Facile Synthesis of Graphene/Cobalt Oxide Nanohexagons for the Selective Detection of Dopamine

This work presents a simple green approach for the chemical synthesis of cobalt oxide nano hexagons (Co₃O₄ NHs) with an average size of 160±40 nm incorporated graphene nanosheets (GR). The techniques used to confirm the formation of GR−Co₃O₄ NHs are transmission electron microscopy (TEM), energy‐dispersive X‐ray spectroscopy (EDX), and X‐ray diffraction spectroscopy (XRD). The dopamine (DA) sensor was fabricated by drop casting GR−Co₃O₄ NHs on the pre‐cleaned glassy carbon electrode (GCE). GR−Co₃O₄ modified GCE displayed a sensitive and selective electrochemical determination of DA compared to only GR and Co₃O₄ NHs modified GCE. Our fabricated sensor showed a wide linear range from 0.2 to 3443 μM with low limit of detection (84 nM) towards the determination of DA. The sensitivity of our fabricated sensor was calculated to be 108 μA mM⁻¹ cm⁻². As well, a significant storage stability, repeatability and reproducibility were attained by GR−Co₃O₄ NHs modified GCE. Human urine samples were targeted for the demonstration of practicality of our sensor.     

A Hafnium Oxide Based Voltammetric Platform for the Sensitive Determination of Octopamine

An electrochemical sensor was constructed by modification of a glassy carbon electrode (GCE) with nanoparticles of hafnium oxide (HfO₂) and multi-walled carbon nanotubes (MWCNTs) for the sensitive determination of octopamine. The platform (HfO₂NPs/MWCNTs/GCE) presented an improved anodic peak for octopamine at 0.65 V. The combination of HfO₂ and MWCNTs resulted in outstanding catalytic activity and enhanced the magnitude of the peak response. Results suggest that a three-electron oxidation occurs for the process of octopamine. Voltammetry of octopamine exhibited a dynamic linear response in the concentration range of 1.6×10⁻⁶∼4.8×10⁻⁵ M with a detection limit of 5.4×10⁻⁷ M for octopamine.     

Novel Sn Doped Co3O4 Thin Film for Nonenzymatic Glucose Bio‐Sensor and Fuel Cell

A facile chemical solution deposition via two‐step spin coating technique was used to fabricate nano‐particulate novel Sn doped Co₃O₄ thin film for glucose sensor and fuel cell applications. Substitution of Sn into Co₃O₄ host lattice lead to a remarkable increase in the electrocatalytic activity of the Co₃O₄ electrode material. Film thickness played a significant role in enhancing the charge transferability of the electrode as was observed from electrochemical impedance spectroscopy (EIS). The best sensor exhibited two wide linear response ranges (2 μM up to ∼0.5 mM and 0.6 mM up to ∼5.5 mM respectively) with sensitivities of 921 and 265 μA cm⁻² mM⁻¹ respectively and low limit of detection of 100 nM (S/N=3). The sensor was very selective towards glucose in the presence of various interference and showed long term stability. Moreover, the developed thin film modified electrode could generate one electron current in nonenzymatic fuel cell setup at room temperature.     

Development of reproducible thiourea sensor with binary SnO2/V2O5 nanomaterials by electrochemical method

In this methodology, the thiourea (TU) sensor was made-up by means of glassy carbon electrode (GCE) layered by the wet-chemically prepared binary SnO₂/V₂O₅ nanomaterials (NMs). The existence of SnO₂ and V₂O₅ in prepared spherical NPs were categorized by X-ray photoelectron spectroscopy (XPS), Field Emission Scanning Electron Microscopy (FESEM), Energy-dispersive X-ray spectroscopy and X-ray Powder Diffraction (XRD). The TU sensor was displayed the linear responses in concentration range (LDR) of 0.1 nM ~ 0.01 mM. The calibration curve of TU sensor was made by plotting current verses concentration of TU, which was measured by electrochemical technique. The sensitivity and lower limit of detection (DL) for TU sensor were calculated from calibration curve, which are found as 17.0918 µAµM^-1cm⁻² and 95.40 ± 4.77 pM respectively. The analytical parameters of TU sensor such as reproducibility, response time and stability were measured and found efficient results. It also was validated in the detection of TU in presence of real bio-samples. Thus, this unique and prospective method is introduced to develop the selective biosensor by electrochemical approach, which might be a pioneer sensor probe for its simple and reliable approach for the safety of healthcare and biomedical fields in a large scales.     

