Differential Pulse Voltammetry Research Articles

Tube-Like Copper Cobalt Oxide Anchored with Multiwalled Carbon Nanotube Nanocomposites Based on a Glassy Carbon Electrode for the Electrochemical Detection of Nilutamide

Abstract Developing a precise and effective method to detect Nilutamide (NIL) is essential due to its contamination of the environment, which poses significant risks to human health and the biosphere. In this study, we employed a simple hydrothermal technique to create a nanocomposite of CuCo2O4 (copper cobalt oxide) and multi-walled carbon nanotube (MWCNT), which was then anchored onto a glassy carbon electrode for NIL detection. Various spectroscopic techniques were employed to confirm the structure of the nanomaterial, and its electrochemical properties were examined using cyclic voltammetry, differential pulse voltammetry, and electrochemical impedance spectroscopy. The CuCo2O4/MWCNT nanocomposite-modified electrode exhibited a wide linear detection range from 0.01 to 170 µM, a high sensitivity of 1.50 μA μM−1 cm−2, a low detection limit of 0.01 μM, outstanding stability, repeatability, and practical applicability for NIL detection.

Selective and sensitive MIP-Based electrochemical Sensor for the analytical determination of Lanreotide

Lanreotide (LAN) is an analog of somatostatin used to treat acromegaly and neuroendocrine tumors. Considering drug toxicity and the lack of sensitive techniques in drug analysis, the development of sensitive analytical methods is of great importance. During this research, a molecular imprinted polymer (MIP) based film [P(HEMA-MAGA)@MIP/GCE] was prepared by photopolymerization technique for electrochemical determination of LAN for the first time. N-methacryloyl-L-glutamic acid (MAGA) and hydroxyethyl methacrylate (HEMA) were used as functional and basic monomers, respectively. The surface alterations were investigated using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) and the chemical composition of the MIP-based sensor. Theelectrochemical characterization of the modifiedelectrodes was assessed using electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). Using differential pulse voltammetry (DPV) in standard solution and spiked serum sample of LAN, the linear response range for LAN was obtained as 1.0x10 − 14 M – 1.0x10 − 13 M. The limit of detection (LOD) values were 1.76x10 − 15 M and 1.82x10 − 15 M in water and commercial human serum, respectively. The limit of quantitation(LOQ) values for these were 5.85x10 − 15 M and 6.07x10 − 15 M, respectively. The P(HEMA-MAGA)@MIP/GCE sensor also showed excellent recovery in pharmaceutical preparation and commercial human serum form with of 99.37 % and 99.27 %, respectively, with a good RSD value (0.51–0.73), confirming the accuracy and precision of the sensor. As a control, the non-imprinted polymer (NIP) was also prepared to serve in the same way but without the template. The selectivity experiments were conducted using somatostatin (SOM) and octreotide (OC) as potential competitors to demonstrate the selectivity of the proposed sensor against LAN molecules.

Design of an Insulin Tracer Protein-Based Biosensor for Insulin Determination

Aim: The regulation of blood glucose levels is controlled by insulin, which is produced by the pancreatic beta system. Inadequate synthesis of beta insulin, results in elevated glucose levels, a condition known as diabetes, which can lead to various chronic health issues. In recent times, the diagnosis of diabetes, particularly type 1, has shifted towards the direct measurement of insulin levels. To facilitate this, an immunosensor was created to enable rapid and sensitive examination of insulin levels, with the goal of improving the quality for life for diabetic patients. Material and Method: For this purpose, an insulin tracer protein based biosensor was designed for the determination of insulin at all solutions. For determination of insulin, electrobiochemical analyses were performed. Optimisation and characterisation studies were performed using differential pulse voltammetry. The performance of bioelectrochemical system was analysed by Receiver Operating Characteristic method. Results: The insulin biosensor cyclic woltammogram was obtained between -0,1 and 0,6 V potantial. At 0,45 V was found as the anodic peak side for determination the insulin. Optimisation and characterisation studies performed at 0,45 V with differential pulse voltammetry. Conclusion: The study successfully identified stable and easy-to-use insulin concentrations, indicating the potential of the newly developed immunosensor for applications in clinical biochemistry laboratories.

