The introduction of low detection limit ion selective electrodes (ISEs) may well pave the way for the determination of trace targets of cationic compounds. This research focuses on the detection of titanium (III) cation using a new PVC-membrane sensor based on synthesized tris(2pyridyl) methylamine (tpm) ionophore. The application and validation of the proposed sensor was done using potentiometric titration, inductively coupled plasma atomic emission spectrometry (ICP-AES), and atomic absorption spectrometry (AAS). The membrane sensor exhibited a Nernstian response to the titanium (III) cation over a concentration range of 1.0 × 10(-6)-1.0 × 10(-2) M and pH range from 1-2.5. The Nernstian slope, the lower of detection (LOD), and the response time (t95%) of the proposed sensor were 29.17 ± 0.24 mV/dec, 7.9 × 10-7 M, and 20 s, respectively. The direct determination of 4-39 μg/ml of titanium (III) standard solution showed an average recovery of 94.60 and a mean relative standard deviation of 1.8 at 100.0 μg/ml. Finally, the utilization of the electrodes as end-point indicators for potentiometric titration with EDTA solutions for titanium (III) sensor was successfully carried out.
A disposable horseradish peroxidase (HRP)-based electrochemical genosensor was developed for chronoamperometric detection of single-stranded asymmetric lolB gene PCR amplicon (118 bp in length) of the food-borne pathogen, Vibrio cholerae. A two-step sandwich-type hybridization strategy using two specific probes was employed for specific detection of the target single-stranded DNA (ssDNA). The analytical performances of the detection platform have been evaluated using a synthetic ssDNA (ST3) which was identical to the target single-stranded amplicon and a total of 19 bacterial strains. Under optimal condition, ST3 was calibrated with a dynamic range of 0.4883-15.6250 nM. By coupling asymmetric PCR amplification, the probe-based electrochemical genosensor was highly specific to the target organism (100% specificity) and able to detect as little as 0.85 ng/μl of V. cholerae genomic DNA.
An electrochemical microbiosensor for DNA has been fabricated based on new acrylic microspheres modified with reactive N-acryloxysuccinimide (NAS) functional groups. Hydrophobic poly(n-butylacrylate-N-acryloxysuccinimide) microspheres were synthesized in an emulsion form with a simple one-step photopolymerization technique. Aminated DNA probe was attached to the succinimde functional group of the acrylic microspheres via covalent bonding. The hybridization of the immobilized DNA probe with the complementary DNA was studied by differential pulse voltametry using anthraquninone-2-sulfonic acid monohydrate sodium salt (AQMS) as the electroactive hybridization label. The influences of many factors such as duration of DNA probe immobilization and hybridization, pH, type of ions, buffer concentrations, ionic strength, operational temperature and non-complementary DNA on the biosensor performance were evaluated. Under optimized conditions, the DNA microbiosensor demonstrated a linear response range to target DNA over a wide concentration range of 1.0 × 10(-16) and 1.0 × 10(-8) M with a lower limit of detection (LOD) of 9.46 × 10(-17) M (R(2) = 0.97). This DNA microbiosensor showed good reproducibility with 2.84% RSD (relative standard deviation) (n = 3). Application of the NAS-modified acrylic microspheres in the construction of DNA microbiosensor had improved the overall analytical performance of the resultant DNA microbiosensor when compared with other reported DNA biosensors using other nano-materials for membranes and microspheres as DNA immobilization matrices.
A non-enzymatic glucose sensor of multi-walled carbon nanotube-ruthenium oxide/composite paste electrode (MWCNT-RuO(2)/CPE) was developed. The electrode was characterized by using XRD, SEM, TEM and EIS. Meanwhile, cyclic voltammetry and amperometry were used to check on the performances of the MWCNT-RuO(2)/CPE towards glucose. The proposed electrode has displayed a synergistic effect of RuO(2) and MWCNT on the electrocatalytic oxidation of glucose in 3M NaOH. This was possible via the formation of transitions of two redox pairs, viz. Ru(VI)/Ru(IV) and Ru(VII)/Ru(VI). A linear range of 0.5-50mM glucose and a limit of detection of 33 μM glucose (S/N=3) were observed. There was no significant interference observable from the traditional interferences, viz. ascorbic acid and uric acid. Indeed, results so obtained have indicated that the developed MWCNT-RuO(2)/CPE would pave the way for a better future to glucose sensor development as its fabrication was without the use of any enzyme.