A Novel Electrochemical Sensor Based on Copper‐based Metal‐Organic Framework for the Determination of Dopamine

A glassy carbon electrode (GCE) modified with a copper‐based metal‐organic framework (MOF) [HKUST‐1, HKUST‐1 = Cu₃(BTC)₂ (BTC = 1,3,5‐benzenetricarboxylicacid)] was developed as a highly sensitive and simple electrochemical sensor for the determination of dopamine (DA). The MOF was prepared by a hydrothermal process, and the morphology and crystal phase of the MOF were characterized by scanning electron microscopy (SEM) and X‐ray diffraction (XRD), respectively. Meanwhile, the electrochemical performance was investigated using cyclic voltammetry (CV), differential pulse voltammetry (DPV), and electrochemical impedance spectroscopy (EIS). Under optimized conditions, the modified electrode showed excellent electrocatalytic activity and high selectivity toward DA. The linear response range was from 5.0 × 10⁻⁷ to 1.0 × 10⁻⁴ M and the detection limit was as low as 1.5 × 10⁻⁷ M. Moreover, the electrochemical sensor was used to detect DA in real samples with excellent results. MOF‐based sensors hold great promise for routine sensing applications in the field of electrochemical sensing.     

Ferrite Nanocomposite Based Electrochemical Sensor: Characterization,Voltammetric and Amperometric Studies for Electrocatalytic Detection of Formaldehyde in Aqueous Media

Development of nanocomposite based electrochemical sensors for detection of toxic chemicals describes an environmentally benign strategy for monitoring the health of ecosystem. Herein, we reported in situ preparation of graphitic carbon nitride (g-C₃N₄) decorated Ag₂S/NiFe₂O₄ nanocomposite sensor by facile precipitation method. The electrochemical studies demonstrated efficient electrocatalytic activity of ternary nanocomposite pasted glassy carbon electrode (g-C₃N₄@Ag₂S/NiFe₂O₄/GCE) for selective detection of formaldehyde. Moreover, fabricated sensor exhibit rapid amperometric response with excellent selectivity, remarkable sensitivity (1681 μA mmol L⁻¹ cm⁻²) and lower detection limit (LOD: 1.63 μmol L⁻¹). It is noteworthy to mention that sensor exhibits good operational and long-term storage stability.     

MWCNTs/Ionic Liquid/Graphene Quantum Dots Nanocomposite Coated with Nickel‐Cobalt Bimetallic Catalyst as a Highly Selective Non‐enzymatic Sensor for Determination of Glucose

In this work, a glassy carbon electrode (GCE) was modified with multiwall carbon nanotubes/ionic liquid/graphene quantum dots (MWCNTs/IL/GQDs) nanocomposite. Then, the nanocomposite was decorated with nickel‐cobalt nanoparticles (Ni?Co NPs), and it was used as a non‐enzymatic glucose sensor. Field emission scanning electron microscopy, X‐ray diffraction spectroscopy, and energy dispersive spectroscopy were employed to prove the electrodeposition of the Ni?Co NPs on the surface of MWCNTs/IL/GQDs/GCE. Also, cyclic voltammetric and amperometric methods were utilized for the investigation of the electrochemical behaviour of the Ni?Co NPs/MWCNTs/IL/GQDs/GCE for glucose oxidation. The novel amperometric sensor displayed two linear ranges from 1.0 to 190.0 μmol L^?1 and 190.0 to 4910 μmol L^?1 with a low detection limit of 0.3 μmol L^?1 as well as fast response time (2 s) and high stability. Also, the sensor showed good selectivity for glucose determination in the presence of ascorbic acid, citric acid, dopamine, uric acid, fructose, and sucrose, as potential interference species. Finally, the performance of the proposed sensor was investigated for the glucose determination in real samples. Ni?Co NPs/MWCNTs/IL/GQDs/GCE showed good sensitivity and excellent selectivity.     

