AgNP-decorated SBA-15 for MWCNT Paste Modified Electrode: A Sensor for Simultaneous Voltammetric Determination of Paracetamol and Sulfamethoxazole

A new electrochemical sensor based on a carbon nanotube paste electrode modified with a Santa Barbara Amorphous material (SBA-15) decorated with silver nanoparticles, namely CNT/SBA/Ag-PE, was developed. It was successfully applied for individual and simultaneous determination of both paracetamol (PC) and sulfamethoxazole (SMZ) medicines. The electrode exhibited a linear dynamic range of 0.12–110 μmol L⁻¹ for paracetamol and 0.06–70 μmol L⁻¹ for sulfamethoxazole, and detection limits of 38 and 19 nmol L⁻¹, respectively. The proposed sensor offered high sensitivity, fast response time and the potential for detecting both drugs simultaneously. The CNT/SBA/Ag-PE enabled the simultaneous determination of PC and SMZ in urine samples with high recovery rates.     

Fabrication and characterization of boron doped diamond microelectrode arrays of varied geometry

Boron doped diamond (BDD) is a well-known electrode material that exhibits an excellent electrochemical potential window with very low background current. With this, microelectrodes and microelectrode arrays (MEAs) have been found to even further lower background currents without compromising sensitivity. As such, BDD MEAs are excellent electrode materials for a variety of electroanalytical applications, capable of multi-mode detection. We fabricated BDD MEAs adapting traditional semiconductor microfabrication processes; the resulting MEAs were patterned in different geometries to find an optimum electrochemical response, depending on the application. This is demonstrated using 4 different MEA geometries of different size and spacing using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS), where the charge transfer resistance (R_ct) increases as the electrodes are farther spaced from one another. Excellent sigmoidal voltammogram shape in CV was obtained for each BDD MEA geometry. BDD MEAs spaced farther from one another were found to give better resolution from the background in fast scan cyclic voltammetric measurements of dopamine due to the decrease in the double layer capacitance (C_dl) as verified with EIS. This work furthers the understanding of BDD MEAs and their pertinence to sensitive electroanalytical techniques.     

Electrochemically Deposited Porous Graphene−Polypyrrole−Polyphenol Oxidase for Dopamine Biosensor

We report a method for the fabrication of glassy carbon electrode modified porous graphene-polypyrrole-polyphenol oxidase (GCE−PG−PPy−PPO) modified electrode for the determination dopamine. The optimization of pH, concentration and detection limit of dopamine was employed by amperomatric technique. The detection limit of dopamine was found to be in a linear range of 2×10⁻⁸ to 4.6×10⁻⁵ M and lower limit detection is 4×10⁻⁹ M. Michealis – Menten constant (Km) and the activation energy were calculated as 31.32 μM and 37.4−Kj mol⁻¹, respectively. The developed biosensor was used to quantify the dopamine in human urine sample.     

An Arrayed Micro‐glutamate Sensor Probe Integrated with On‐probe Ag/AgCl Reference and Counter Electrodes

Complete all‐in‐one multi‐arrayed glutamate (Glut) sensors have been constructed on a silicon‐based micromachined probe composed of micro‐platinum (Pt) working electrodes, a micro‐silver/silver chloride (Ag/AgCl) reference electrode (RE), and a micro‐Pt counter electrode (CE). The OCP shift of the electrodeposited Ag/AgCl on‐probe micro‐reference electrode compared with a Ag/AgCl wire is <0.1 mV/h. The composition ratio of Ag, Cl, and Pt on the electrodeposited on‐probe micro‐reference electrode is observed to be 1.00 : 0.48 : 0.02 analyzed by EDS. The miniaturized amperometric Glut biosensors were constructed on working electrode sites (electrode area: ∼8.5×10⁻⁵ cm²) of the microprobe modified with glutamate oxidase (GlutOx) enzyme layers for the selective, fast, and continuous detection of L‐glutamate. The sensor selectivity towards common electroactive interferents has been improved significantly by coating the electrode surface with perm‐selective polymer layers, overoxidized polypyrrole (PPY) and Nafion®. The sensitivity, detection range, and response time of the proposed all‐in‐one Glut biosensors are 204.7±5.8 nA μM⁻¹ cm⁻² (N=5), 4.99–109 μM, and 2.7±0.3 sec, respectively and no interferent signals of AA and DA were observed. The sensor can be reused over 19 times of continuous repetitive operation (total measurement time: ∼4 hours) and the sensor sensitivity can retain up to four weeks of storage.     