Hydrothermally Synthesized Cerium Phosphate with Functionalized Carbon Nanofiber Nanocomposite for Enhanced Electrochemical Detection of Hypoxanthine

This work presents the detection of hypoxanthine (HXA), a purine derivative that is similar to nucleic acids who overconsumption can cause health issues, by using hydrothermally synthesized cerium phosphate (CePO4) followed by a sonochemical approach for CePO4 decorated with a functionalized carbon nanofiber (CePO4@f-CNF) nanocomposite. The formation of the nanocomposite was confirmed with X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive spectroscopy (EDS). A CePO4@f-CNF nanocomposite is used to modify a glassy carbon electrode (GCE) to analyze the electrochemical detection of HXA. Cyclic voltammetry (CV), Electrochemical impedance spectroscopy (EIS), and Differential pulse voltammetry (DPV) were used to examine the electrochemical properties of the composite. As a result, the modified electrode exhibits a larger active surface area (A = 1.39 cm2), a low limit of detection (LOD) at 0.23 µM, a wide linear range (2.05–629 µM), and significant sensitivity. Therefore, the CePO4@f-CNF nanocomposite was used to study the real-time detection in chicken and fish samples, and it depicted significant results.

Review of Detection Limits for Various Techniques for Bacterial Detection in Food Samples

Foodborne illnesses can be infectious and dangerous, and most of them are caused by bacteria. Some common food-related bacteria species exist widely in nature and pose a serious threat to both humans and animals; they can cause poisoning, diseases, disabilities and even death. Rapid, reliable and cost-effective methods for bacterial detection are of paramount importance in food safety and environmental monitoring. Polymerase chain reaction (PCR), lateral flow immunochromatographic assay (LFIA) and electrochemical methods have been widely used in food safety and environmental monitoring. In this paper, the recent developments (2013–2023) covering PCR, LFIA and electrochemical methods for various bacterial species (Salmonella, Listeria, Campylobacter, Staphylococcus aureus (S. aureus) and Escherichia coli (E. coli)), considering different food sample types, analytical performances and the reported limit of detection (LOD), are discussed. It was found that the bacteria species and food sample type contributed significantly to the analytical performance and LOD. Detection via LFIA has a higher average LOD (24 CFU/mL) than detection via electrochemical methods (12 CFU/mL) and PCR (6 CFU/mL). Salmonella and E. coli in the Pseudomonadota domain usually have low LODs. LODs are usually lower for detection in fish and eggs. Gold and iron nanoparticles were the most studied in the reported articles for LFIA, and average LODs were 26 CFU/mL and 12 CFU/mL, respectively. The electrochemical method revealed that the average LOD was highest for cyclic voltammetry (CV) at 18 CFU/mL, followed by electrochemical impedance spectroscopy (EIS) at 12 CFU/mL and differential pulse voltammetry (DPV) at 8 CFU/mL. LOD usually decreases when the sample number increases until it remains unchanged. Exponential relations (R2 > 0.95) between LODs of Listeria in milk via LFIA and via the electrochemical method with sample numbers have been obtained. Finally, the review discusses challenges and future perspectives (including the role of nanomaterials/advanced materials) to improve analytical performance for bacterial detection.

Electrochemical Sensor Modified with Graphene Oxide Decorated with Copper Oxide Nanoparticles for Velpatasvir’s Monitoring in Spiked Human Plasma.