Non‐enzymatic Fructose Sensor Based on Co3O4 Thin Film

In this study, we report on the selective of fructose on Co₃O₄ thin film electrode surface. A facile chemical solution deposition technique was used to fabricate Co₃O₄ thin film on fluorine doped tin oxide, FTO, glass. Electrode characterization was done using XRD, HRTEM, SEM, AFM, and EIS. The constructed sensor exhibited two distinctive linear ranges (0.021–1.74 mM; 1.74–∼15 mM) covering a wide linear range of up to ∼15 mM at an applied potential of +0.6 V vs Ag/AgCl in 0.1 M NaOH solution. The sensor demonstrated high, reproducible and repeatable (R.S.D of <5 %) sensitivity of 495 (lower concentration range) & 53 (higher concentration range) μA cm⁻² mM⁻¹. The sensor produced a low detection limit of ∼1.7 μM (S/N =3). The electrode was characterised by a fast response time of <6 s and long term stability. The repeatability and stability of the electrode resulted from the chemical stability of Co₃O₄ thin film. The sensor was highly selective towards fructose compared to the presence of other key interferences i. e. AA, AC, UA. The ease of the electrode fabrication coupled with good electrochemical activity makes Co₃O₄ thin film, a promising candidate for non‐enzymatic fructose detection.     

Analytical sensing of hydrogen peroxide on Ag nanoparticles–multiwalled carbon nanotube-modified glassy carbon electrode

A sensor based on silver nanoparticles (NPs)/multiwalled carbon nanotube (CNT)-modified glassy carbon electrode (GCE) was prepared and employed for accurate and rapid determination of hydrogen peroxide (H₂O₂). In summary, by using a mechanochemical method, multiwalled CNTs dispersed in ethanol and used for modification of GCE. After that, by using a double-pulse technique, silver NPs are electrodeposited on surface of multiwalled CNTs/ GCE. Parameters that are affected by electrocatalytic reduction of H₂O₂ on the modified electrode, such as multiwalled CNT concentration and double-pulse parameters, were optimized using Minitab software. The optimal modified electrode was characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and cyclic voltammetry. The proposed H₂O₂ sensor exhibited excellent characteristics for the sensing of H₂O₂, such as wide linear range from 0.1 to 10 mM, a low detection limit of 2 μM, high repeatability, and no interference by a number of substances.     

A Self‐assembled L‐Cysteine and Electrodeposited Gold Nanoparticles‐reduced Graphene Oxide Modified Electrode for Adsorptive Stripping Determination of Copper

Glassy carbon electrode (GCE) modified with L‐cysteine and gold nanoparticles‐reduced graphene oxide (AuNPs‐RGO) composite was fabricated as a novel electrochemical sensor for the determination of Cu²⁺. The AuNPs‐RGO composite was formed on GCE surface by electrodeposition. The L‐cysteine was decorated on AuNPs by self‐assembly. Physicochemical and electrochemical properties of L‐cysteine/AuNPs‐RGO/GCE were characterized by scanning electron microscopy, atomic force microscopy, energy dispersive spectroscopy, Raman spectroscopy, X‐ray diffraction, cyclic voltammetry and adsorptive stripping voltammetry. The results validated that the prepared electrode had many attractive features, such as large electroactive area, good electrical conductivity and high sensitivity. Experimental conditions, including electrodeposition cycle, self‐assembly time, electrolyte pH and preconcentration time were studied and optimized. Stripping signals obtained from L‐cysteine/AuNPs‐RGO/GCE exhibited good linear relationship with Cu²⁺ concentrations in the range from 2 to 60 μg L⁻¹, with a detection limit of 0.037 μg L⁻¹. Finally, the prepared electrode was applied for the determination of Cu²⁺ in soil samples, and the results were in agreement with those obtained by inductively coupled plasma mass spectrometry.     