A new cobalt(II) ion selective electrode based on palladium(II) dichloro acetylthiophene fenchone azine(I) has been developed. The best membrane composition is found to be 10:60:10:21.1 (I)/PVC/NaTPB/DOP (w/w). The electrode exhibits a Nerstian response in the range of 1.0 × 10(-1)-1.0 × 10(-6)M with a detection limit and slope of 8.0 × 10(-7)M and 29.6 ± 0.2 mV per decade respectively. The response time is within the range of 20-25s and can be used for a period of up to 4 months. The electrode developed reveals good selectivity for cobalt(II) and could be used in pH range of 3-7. The electrode has been successfully used in the determination of cobalt(II) in water samples.
The removal of Reactive Black 5 dye in an aqueous solution by electrocoagulation (EC) as well as addition of flocculant was investigated. The effect of operational parameters, i.e. current density, treatment time, solution conductivity and polymer dosage, was investigated. Two models, namely the artificial neural network (ANN) and the response surface method (RSM), were used to model the effect of independent variables on percentage of dye removal. The findings of this work showed that current density, treatment time and dosage of polymer had the most significant effect on percentage of dye removal (p<0.001). In addition, interaction between time and current density, time and dosage of polymer, current density and dosage of polymer also significantly affected the percentage of dye removal (p=0.034, 0.003 and 0.024, respectively). It was shown that both the ANN and RSM models were able to predict well the experimental results (R(2)>0.8).
Mature landfill leachate is typically non-biodegradable and contains high concentration of refractory organics. The aim of this research was to optimize operating parameters in electro-Fenton process, for the removal of recalcitrant organics from semi-aerobic landfill leachate using response surface methodology (RSM). Effectiveness of important process parameters H(2)O(2)/Fe(2+) molar ratio, current density, pH and reaction time were determined, optimized and modeled successfully. Significant quadratic polynomial models were obtained (R(2)=0.9972 and 0.9984 for COD and color removals, respectively). Numerical optimization based on desirability function were employed; in a 43 min trial 94.07% of COD and 95.83% of color were removed at pH 3 and H(2)O(2)/Fe(2+) molar ratio 1, while current density was 49 mA/cm(2). The results indicate that E-Fenton process was an effective technology for semi-aerobic landfill leachate treatment.
This study investigated the electrochemical oxidation of stabilized leachate from Pulau Burung semi-aerobic sanitary landfill by conducting laboratory experiments with sodium sulfate Na(2)SO(4) (as electrolyte) and graphite carbon electrodes. The control parameters were influent COD, current density and reaction time, while the responses were BOD removal, COD removal, BOD:COD ratio, color and pH. Na(2)SO(4) concentration was 1 g/L. Experiments were conducted based on a three-level factorial design and response surface methodology (RSM) was used to analyze the results. The optimum conditions were obtained as 1414 mg/L influent COD concentration, 79.9 mA/cm(2) current density and 4 h reaction time. This resulted in 70% BOD removal, 68% COD removal, 84% color removal, 0.04 BOD/COD ratio and 9.1 pH. Electrochemical treatment using graphite carbon electrode was found to be effective in BOD, COD and color removal but was not effective in increasing the BOD/COD ratio or enhancing biodegradability of the leachate. The color intensity of the treated samples increased at low influent COD and high current density due to corrosion of electrode material.
Leachate pollution is one of the main problems in landfilling. Researchers have yet to find an effective solution to this problem. The technology that can be used may differ based on the type of leachate produced. Coliform bacteria were recently reported as one of the most problematic pollutants in semi-aerobic (stabilized) leachate. In the present study, the performance of the Electro-Fenton process in removing coliform from leachate was investigated. The study focused on two types of leachate: Palau Borung landfill leachate with low Coliform content (200 MPN/100 m/L) and Ampang Jajar landfill leachate with high coliform content (>24 × 10(4)MPN/100 m/L). Optimal conditions for the Electro-Fenton treatment process were applied on both types of leachate. Then, the coliform was examined before and after treatment using the Most Probable Number (MPN) technique. Accordingly, 100% removal of coliform was obtained at low initial coliform content, whereas 99.9% removal was obtained at high initial coliform content. The study revealed that Electro-Fenton is an efficient process in removing high concentrations of pathogenic microorganisms from stabilized leachate.