Abstract Velpatasvir, an antiviral agent co-formulated with sofosbuvir used to treat hepatitis C, has recently demonstrated beneficial therapeutic effects against COVID-19. Therefore, therapeutic drug monitoring of velpatasvir is essential to achieve the desired clinical outcomes. An electrochemical sensor modified with synthesized copper oxide nanoparticles on the surface of graphene oxide (CuO/GO-NPs) was fabricated for the analysis of velpatasvir for the first time. Characterization was carried out using Fourier-transform infrared spectroscopy, X-ray diffraction, and scanning electron microscopy with energy-dispersive X-ray spectroscopy. The voltammetric determinations were conducted using differential pulse and cyclic voltammetry, where the modified electrode exhibited better sensitivity than the unmodified one. The method was validated according to the International Council for Harmonisation (ICH) guidelines, exhibiting linearity within a range of 1.0 ×10-7 – 1.0 × 10-5 M, covering velpatasvir’s maximum plasma concentration (Cmax), with a quantification limit of 2.89 × 10-7 M and a detection limit of 9.03 × 10-8 M. The developed sensor was successfully applied to spiked human plasma at velpatasvir’s Cmax level. The method’s greenness was assessed using the Analytical Eco-scale and the Green analytical procedure index tools. This method holds promise as a green simple approach to implemented in future velpatasvir’s therapeutic drug monitoring studies.

Electrochemical detection of benzenediols using carbon-supported catalysts

A novel implementation of an electrochemical sensors making use of Screen-Printed Electrodes (SPE) has been discussed. SPE's modified with Carbon-supported Platinum (Pt/C) and Gold (Au/C) were used to detect the three benzenediol isomers, Catechol (CC), Hydroquinone (HQ) and Resorcinol (RS) in acidic media using traditional electrochemical analytical methods such as Cyclic Voltammetry (CV), Chronoamperometry (CA) and Differential Pulse Voltammetry (DPV). Detection of each benzenediol in isolation was possible by CV measurements, and peak oxidation potentials for each isomer were noted. Simultaneous detection of more than one, or all analytes in the same solution was also observed through DPV, once again noting the peak oxidation potentials. Quantification limits were observed using CA's across concentration values ranging from close to saturation down to 1 mM for CC and HQ, and 100 nM for RS, until the recorded current values were nearly indistinguishable to a blank 1 M HCl solution containing no analyte(s), and also evaluating the maximum possible linear range of sensing. The analytes were introduced to the sensor elements in controlled amounts and the electrochemical responses of the sensor elements were recorded and processed. Measurements were repeated across two potentiostats to ensure reproducibility. With these results, successful detection of benzenediols in acidic environment was possible using modified SPE's, proving a potential viable mechanism for quick, simple and inexpensive Volatile Toxic Organic Compounds (VTOC) detection and monitoring.

Plant-based zinc nanoflowers assisted molecularly imprinted polymer for the design of an electrochemical sensor for selective determination of abrocitinib

The first electrochemical sensor application in the literature is described for the sensitive and selective determination of the selective Janus kinase (JAK)-1 inhibitor abrocitinib (ABR). ABR is approved by the U.S. Food and Drug Administration (FDA) for the treatment of atopic dermatitis. The molecularly imprinted polymer (MIP)-based sensor was designed to incorporate zinc nanoflower (ZnNFs)-graphene oxide (GO) conjugate (ZnNFs@GO), synthesized from the root methanolic extract (RME) of the species Alkanna cappadocica Boiss. et Bal. to improve the porosity and effective surface area of the glassy carbon electrode (GCE). Furthermore, the MIP structure was prepared using ABR as a template molecule, 4-aminobenzoic acid (4-ABA) as a functional monomer, and other additional components. Scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR) were used to characterize the surface and structure of the synthesized nanomaterial and MIP-based surface. Among the electrochemical methods, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were preferred for detailed electrochemical characterization, and differential pulse voltammetry (DPV) was preferred for all other electrochemical measurements using 5.0 mM [Fe(CN)6]3–/4– solution as the redox probe. The MIP-based sensor, which was the result of a detailed optimization phase, gave a linear response in the 1.0 × 10–13 – 1.0 × 10–12 M range in standard solution and serum sample. The obtained limit of detection (LOD) and limit of quantification (LOQ) values and recovery studies demonstrated the sensitivity, accuracy, and applicability of the sensor. Selectivity, the most important feature of the MIP-based sensor, was verified by imprinting factor calculations using ibrutinib, ruxolitinib, tofacitinib, zonisamide, and acetazolamide.Graphical

Enhanced detection of heavy metal ions using Ag nanoparticles and single-walled carbon nanotubes within Cu-based metal-organic frameworks