A Novel Cerium Tungstate Nanosheets Modified Electrode for the Effective Electrochemical Detection of Carcinogenic Nitrite Ions

In this present scenario, for the first time, we propose a facile and simple wet chemical approach for the fabrication of two‐dimensional (2D) cerium tungstate (CeW₂O₉;CeW) nanosheets and evaluated as an electrochemical sensor for the detection of nitrite ions. The successful formation of CeW₂O₉ nanosheets was confirmed by various physicochemical techniques such as X‐ray diffraction, Fourier transform infrared spectroscopy, Raman, Scanning electron microscope, Transmission electron microscope and Energy dispersive X‐ray studies. The electrochemical properties of the CeW nanosheets were studied by using cyclic voltammograms (CV) and chronoamperometric techniques. As an electrochemical sensor, the CeW nanosheets modified glassy carbon electrode (GCE) showed superior electrocatalytic activity in the oxidation of nitrite in terms of higher anodic peak current and lower oxidation potential when compared with unmodified GCE. CeW nanosheets based electrochemical sensor has been fabricated which detect nitrite in wide linear response range, good sensitivity and very low detection limit of 0.02–986 μM, 2.85 μA μM⁻¹ cm⁻² and 8 nM, respectively. Moreover, the CeW nanosheets modified GCE exhibited excellent selectivity even in the presence of common metal ions and biologically co‐interfering compounds. For the practical viability of the prepared amperometric sensor has been utilized in various water samples such as tap, lake and drinking water and the obtained recoveries are appreciable.     

Molecularly Imprinted Poly-o-phenylenediamine Electrochemical Sensor for Entacapone

We have developed a molecularly imprinted polymer (MIP) electrochemical sensor for entacapone (ETC) based on an electropolymerised polyphenylenediamine (Po-PD) on a glassy carbon electrode (GCE) surface. The direct electropolymerisation of the o-phenylenediamine monomer (o-PD) was carried out with ETC as a template. The steps of electropolymerization process, template removal and binding of the analyte were tested by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) using [Fe(CN)₆]³⁻/[Fe(CN)₆]^{4 −} as a redox probe. The operation of the sensor has been investigated by differential pulse voltammetry (DPV). Under optimal experimental conditions, the response of the DPV was linearly proportional to the ETC concentration between 1.0×10⁻⁷ and 5.0×10⁻⁶ M ETC with a limit of detection (LOD) of 5.0×10⁻⁸ M. The developed sensor had excellent selectivity without detectable cross-reactivity for levodopa and carbidopa. The MIP sensor was successfully used to detect ETC in spiked human serum samples.     

Gold Nanoparticles-electrochemically Reduced Graphene Oxide/Poly(indole-5-carboxylic acid) Nanocomposite for Electrochemical Non-enzymatic Sensing of Hydrogen Peroxide

Herein, co-electrodeposition of AuNPs and ERGO onto GCE was conducted to prepare the modified electrode, GCE/AuNPs-ERGO. The poly(indole-5-carboxylic acid) (P(In-5-COOH) was then coated onto the GCE/AuNPs-ERGO with the help of electropolymerization. FT-IR, FE-SEM and EDX, and XRD techniques were employed to characterize the prepared nanocomposite. The nanocomposite modified electrode (GCE/AuNPs-ERGO/P(In-5-COOH)) was examined for the electrochemical reduction of H₂O₂ using chronoamperometry. A high reduction current for H₂O₂ was observed due to the synergistic effect between AuNPs-ERGO and P(In-5-COOH). The proposed sensor demonstrated a wide linear range of 0.025–750 μmol L⁻¹, with a LOD of 0.008 μmol L⁻¹ at −0.4 V. Furthermore, the developed sensor was applied for the detection of H₂O₂ in fetal bovine serum and urine samples.     