A Novel Label-free Chronoamperometric Immunosensor Based on a Biocomposite Material for Rapid Detection of Carcinoembryonic Antigen

In this research, poly(diallyldimethylammonium chloride)-capped gold nanoparticles, nickel ferrite particles, and carbon nanotubes were combined to form a PANC metal composite. The prepared metal composite modified onto a glassy carbon electrode was electropolymerized with poly(o-phenylenediamine) and immobilized with horseradish peroxidase, anti-carcinoembryonic antigen antibody, and bovine serum albumin to create the label-free immunosensors for rapid detection of carcinoembryonic antigen (CEA) using chronoamperometry. This developed biocomposite material modified onto a glassy carbon electrode presented an excellent electrocatalytic response to the redox reaction of hydrogen peroxide as a sensing probe, from which the kinetic parameters including of a charge transfer rate constant, a diffusion coefficient value, an electroactive surface area, and a surface concentration were calculated to be 1.85 s⁻¹, 4.28×10⁻⁶ cm² s⁻¹, 0.14 cm² and 1.87×10⁻⁸ mol cm⁻², respectively. The developed immunosensors also exhibited a wide linear range of CEA concentration from 0.01 to 25 ng mL⁻¹ with high sensitivity (96.21 μA cm⁻² ng⁻¹ mL) and low detection limit (0.72 pg mL⁻¹), excellent selectivity without interfering effects from possible species (amoxicillin, ascorbic acid, aspirin, caffeine, cholesterol, dopamine, glucose, and uric acid), outstanding stability (n=100, %I>50 %), repeatability (%RSD=0.34, n=10), reproducibility (%RSD=4.06, n=10), and rapid analysis (25 s each operation time). This proposed method was successfully applied for CEA detection in whole blood samples with satisfactory results, suggesting that this developed sensing platform may be considered to be exploited for fabrication of other label-free electrochemical immunosensors for the real sample analysis.     

Gold-dendrimer Nanocomposite Based Electrochemical Sensor for Dopamine

An electrochemical sensor for dopamine was developed by electrodepositing poly(propylene imine) (PPI) dendrimer and gold nanoparticles (AuNPs) onto a glassy carbon electrode (GCE). Electrochemical characterisation of the sensor was carried out by cyclic voltammetry and electrochemical impedance spectroscopy in ferri/ferrocyanide electrolyte. The nanocomposite electrode (GCE-PPI-AuNPs) showed improved electroactive surface area and electrochemical response over bare GCE. The sensor recorded a detection limit of 0.16 μM over a concentration range of 0.1 μM to 125 μM. The sensor was applied for dopamine detection in human serum samples and in the presence of interfering substances such as ascorbic acid and epinephrine.     