Heavy metal ions (HMIs) are major water pollutants, and their toxicity for humans is a great concern for scientists and environmentalists. They are harmful to health even at trace levels; therefore, identifying and removing heavy metals from water is critical. Herein, we report highly selective and sensitive multi-analyte detection of HMIs in water using an electrochemical sensor probe based on Ag nanoparticles and single-walled carbon nanotubes incorporating copper benzene tri-carboxylate metal–organic frameworks (Ag/SWNTs@CuBTC-MOFs). The materials were characterized using FTIR, XPS, XRD, and FE-SEM with EDX mapping, TEM, TG-DTA, BET surface area, CV, and EIS. The Ag/SWNTs@CuBTC-MOF electrochemical sensor was tested by differential pulse voltammetry over a pH range of 3–10 for various HMIs. It shows high pH-dependent sensitivity towards Hg2+ (pH-5.0), Ni2+ (pH-7.0), and Fe3+ (pH-10.0) ions and a limit of detection of 1.39 nM, 2.6 nM, and 3.03 nM, respectively. The fabricated sensor probe exhibits high selectivity, good linearity, and a limit of detection below the maximum contamination limit, as the US Environmental Protection Agency suggested.

Fabrication of MXene/chitosan/polyurea nanocomposite decorated on a graphenized substrate for electro-enhanced solid-phase microextraction of diclofenac followed by its determination using differential pulse voltammetry.

A novel solid-phase microextraction fiber based on MXene-chitosan-polyurea (MXene/CS/EPPU) nanocomposite decorated on a graphenized pencil lead fiber (MXene/CS/EPPU/GPLF) was prepared and utilized for electro-enhanced solid-phase microextraction (EE-SPME) of diclofenac (DCF) in biological samples. After extraction and desorption of DCF, it was determined by differential pulse voltammetry (DPV). For this purpose, the working electrode was prepared by deposition of the mentioned MXene/CS/EPPU nanocomposite onto the graphenized pencil lead. The synthesized SPME fiber was characterized using scanning electron microscopy and X-ray diffraction techniques. The effect of various parameters influencing the extraction and the desorption process were investigated, including applied voltage in the extraction and desorption steps, extraction and desorption times, and pH. The developed method exhibited a rather wide linearity in the range 2-1200 ng mL-1 (R2 = 0.985) for the determination of DCF in plasma samples. The limit of detection and the limit of quantification for plasma samples were estimated to be 0.58 and 1.9 ng mL-1 based on the 3Sb/m and 10Sb/m definitions, respectively. The method's accuracy and applicability have been evaluated by the analysis of plasma samples, leading to the relative recoveries in the range 87.0% and 98.0% with the relative standard deviations lower than 3.1%.

Flower-like 3D SnS decorated on nickel metal-organic framework for electrochemical detection of dimetridazole in food samples

Dimetridazole (DMZ) is a broad-spectrum antibiotic effective against bacterial and protozoan infections in humans and poultry farms. However, excessive DMZ intake leads to harmful effects. Thus, minimizing its environmental presence is crucial for sustaining daily life. This study presents an innovative approach to construct flower-like SnS particle decorations on a nickel metal-organic framework (Ni-MOF@SnS) as an electrocatalyst for DMZ detection. The Ni-MOF@SnS/GCE sensor exhibits exceptional electrocatalytic behavior, including a significantly reduced detection limit of 1.6 nM, extensive linear ranges from 0.01 μM to 60 μM and from 60 μM to 231 μM at lower and higher DMZ concentrations, respectively. It also shows enhanced sensitivity (0.139 μA μM−1 cm−2) and remarkable selectivity for DMZ detection using differential-pulse voltammetry (DPV). Furthermore, the proposed sensor demonstrates good recovery results with actual food samples.