A novel glassy carbon electrode (GCE) modified with a composite film of poly (4-vinylpyridine) (P4VP) and multiwalled carbon nanotubes (P4VP/MWCNT GCE) was used for the voltammetric determination of paracetamol (PCT). This novel electrode displayed a combined effect of P4VP and MWCNT on the electro-oxidation of PCT in a solution of phosphate buffer at pH 7. Hence, conducting properties of P4VP along with the remarkable physical properties of MWCNTs might have combined effects in enhancing the kinetics of PCT oxidation. The P4VP/MWCNT GCE has also demonstrated excellent electrochemical activity toward PCT oxidation compared to that with bare GCE and MWCNT GCE. The anodic peak currents of PCT on the P4VP/MWCNT GCE were about 300 fold higher than that of the non-modified electrodes. By applying differential pulse voltammetry technique under optimized experimental conditions, a good linear ratio of oxidation peak currents and concentrations of PCT over the range of 0.02-450 μM with a limit of detection of 1.69 nM were achieved. This novel electrode was stable for more than 60 days and reproducible responses were obtained at 99% of the initial current of PCT without any influence of physiologically common interferences such as ascorbic acid and uric acid. The application of this electrode to determine PCT in tablets and urine samples was proposed.
We developed a multiplex enzyme-based electrochemical genosensor for sequence-specific detection of multiplex linear-after-the-exponential-PCR amplicons that targeted toxigenic Vibrio cholerae O1 and O139 using novel screen-printed gold electrode bisensors.
Nanostructured network-like MnO2-NiO composite electrodes were electrodeposited onto stainless steel substrates via different electrodeposition modes, such as chronopotentiometry, chronoamperometry, and cyclic voltammetry, and then subjected to heat treatment at 300°C for metal oxide conversion. X-ray diffraction, field emission scanning electron microscopy, and transmission electron microscopy were used to study the crystalline natures and morphologies of the deposited films. The electrochemical properties were investigated using cyclic voltammetry and charge/discharge tests. The results revealed that the electrochemical performance of the as-obtained composite electrodes depended on the electrodeposition mode. The electrochemical properties of MnO2-NiO composite electrodes prepared using cyclic voltammetry exhibited the highest capacitance values and were most influenced by the deposition cycle number. The optimum specific capacitance was 3509 Fg-1 with energy and power densities of 1322 Wh kg-1 and 110.5 kW kg-1, respectively, at a current density of 20 Ag-1 in a mixed KOH/K3Fe(CN)6 electrolyte.
The composite metal oxide electrode films were fabricated using ex situ electrodeposition method with further heating treatment at 300°C. The obtained composite metal oxide film had a spherical structure with mass loading from 0.13 to 0.21 mg cm(-2). The structure and elements of the composite was investigated using X-ray diffraction (XRD) and energy dispersive X-ray (EDX). The electrochemical performance of different composite metal oxides was studied by cyclic voltammetry (CV) and galvanostatic charge-discharge (CD). As an active electrode material for a supercapacitor, the Co-Mn composite electrode exhibits a specific capacitance of 285 Fg(-1) at current density of 1.85 Ag(-1) in 0.5 M Na2SO4 electrolyte. The best composite electrode, Co-Mn electrode was then further studied in various electrolytes (i.e., 0.5 M KOH and 0.5 M KOH/0.04 M K3Fe(CN) 6 electrolytes). The pseudocapacitive nature of the material of Co-Mn lead to a high specific capacitance of 2.2 x 10(3) Fg(-1) and an energy density of 309 Whkg(-1) in a 0.5 M KOH/0.04 M K3Fe(CN) 6 electrolyte at a current density of 10 Ag(-1). The specific capacitance retention obtained 67% of its initial value after 750 cycles. The results indicate that the ex situ deposited composite metal oxide nanoparticles have promising potential in future practical applications.