Choline Oxidase Based Composite ZrO2@AuNPs with Cu2O@MnO2 Platform for Signal Enhancing the Choline Biosensors

A novel metal composite material based on zirconium dioxide decorated gold nanoparticles (ZrO₂@AuNPs), copper (I) oxide at manganese (IV) oxide (Cu₂O@MnO₂) and immobilized choline oxidase (ChOx) onto a glassy carbon electrode (GCE) (ChOx/Cu₂O@MnO₂-ZrO₂@AuNPs/GCE) has been developed for enhancing the electro-catalytic property, sensitivity and stability of the amperometric choline biosensor. The ChOx/Cu₂O@MnO₂-ZrO₂@AuNPs/GCE displayed an excellent electrocatalytic response to the oxidation of the byproduct H₂O₂ from the choline catalyzed reaction, which exhibited a charge transfer rate constant (K_s) of 0.97 s⁻¹, a diffusion coefficient value (D) of 4.50×10⁻⁶ cm² s⁻¹, an electroactive surface area (A_e) of 0.97 cm² and a surface concentration (γ) of 0.54×10⁻⁸ mol cm⁻². The modified electrode also provided a wide linear range of choline concentration from 0.5 to 1,000.0 μM with good sensitivity (97.4 μA cm⁻² mM⁻¹) and low detection limit (0.3 μM). The apparent Michaelis-Menten constant was found to be 0.08 mM with I_max of 0.67 μA. This choline biosensor presented high repeatability (%RSD=2.9, n=5), excellent reproducibility (%RSD=2.9, n=5), long time of use (n=28 with %I>50.0 %) and good selectivity without interfering effects from possible electroactive species such as ascorbic acid, aspirin, amoxicillin, caffeine, dopamine, glucose, sucrose and uric acid. This optimal method was successfully applied for choline measurement in prepared human blood samples which demonstrated accurate and excellent reliability in the recovery range from 96.7 to 102.0 %.     

Enhanced Electrocatalytic Activity of Ni‐CNT Nanocomposites for Simultaneous Determination of Epinephrine and Dopamine

A promising electrochemical sensor based nickel‐carbon nanotube (Ni‐CNT) modified on glassy carbon (GC) electrode had been developed and the properties of the modified electrode were characterized by multispectroscopic analysis. The fabricated sensor (GC/Ni‐CNT) electrode was utilized to determine the catecholamines such as epinephrine and dopamine simultaneously. Differential pulse voltammetry and amperometry were used to verify the electrochemical behavior of the studied compounds. The GC/Ni‐CNT based amperometric sensor showed a wide linear range and low detection limit with high analytical sensitivity of 8.31 and 6.61 μA μM^?1 for EP and DA, respectively which demonstrates better characteristics compared to other electrodes reported in the literature. Further, no significant change in amperometric current response was observed in presence of biological interference species such as glucose, cysteine, citric acid, uric acid and ascorbic acid in the detection of EP and DA. The utility of this GC/Ni‐CNT electrode was well established for the determination of EP and DA in human urine samples.     

Disposable Sandwich‐type Electrochemical Sensor for Selective Detection of Glucose Based on Boronate Affinity

A disposable sandwich‐type electrochemical sensor for selective detection of glucose was established. The primary receptor, 3‐aminophenylboronic acid was grafted covalently onto the surface of screen‐printed carbon electrodes through an in situ‐generated diazo‐reaction. Glucose was first captured by boronic acid group on the electrode, followed by captureing an electroactive ferroceneboronic acid (FcBA) as the secondary receptor to form bidentate glucose‐boronic complex. Electrochemical impedance spectroscopy was applied to characterize the construction of sandwich‐type disposable sensor. In the sandwich assay, current response of captured FcBA on the electrode was dependent on the concentration of glucose. The sandwich assay showed higher selectivity for glucose than that for fructose, mannose, galactose and other electroactive interferences including uric acid, ascorbic acid and dopamine, and exhibited a dynamic concentration range of glucose from 0.5 to 20.0 mmol L⁻¹. The disposable sensor demonstrated a good reproducibility with 2.2 % relative standard deviation (RSD). In addition, the disposable glucose sensor was used in detection of the trace glucose in the clinical urine samples.     