An electrochemical sensor based on electrochemically activated carbon cloth and poly (o-aminothiophenol) cross-linked nanogold imprinted layer for the determination of tert-butylhydroquinone

In this study, an electrochemical sensor based on MoS2 with enhanced electrochemical signals from electrochemically activated carbon cloth (EACC) electrodes and cross-linked o-aminothiophenol functionalized AuNPs (o-ATP@AuNPs) was developed for the detection of the unsaturated vegetable oil antioxidant tert-butylhydroquinone (TBHQ). In this approach, carbon cloth is activated through the implementation of electrochemical methods, thereby effectively increasing its specific surface area. The resulting EACC, serving as an electrode substrate, enables the growth of additional nanomaterials and enhances conductivity. The incorporation of MoS2 effectively augments the sensitivity of the electrochemical sensor. Subsequently, MIP/MoS2/EMCC is formed via electropolymerization, utilizing TBHQ as the template molecule and o-ATP@AuNPs as the functional monomer. The SS bond of o-ATP ensures a strong and stable connection between MoS2 and o-ATP@AuNPs, thereby facilitating the immobilization of MIP. In addition, the high conductivity possessed by o-ATP@AuNPs could effectively improve the sensitivity of the electrochemical sensor. Under the optimal conditions, MIP/MoS2/EMCC could determine TBHQ in the range of 1 × 10−3 μM to 120 μM by differential pulse voltammetry (DPV) with a detection line of 0.72 nM. The proposed MIP/MoS2/EMCC is expected to be applied in the future for the selective and sensitive detection of TBHQ in vegetable oils.

Novel palladium nanoparticles/4-aminophenol functionalized nitrogen-doped graphene quantum dots-based nanocomposite electrochemical sensor: Synthesis, characterization, capacitance, and dopamine sensing

In this study, an ultrasensitive electrochemical sensor based on palladium nanoparticles/4-aminophenol functional nitrogen-doped graphene quantum dots (PdNPs/4AP N-GQDs) composite was fabricated to detect dopamine (DA). The sensor was characterized by FTIR, UV–Vis, TEM, EDX, and XRD methods. The electrochemical analysis of the nanocomposite modified glassy carbon electrode (GCE) was conducted by cyclic voltammetry (CV). HOMO-LUMO energy levels and band gap energy was calculated from cyclic voltammograms, and the band gap energy was found to be small at 0.06 eV. The electrode reaction properties of dopamine on this developed ultrasensitive electrode were investigated by CV and differential pulse voltammetry (DPV), which showed that the electrode had electrocatalytic activity for dopamine sensing. Moreover, the developed electrode exhibited good sensitivity and improved performance, and the linear calibration curve for dopamine was calculated to have a LOD (limit of detection) of 21 pM in the range of 250 pM to 10 nM. Finally, the selectivity of the GQDs nanocomposite modified GCE towards dopamine was studied in the presence of several bioactive compounds with inhibitory effects. In addition, the specific capacitance of the nanocomposite material at 5 mV s−1 was found to be as high as 0.777F g−1. Furthermore, the dopamine selectivity of the sensor among some organic and inorganic interfering bioanalytes was investigated and the sensor was found to have excellent DA selectivity despite the bioanalytes.

Electrochemical sensor based on nickel selenide/hydroxylated multiwalled carbon nanotubes nanocomposites for sensitive detection of maltol

An effective electrochemical sensor based on electrodeposition of nickel selenide nanoparticles (Ni3Se4) on the surface of a glass carbon electrode (GCE) modified with hydroxylated multiwalled carbon nanotubes (MWCNTs-OH) has been successfully developed for determination of maltol. The chemical composition and morphology of Ni3Se4/MWCNTs-OH composites are characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) are employed to investigate the electrochemical behavior of maltol at Ni3Se4/MWCNTs-OH/GCE. Consequently, electrochemical sensor based on Ni3Se4/MWCNTs-OH/GCE for detection of maltol displays good electrocatalyst performance. The obtained oxidation peak current of maltol at Ni3Se4/MWCNTs-OH/GCE increases linearly with the increase in concentration of maltol in the range of 0.1 μM–2000 μM, and the calculated detection limit (LOD) is 17.5 nM (S/N = 3). In addition, the fabricated electrochemical sensor shows satisfactory stability, reliable reproducibility and excellent selectivity, and is successfully used to detect maltol in real samples with acceptable accuracy.