Synthesis and Characterization of Co3O4/Multiwalled Carbon Nanotubes Nanocomposite for Amperometric Sensing of Hydrazine

Co₃O₄ nanoparticles (NPs) were synthesized and decorated on the multi‐walled carbon nanotubes (MWCNTs) through a simple hydrothermal procedure. The deposited Co₃O₄ NPs on the sidewalls of MWCNTs were found to be cubic crystal structure and homogenously dispersed with a narrow particle size distribution centered at around 6 nm. The Co₃O₄/MWCNTs nanocomposite was then utilized for the electrochemical detection of hydrazine, and exhibited a high sensitivity of 34.5 µA mM^?1, a low detection limit of 0.8 µM (S/N=3), a wide linear range of 20 µM to 1.1 mM along with a short response time of less than 5 s.     

A glassy carbon electrode modified with a film composed of cobalt oxide nanoparticles and graphene for electrochemical sensing of H2O2

We have prepared a graphene-based hybrid nanomaterial by electrochemical deposition of cobalt oxide nanoparticles (CoO_xNPs) on the surface of electrochemically reduced graphene oxide deposited on a glassy carbon electrode (GCE). Scanning electron microscopy and cyclic voltammetry were used to characterize the immobilized nanoparticles. Electrochemical determination of H₂O₂ is demonstrated with the modified GCE at pH 7. Compared to GCEs modified with CoO_xNPs or graphene sheets only, the new electrode displays larger oxidative current response to H₂O₂, probably due to the synergistic effects between the graphene sheets and the CoO_xNPs. The sensor responds to H₂O₂ with a sensitivity of 148.6 μA mM^?1 cm^?2 and a linear response range from 5 μM to 1 mM. The detection limit is 0.2 μM at a signal to noise ratio (SNR) of three. The method was successfully applied to the determination of H₂O₂ in hydrogen peroxide samples.

Binderless Solution Processed Zn Doped Co3O4 Film on FTO for Rapid and Selective Non‐enzymatic Glucose Detection

A simple solution based deposition process has been used to fabricate Zn doped Co₃O₄ electrode as an electrocatalyst for non‐enzymatic oxidation of glucose. XRD, HRTEM, SEM, EELS, AFM, EIS was used to characterise the electrode. The addition of Zn as dopant on Co₃O₄ resulted in enhanced electrochemical performance of Zn:Co₃O₄ material compared to pristine Co₃O₄ due to increased charge transferability. The as prepared electrode showed fast response (<7 s) time, good sensitivity (193 μA mM⁻¹ cm⁻²) in the linear range of 5 μM–0.62 mM, good selectivity towards glucose at a relatively lower applied potential of +0.52 V in 0.1 M NaOH solution. A detection limit of ∼2 μM was measured for the Zn:Co₃O₄ electrode. The applied fabrication method resulted in good inter and intra electrode reproducibility as was shown by the lower relative standard deviation values (R.S.D). The electrode retained 70 % of initial current response after 30 days. Although the as prepared Zn:Co₃O₄ electrodes did not result in highest reported sensitivity, and lowest limit of detection; the ease of fabrication and scalability of production, good inter and intra electrode reproducibility makes it a potential candidate for commercial application as glucose sensor.     

Phosphomolybdic acid functionalized graphene loading copper nanoparticles modified electrodes for non-enzymatic electrochemical sensing of glucose

A sensitive non-enzymatic glucose electrochemical biosensor (Cu/PMo₁₂-GR/GCE) was developed based on the combination of copper nanoparticles (CuNPs) and phosphomolybdic acid functionalized graphene (PMo₁₂-GR). PMo₁₂-GR films were modified on the surface of glassy carbon electrode (GCE) through electrostatic self-assembly with the aid of poly diallyl dimethyl ammonium chloride (PDDA). Then CuNPs were successfully decorated onto the PMo₁₂-GR modified GCE through electrodeposition. The morphology of Cu/PMo₁₂-GR/GCE was characterized by scanning electron microscope (SEM). Cyclic voltammetry (CV) and chronoamperometry were used to investigate the electrochemical performances of the biosensor. The results indicated that the modified electrode displayed a synergistic effect of PMo₁₂-GR sheets and CuNPs towards the electro-oxidation of glucose in the alkaline solution. At the optimal detection potential of 0.50 V, the response towards glucose presented a linear response ranging from 0.10 μM to 1.0 mM with a detection limit of 3.0 × 10⁻² μM (S/N = 3). In addition, Cu/PMo₁₂-GR/GCE possessed a high selectivity, good reproducibility, excellent stability and acceptable recovery, which indicating the potential application in clinical field.     