Development of Bio-inspired Composite Materials for the Detection of Traces of Silver Present in Water: Use of Taguchi Methodology to Design Low-cost Carbon Paste Electrodes

Carbon Paste Electrodes (CPE) modified with Grapefruit-Peels (GP) functionalized with Urea (GPU) and, Melamine (GPM) were designed for the detection of Ag⁺ in water. Taguchi L₉ methodology was used to determine the optimal graphite-Active material ratio. The best electrochemical response was for CPE-GPU with an 80 : 20 ratio. The results obtained showed a linear detection range between 0.5 to 28 μg L⁻¹, with a detection limit of 0.73 μg L⁻¹ and a limit of quantification of 1.04 μg L⁻¹. Attributable to CPE-GPU characteristics: electroactive surface area 0.175 cm², roughness factor 3.87, resistance 0.09 Ω and, mostly −NH₂ groups on its surface. The composite material offers a viable option to be used for the determination of silver traces in situ in industrial processes.     

Graphene Quantum Dots‐based Electrochemical Biosensor for Catecholamine Neurotransmitters Detection

An useful electrochemical sensing approach was developed for epinephrine (EP) detection based on graphene quantum dots (GQDs) and laccase modified glassy carbon electrodes (GC). The miniature GC biosensor was designed and constructed via the immobilization of laccase in an electroactive layer of the electrode coated with carbon nanoparticles. This sensing arrangement utilized the catalytic oxidation of EP to epinephrine quinone. The detection process was based on the oxidation of catecholamine in the presence of the enzyme – laccase. With the optimized conditions, the analytical performance demonstrated a high degree of sensitivity −2.9 μA mM⁻¹ cm⁻², selectivity in a broad linear range (1–120×10⁻⁶ M) with detection limit of 83 nM. Moreover, the method was successfully applied for EP determination in labeled pharmacological samples.     

A Sonogel/L-Cystein and a SAM L-Cystein Modified Electrodes for Detection of Dopamine

Summary: The Sonogel-Carbon electrode is a special class of sol-gel electrode that exhibits favourable mechanics and electric properties that can be used as electrochemical sensors. In this study, a Sonogel-Carbon modified with L-Cysteine was used to prepare a novel electrochemical sensor. The objective of this new electrode modification was to seek new electrochemical performances for thedetection of dopamine (DA). The influence of natural interferents such as Ascorbic Acid (AA) and Uric Acid (UA) was explored. The concentration of theses strong interferent was increased to a certain level in order to determine to what extends AA and UA may disturb the neurotransmitters electroanalysis. Our work showed that the modified electrode offers interesting analytical performances such as: (a) Fast and linear responses towards the neurotransmitter dopamine: The differential pulse voltammetry current peak was linear with the DA concentration in the range 2 · 10⁻⁷ M to 10⁻⁵ M with a detection limit of 4 · 10⁻⁸ M (S/N = 3). (b) Simultaneous detection and well-resolved signals between the DA, AA and UA: The new sensor could sensitively and separately determine DA in the presence of 1000 and 900 times higher concentrations of AA and UA respectively. Optimization of parameters such as the amount of L-cysteine in the Sonogel-Carbon mixture, interference effect, perm-selectivity and mechanical stability of the sensor are discussed. A comparison with a SAM L-Cysteine/gold electrode was also made. On the other hand the new Sonogel modified electrode has been applied to the determination of dopamine in urine samples with satisfactory results. With good selectivity and sensitivity, the proposed sensor is a simple tool for the selective detection of DA, AA and UA in biological samples.     

Electrochemical Detection of Para‐nitrophenol using Copper Metal Nanoparticles Modified Gold Electrode

para‐Nitrophenol (p‐NP) is a high priority environmental pollutant. For the sake of safety, sensitive detection of its presence in water resources and food is highly important. The present article describes the use of copper metal nanoparticles for selective and sensitive electrochemical detection of p‐NP in pure and real sample. For this the gold electrode was fabricated by polyvenylpyrrolidone stabilized copper metal nanoparticles (ca . 4 nm d.) via self‐assembled 4,4′‐bipyridine monolayer and characterized by microscopic and electrochemical techniques. The newly developed sensor permits for sensitive detection of p‐NP in a linear concentration range of 1–500 μM with lowest detection limit of 0.34 nM and high sensitivities 247.1 μA cm⁻² μM⁻¹. The sensor electrode exhibited high stability, reproducibility, good selectivity in the presence of potential interfering agents and had an excellent capability for the selective determination of p‐NP in river water without preliminary treatments.     