Electrochemical Nanosensor for the Simultaneous Determination of Anticancer Drugs Epirubicin and Topotecan Using UiO-66-NH2/GO Nanocomposite Modified Electrode

In this work, UiO-66-NH2/GO nanocomposite was prepared using a simple solvothermal technique, and its structure and morphology were characterized using field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray diffraction (XRD). An enhanced electrochemical sensor for the detection of epirubicin (EP) was proposed, which utilized a UiO-66-NH2/GO nanocomposite-modified screen-printed graphite electrode (UiO-66-NH2/GO/SPGE). The prepared UiO-66-NH2/GO nanocomposite improved the electrochemical performance of the SPGE towards the redox reaction of EP. Under optimized experimental conditions, this sensor demonstrates a remarkable limit of detection (LOD) of 0.003 µM and a linear dynamic range from 0.008 to 200.0 µM, providing a highly capable platform for sensing EP. Furthermore, the simultaneous electro-catalytic oxidation of EP and topotecan (TP) was investigated at the UiO-66-NH2/GO/SPGE surface utilizing differential pulse voltammetry (DPV). DPV measurements revealed the presence of two distinct oxidation peaks of EP and TP, with a peak potential separation of 200 mV. Finally, the UiO-66-NH2/GO/SPGE sensor was successfully utilized for the quantitative analysis of EP and TP in pharmaceutical injection, yielding highly satisfactory results.

CeO2 nanoparticles modified screen-printed carbon electrode: Electrochemical sensing platform for sulfite determination in water samples

In the present work, the CeO2 nanoparticles (CeO2 NPs) were prepared by hydrothermal method and the crystal structure and morphology analysis were studied by using a series of characterizations. Then, the screen-printed carbon electrode (SPCE) modified with CeO2 NPs was employed to develop a simple and novel sensor for sulfite determination in water samples. The CeO2 NPs/SPCE showed significant current response for sulfite oxidation. The use of the developed sensor with differential pulse voltammetry (DPV) method provides a wide linear range for sulfite determination (0.08–870.0 µM) with a low limit of detection (LOD) (0.023 µM). Finally, the results determination of sulfite in water samples showed good recoveries between 96.7% and 102.7% with a relative standard deviation (RSD) less than 3.6%.

Development of an efficient electrochemical sensor based on CuAl-LDH using an electrostatic repulsion approach for the selective determination of dopamine in the presence of uric acid and ascorbic acid species

This study provides a unique electrochemical sensor that exhibits both excellent sensitivity and selectivity, while also being environmentally friendly. The CuAl-LDH/GCE sensor, proposed as the recommended sensor, was synthesized using a straightforward one-step co-precipitation procedure. It was first used to measure dopamine levels using differential pulse voltammetry. At the ideal pH level of 8, dopamine has a positive charge, but ascorbic acid and uric acid have a negative charge. LDH, on the other hand, carries a negative charge and exhibits high electrostatic attraction towards dopamine, but is electrostatically repelled by negatively charged ascorbic acid and uric acid. Hence, CuAl-LDH/GCE has the potential to specifically ascertain the existence of dopamine in the presence of these particular species. The examination of the composition and morphology of CuAl-LDH was conducted using various analytical techniques, including scanner electron microscopy (FESEM), transmission electron microscope (TEM), element mapping (MAP), Fourier transform infrared (FTIR), energy-dispersive X-ray spectroscopy (EDX), Brunauer Emmett Teller (BET), X-ray photoelectron diffraction (XRD), and Raman techniques. Under ideal circumstances, the calibration graph of dopamine was generated using differential pulse voltammetry. A linear range of 4.194–1151.54 μM was achieved for dopamine, with a limit of detection of 0.33 μM. The findings of the study indicate that the sensor created for dopamine determination has exceptional stability, repeatability, and reproducibility. The sensor that was presented was effectively used for the measurement of dopamine in both pharmaceutical ampoules and human plasma samples.