Human papilloma virus (HPV) affects predominantly the genital area, which includes vagina, cervix, penis, vulva scrotum, rectum and anus. Among 100 types of HPV, 14 types are considered to cause the risky cancer. The gene HPV-16 E7 is responsible for the development of cancer with the infected women. Earlier identification of this gene sequence avoids the cancer progression. The targeted HPV-16 E7 sequence was sandwiched by capture and reporter sequences on the carbodiimidazole-modified interdigitated electrode (IDE) surface. Target sequence at 100 f. was paired to the capture sequence immobilized on IDE sensing surface. To this surface, different concentrations of reporter sequence with and without gold rod (GNR) were evaluated. In both cases the detections were attained 1 aM by the reporter sequence pairing and with GNR increments in current were found. This enhancement was found to be 1000 folds, considering the condition was revealed in the absence of reporter. This sandwich detection strategy of capture-target-reporter sequences for HPV-16 detection on the IDE sensing surface helps to diagnose the association of cervical cancer.
Plasticized magnesium ion conducting polymer blend electrolytes based on chitosan (CS): polyvinyl alcohol (PVA) was synthesized with a casting technique. The source of ions is magnesium triflate Mg(CF3SO3)2, and glycerol was used as a plasticizer. The electrical and electrochemical characteristics were examined. The outcome from X-ray diffraction (XRD) examination illustrates that the electrolyte with highest conductivity exhibits the minimum degree of crystallinity. The study of the dielectric relaxation has shown that the peak appearance obeys the non-Debye type of relaxation process. An enhancement in conductivity of ions of the electrolyte system was achieved by insertion of glycerol. The total conductivity is essentially ascribed to ions instead of electrons. The maximum DC ionic conductivity was measured to be 1.016 × 10-5 S cm-1 when 42 wt.% of plasticizer was added. Potential stability of the highest conducting electrolyte was found to be 2.4 V. The cyclic voltammetry (CV) response shows the behavior of the capacitor is non-Faradaic where no redox peaks appear. The shape of the CV response and EDLC specific capacitance are influenced by the scan rate. The specific capacitance values were 7.41 F/g and 32.69 F/g at 100 mV/s and 10 mV/s, respectively. Finally, the electrolyte with maximum conductivity value is obtained and used as electrodes separator in the electrochemical double-layer capacitor (EDLC) applications. The role of lattice energy of magnesium salts in energy storage performance is discussed in detail.
Cobalt oxide nanocubes incorporated with reduced graphene oxide (rGO-Co3O4) was prepared by using simple one-step hydrothermal route. Crystallinity and structural characteristics of the nanocomposite were analyzed and confirmed using X-ray diffraction (XRD) and Raman analysis, respectively. The cubical shape of the Co3O4 nanostructures and the distribution of Co3O4 nanocubes on the surface of rGO sheets were identified through field emission scanning electron microscopy (FESEM) and energy dispersive X-ray (EDX) mapping analysis, respectively. Raman spectra depicted the presence of D and G bands for GO and rGO with different ID/IG values and thus confirmed the reduction of GO into rGO. The electrochemical study reflects that the rGO-Co3O4 nanocomposite shows good electrocatalytic activity in oxidation of depression biomarker serotonin (5-HT) in phosphate buffer (pH 7.2). The detection of 5-HT was carried out by using rGO-Co3O4 nanocomposite modified glassy carbon electrode under dynamic condition using amperometry technique with a linear range of 1-10 μM. The limit of detection and limit of quantification were calculated and found to be 1.128 and 3.760 μM, respectively with a sensitivity value of 0.133 μΑ·μM-1. The sensor showed selectivity in the presence of different interferent species such as ascorbic acid, dopamine and uric acid.
Abdominal aortic aneurysm (AAA) is a serious, life-threatening vascular disease that presents as an enlarged area of the aorta, which is the main artery that carries blood away from the heart. AAA may occur at any location in the aorta, but it is mainly found in the abdominal region. A ruptured AAA causes serious health issues, including death. Traditional imaging techniques, such as computed tomography angiogram, magnetic resonance imaging, and ultrasound sonography, have been used to identify AAAs. Circulating biomarkers have recently become attractive for diagnosing AAAs due to their cost-effectiveness compared to imaging. Insulin-like growth factor 1 (IGF-1), a secreted hormone vital for human atherosclerotic plaque stability, has been found to be an efficient biomarker for AAA identification. In this report, immunosensing was performed by using an InterDigitated electrode (IDE) sensor to detect circulating levels of IGF-1. The detection limit of IGF-1 was found to be 100 fM with this sensor. Moreover, related protein controls (IGF-2 and IGFBP3) were not detected with the same antibody, indicating selective IGF-1 detection. Thus, immunosensing by using an IDE sensor may help to effectively diagnose AAAs and represents a basic platform for further development.