Electroanalytical Detection of n‐Butylamine at a Nickel/Carbon Nanotube Composite

We report the electroanalytical detection of n‐butylamine at a nickel/carbon nanotube (Ni/CNT) composite. Scanning Electron Microscopy (SEM) characterisation of the composite demonstrated that it consisted of bulk nickel particles ca. 2 μm in diameter entangled in CNT bundles. The spontaneous formation of Ni(OH)₂ was optimised, and comparison with a 3 mm nickel electrode showed that ca. 4 μg of the Ni/CNT composite cast on a 3 mm GC electrode possessed bulk nickel characteristics while also having higher activity and higher sensitivity towards the electrochemical detection of n‐butylamine. However, the Ni/CNT composite showed no response to ammonia, in contrast to the macro‐nickel‐electrode.     

Portable smartphone-based microfluidic electrochemical immunosensor for ultrasensitive detection of alpha-fetoprotein in human serum

Rapid and accurate tracing of biomarkers is essential for early detecting and diagnosing of cancer. Therefore, a valid and convenient strategy needs to be developed for efficient monitoring of cancer biomarkers. Herein, we constructed a portable microfluidic electrochemical immunosensor based on three-dimensional reduced graphene oxide (3D rGO) doped with gold nanoparticles (Au NPs) for ultrasensitive determination of alpha-fetoprotein (AFP). The designed microfluidic chip, with the advantages of small injection volume, detachable structure and high integration, was fabricated by 3D printing, which only needed 9 μL of reagent to realize the high sensitivity detection. In addition, the 3D Au NPs-rGO composites with high specific surface area and electrons transfer capacity can effectively increase electroactive sites and enhance electrochemical signals. Benefiting from these features, the 3D Au NPs-rGO microfluidic electrochemical immunochip showed a wide detection range between 0.1 pg/mL–200 ng/mL and a best detection limit of 0.045 pg/mL with the high sensitivity of 175.008 μA (ng/mL)⁻¹ cm⁻². Meanwhile, the proposed immunosensor exhibited reliable AFP detection in human serum samples, which demonstrated that this portable smartphone-based microfluidic electrochemical immunosensor hold great promises in clinical detection and huge potential in personalized healthcare.     

Determination of aflatoxin B1 by biomass derived porous carbon modified electrode with molecularly imprinted polymer

Aflatoxin determination is imperative among agricultural and food products as the pollution of the toxic aflatoxin could cause severe hazards towards animals and human beings. Here, we prepared Elaeagnus gum derived porous carbon material as electrode modified material. In situ electropolymerization of molecularly imprinted polymer utilizing phenol as monomer and aflatoxin B₁ as target template was further processed onto the porous carbon surface to achieve aflatoxin B₁ sensing ability. This sensitive MIP sensor has a detection range from 5 pM to 100 pM of aflatoxin B₁, an electrochemical sensitivity of 82.4 μA log(pM)⁻¹ cm⁻² with a detection limit of 1.7 pM, and a recovery rate of real sample measurement is 98.21 %. Good selectivity, fair repeatability and stability was confirmed. This work demonstrates the promising application of Elaeagnus gum derived porous carbon modified electrode sensor for food and drug monitoring.     