Characterization of polysulfides (Sx2−) in seawater euxinic conditions by electroanalytical methods

Polysulfides (Sx2−) are important reduced sulfur species (RSS) that play a role in numerous environmental processes. A sound analytical method for the measurement of Sx2− in euxinic waters is lacking. In this work, differential pulse voltammetry (DPV) at the Hg electrode was used to measure the presence of Sx2− in a model seawater solution and an euxinic marine lake (Rogoznica Lake - RL Croatia), in which the concentration of RSS, mainly HS−, varies between 100 and 4000 μM. In the DPV, an adsorption phenomenon associated with Sx2− reduction on Hg produces a characteristic current minimum at −1.0 V (vs. Ag/AgCl), the magnitude of which is proportional to the concentration of polysulfidic sulfur.The DPV current minima were recorded in the model solution K2Sx NaCl/NaHCO3 (pH ~ 8.2) in a concentration range from 10 to 100 μM of polysulfidic sulfur. Total RSS was measured by cyclic voltammetry, and sampled DC voltammetry showed the ratio between HS− and S0 within the Sx2−. Using the same methodology, the presence of Sx2− below the chemocline enriched by photoptrophic sulfur bacteria was measured in the euxinic layer of RL at concentrations of up to 70 μM of polysulfidic sulfur. The results suggest that euxinic RL samples can be considered as polydisperse solutions of S0 or of S-rich compounds that can change their physicochemical properties and speciation during sample manipulation. These changes can be detected by electrochemistry. Atomic force microscopy proved the release of bacterial cellular S0 during the acidification and purging step in the electrochemical measurements, which contributed to the voltammetric RSS signal.

Mxene-derived Na2O7Ti3 nanoribbon as a promising electrode material for the detection of ethyl paraoxon in complex matrices

This study reports the development of MXene (Ti3C2Tx) derived sodium titanate nanoribbon-based electrochemical sensor for pesticide detection. Titanium Carbide (Ti3C2) MXene-derived sodium titanate nanoribbon (MNR) was obtained by facile hydrothermal synthesis and characterized by powder X-ray Diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray analysis(EDS) and, high-resolution transmission electron microscopy (HR-TEM). The synthesized water-dispersed MNR was stabilized with Nafion and deposited on the surface of glassy carbon electrodes (GCE), which provide a symmetrical uniform electrode surface. Further, the electrodes were electrochemically characterized with cyclic voltammetry (CV), differential pulse voltammetry (DPV), linear sweep voltammetry(LSV), and electrochemical impedance spectroscopy (EIS). The electrochemical sensing of ethyl paraoxon was carried out in 0.1 M phosphate buffer (PB) by CV, LSV, and DPV. The developed electrochemical sensor exhibited a limit of detection (LOD) of 0.22 nM, a very wide detection range from 0.69 nM to 174.03 nM, and a reliable sensitivity of 0.707 µA/nM/cm2. Moreover, the developed sensor was also employed for the detection of ethyl paraoxon in real samples (vegetable extract spiked with the pesticide). The results suggest that the developed MNR-based sensor would be a potential approach for efficient and accurate detection of ethyl paraoxon in ambient samples, with minimal interference.

Two-dimensional titanium carbide MXene embedded in exfoliated graphite nanoplatelets for voltammetric sensing of thiamethoxam in beekeeping products

To prepare a novel and highly sensitive electrochemical sensor for determination of Thiamethoxam (a neonicotinoid insecticide), a nanohybrid material was utilized based on two-dimensional titanium carbide (Ti3C2Tx), belonging to the MXenes class, and exfoliated graphite nanoplatelets. The resulting material was characterized with different techniques, such UV-Vis, XRD, SEM, TEM and XPS. The sensor displayed a remarkable improvement in current responses for the electrochemical reduction of thiamethoxam compared to the bare glassy carbon electrode. Under optimized conditions, a calibration curve was built by differential pulse voltammetry in the range of 0.048 to 30 µmol L−1 with limit of detection of 20 nmol L−1. Recovery data from 90 to 105% were obtained in beekeeping samples using the proposed sensor. Additionally, the sensor presented accurate and precise data when compared to chromatographic method data, and it was validated with statistical tests.