Fe2O3-decorated boron/nitrogen-co-doped carbon nanosheets as an electrochemical sensing platform for ultrasensitive determination of paraquat in natural water

Boron/nitrogen-co-doped carbon (BCN) nanosheets decorated with Fe₂O₃ nanocrystals (Fe₂O₃–BCN) were cast on a glassy carbon electrode (GCE) and applied as an electrochemical sensor to effectively detect paraquat (PQ), a toxic herbicide, in aqueous environments. A linear experiment performed using square wave voltammetry (SWV) under optimized experimental conditions produced a decent linear relationship and a low detection limit (LOD) of 2.74 nmol/L (S/N = 3). Repeatability, reproducibility, stability, and interference experiments confirmed that the Fe₂O₃–BCN/GCE system exhibited decent electrochemical sensing performance for PQ molecules. Notably, the designed sensor showed high selectivity and a decent linear relationship with PQ concentration in natural water samples. To the best of our knowledge, this is the first study on the preparation of Fe₂O₃–BCN nanosheets for PQ detection. The proposed sensor can be employed as an effective alternative tool for distinguishing and processing PQ.     

Electrochemical Determination of Fenitrothion Organophosphorus Pesticide Using Polyzincon Modified‐glassy Carbon Electrode

In this paper, a glassy carbon electrode (GCE) was modified with polyzincon. The modified electrode was used as a simple, inexpensive and highly sensitive electrochemical sensor for the determination of organophosphorus pesticide fenitrothion. To fabricate the electrochemical sensor, GCE was immersed in 0.10 mmol L⁻¹ zincon solutions at pH 7.0 and then successively scanned between −1.00 to 2.20 V (vs . Ag/AgCl) at a scan rate of 70 mV s⁻¹ for six cycles. The morphology and structure of the polyzincon were studied with atomic force microscopy and scanning electron microscopy. A comparison of the electrochemical behavior of fenitrothion on the unmodified and polyzincon modified‐GCE showed that in the modified electrode not only the oxidation peak current increased, but also the overpotential shifted to lower one. The experimental conditions such as sample solution pH, accumulation potential, and time were optimized. The differential pulse voltammetric responses of fenitrothion at potential about −0.60 V was used for the determination of fenitrothion. The peak current increased with increasing the concentration of fenitrothion in the range of 5 to 8600 nmol L⁻¹ with a detection limit of 1.5 nmol L⁻¹. Finally, the electrochemical sensor was used for the analysis of fenitrothion in water and fruit samples.     

Ferrocene Decorated N-doped Carbon Modified Electrode with Enhanced Electrocatalytic Activity towards Non-enzymatic Glucose Detection

The nitrogen doped carbon (NDCN) have been synthesized by flame synthetic method to prepare ferrocene decorated NDCN. The hydrolysis product (FC-SH) of ferrocene benzyne derivative (FC-SAc) was immobilized onto NDCN modified GCE and used for glucose detection with high sensitivity. Cyclic voltammetric analysis reveal that FC-S-NDCN/GCE exhibit excellent activity for glucose oxidation when compared to FC/GCE. The FC-S-NDCN/GCE with wide linear responses range from 0.001 to 0.01 mM with the regression co-efficient of 0.998. The FC-S-NDCN/GCE show low detection limit (LOD) of 0.08 μM and exhibit sensitivity of 1580 μA mM⁻¹ cm⁻². The FC-S-NDCN glucose sensor exhibit wide linear range, high sensitivity and lower detection limit on determination of glucose.