Fabrication of Co3O4 particles-modified multi-walled carbon nanotube and poly(phenosafranine) composite electrode for selective and sensitive rutin detection

The preparation and characterisation of a new composite electrode with Co₃O₄ particles-modified multi-walled carbon nanotube (MWCNT) and poly(phenosafranine), as well as its novel application for the voltammetric detection of rutin was described. The resulting composite electrode was characterised using scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and electrochemical impedance spectroscopy (EIS). In the optimised experimental conditions, the oxidation peak current (I_pa) of rutin showed a linear increase in concentration, between 0.008–0.6 and 0.80–6.0 μmol L⁻¹, with a detection limit of 0.00379 μmol L⁻¹. Due to its good selectivity and stability, the composite electrode was successfully applied in detecting rutin in pharmaceutical formulations.     

An electrochemical sensor based on molecularly imprinted polydopamine coated on reduced graphene oxide for selective detection of ornidazole

The electrochemical sensing of ornidazole (OR) was achieved with a highly selective sensor fabricated by a combination of an electrochemically reduced graphene oxide (ERGO) and molecularly imprinted polydopamine (PDA). The sensor (OR-imp@PDA/ERGO/GCE) was synthesized by electrochemical polymerization of dopamine (DA) on ERGO modified glassy carbon electrode (GCE). The analytical response of the sensor changed linearly with OR concentration varying from 1.5 × 10⁻⁹ M to 1.0 × 10⁻⁸ M and 1.0 × 10⁻⁸ M to 2.0 × 10⁻⁷ M, and the detection limit was defined as 1.1 × 10⁻⁹ M. The proposed sensor ensured the highly sensitive detection of OR concentration because of the advantages of ERGO and molecularly imprinted PDA.     

Voltammetric Detection of Captopril in a Commercial Drug Using a Gold-Copper Metal-organic Framework Nanocomposite Modified Electrode

We report the application of an electrochemical sensor based on gold-copper metal-organic framework immobilized on the surface of a glassy carbon electrode to the detection of captopril (CAP), an angiotensin-converting enzyme inhibitor. Cyclic voltammetric studies showed that the joint action of gold nanoparticles and copper-1,3,5-benzenetricarboxylate (Cu−BTC) enhanced the electrochemical response to the Cu-captopril complex that is adsorbed onto the surface of the electrode. Release of gold nanoparticles from Au@Cu−BTC not only increased the conductivity of the electrode but also provided a more favorable environment for the deposition of reduced Cu that is catalytically renewed on the electrode surface. The anodic current of the Cu^(II)−CAP oxidation peak varied linearly within two concentration ranges, namely 0.5 to 7.0 μmol L⁻¹ and 10 to 2500 μmol L⁻¹, with a limit of detection of 0.047 μmol L⁻¹. The mean recovery for the determination of captopril in commercial tablets was 100.3 % suggesting that the method has considerable potential for future industrial applications.     

Real‐time Selective Detection of Hydrogen Peroxide Based on a Tantalum Deposited Pencil Lead Electrode for Evaluation of Enzyme Activities

In this study, we have carried out electrodeposition of tantalum (Ta) nanostructures on pencil lead electrode in non‐aqueous media at room temperature by applying a constant potential. The deposited Ta on pencil lead was examined for the catalytic effect regarding hydrogen peroxide (H₂O₂) reduction with voltammetry and amperometry. Ta/pencil lead electrode exhibited amperometric sensitivity of 0.317 μA mM⁻¹ cm⁻² and fast response time of 0.75 s, where selective detection of H₂O₂ was fulfilled without interruption from common electroactive biomaterials such as O₂, uric acid, ascorbic acid, dopamine, acetamidophenol, and glucose. For practical applications, the dynamic concentration changes of H₂O₂ during catalase and glucose oxidase‐involved reactions, either eliminating or producing H₂O₂, were successfully traced in real time with as‐prepared electrode. From the kinetics study for catalase and glucose oxidase, we evaluated Michaelis constants (K _m^app) as 7.8 mM for catalase and 37 mM for glucose oxidase, respectively.