcentrated on the modified electrode surface for 270 s using Britton Robinson (B-R) buffer (0.1 M, pH 4) at −1.0 V versus Ag/AgCl, followed by electrochemical oxidation of the accumulated Cd(II) in the positive scan of SWASV after a quiet time of 10 s. Under optimized parameters, the proposed method showed a linear range of 0.3–100 nM Cd(II) with a detection limit of 0.032 nM. The fabricated HDPBA-modified carbon paste electrode exhibited excellent sensitivity, selectivity, stability, and reproducibility (with RSD of 3.8%). The developed HDPBA‒CPE was used for the quantification of Cd(II) in tobacco and environmental water samples, and it was found to be applicable for the determination of different types of real samples.

Electrochemical Behavior and Ultrasensitive, Simple and Effective Voltammetric Determination of Acetaminophen Using Modified Glassy Carbon Electrode Based on 4‐Hydroxyquinoline‐3‐carboxylic Acid

AbstractAn electrochemical oxidation of acetaminophen (ACOP) has been successfully performed by using glassy carbon electrode covered with 4‐hydroxyquinoline‐3‐carboxylic acid (4HQ3CA) to reinforce electrode's feature. To characterize the modified electrode (4HQ3CA/GC), electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and Fourier transform infrared spectroscopy (FT‐IR) techniques were used. The finding optimum conditions (supporting electrolyte, pH) and the electrochemical determination studies were performed with differential pulse voltammetry (DPV). It was decided that the supporting electrolyte medium suitable for ACOP determination was Britton‐Robinson (BR) buffer and the effect of pH change on the oxidation peak of ACOP in this media was investigated. The effect of changing scan rate on the oxidation peak of ACOP was examined and this study showed that the oxidation process of ACOP on the 4HQ3CA/GC modified electrode surface was diffusion and adsorption controlled process. A wide concentration range from 0.0025 μM to 141 μM with a limit of detection (LOD) of 5.98×10−10 M (3 s/m) was obtained. This prepared sensor was carried out for the determination of ACOP in pharmaceutical sample.