Graphene decorated with graphitic nanospheres functionalized with pyrene butyric acid (PBA) is used for the first time to fabricate a DNA biosensor. The electrode was formed by attaching a DNA probe onto PBA, which had been stacked onto a graphene material decorated with graphene nanospheres (GNSs). The nanomaterial was drop-coated onto a carbon screen-printed electrode (SPE) to create the GNS-PBA modified electrode (GNS-PBA/SPE). A simple method was used to produce GNS by annealing graphene oxide (GO) solution at high temperature. Field emission scanning electron micrographs confirmed the presence of a spherical shape of GNS with a diameter range of 40-80 nm. A stable and uniform PBA-modified GNS (GNS-PBA) was obtained with a facile ultrasonication step. Thus allowing aminated DNA probes of genetically modified (GM) soybean to be attached to the nanomaterials to form the DNA biosensor. The GNS-PBA/SPE exhibited excellent electrical conductivity via cyclic voltammetry (CV) and differential pulse voltammetry (DPV) tests using potassium ferricyanide (K3[Fe(CN)6]) as the electroactive probe. By employing an anthraquinone monosulfonic acid (AQMS) redox intercalator as the DNA hybridization indicator, the biosensor response was evaluated using the DPV electrochemical method. A good linear relationship between AQMS oxidation peak current and target DNA concentrations from 1.0 × 10-16 to 1.0 × 10-8 M with a limit of detection (LOD) of less than 1.0 × 10-16 M was obtained. Selectivity experiments revealed that the voltammetric GM DNA biosensor could discriminate complementary sequences of GM soybean from non-complementary sequences and hence good recoveries were obtained for real GM soybean sample analysis. The main advantage of using GNS is an improvement of the DNA biosensor analytical performance.
C-reactive protein (CRP) is an acute phase reactant to be a marker of inflammation and has been correlated with the cardiac injury. An immunoassay was performed using anti-human CRP antibody on an InterDigitated electrode (IDE) sensor to determine and specify CRP concentration for diagnosing the condition of myocardial inflammation. To promote the detection, gold nanoparticle (GNP) was seeded on the aminated-IDE surface. Anti-CRP was hitched on the GNP-seeded surface and identified the abundance of CRP. The limit of quantification was found as 100 fM, and the higher current response was noticed by increasing CRP concentrations with the sensitivity at 1 pM. Furthermore, CRP-spiked human serum did not interfere the determination of CRP and increased the current response, indicating suitability for a real-life sample. Similarly, the control experiments with nonimmune antibody Troponin I are not showing the definite current responses, proving the selective identification of CRP. This method of diagnosing is needful to determine the cardiovascular injury at the right time.
Aptamers are short single-stranded oligonucleotides (either DNA or RNA) that can fold into well-defined three-dimensional (3D) spatial structures which enable them to capture their specific target by complementary shape interactions. Aptamers are selected from large random libraries through the SELEX process and only a small fraction of the sequence is involved in direct docking with the target. In this paper, we describe the possible truncation variants of zearalenone (ZEA) aptamer which might be an effective binding region for the target. The originally selected zearalenone (ZEA) aptamer was 80-mer in length and shown to bind the target with a high affinity (Kd = 41 ± 5 nM). Herein, computational docking simulation was performed with 15 truncated variants to determine the predicted binding energy and responsible binding site of the aptamer-analyte complex. The results revealed that 5 truncated variants had binding energy lower than - 7.0 kcal/mol. Circular dichroism analysis was performed on the shortlisted aptamer and the conformational change of aptamers was observed with the presence of an analyte. Aptamer Z3IN (29-mer) was chosen as the most enhanced affinity for its target with a dissociation constant of 11.77 ± 1.44 nM. The aptamer was further applied in the electrochemical aptasensor of ZEA based on an indirect competitive format. The results demonstrated that the truncated aptamer leads to an enhancement of the sensitivity of the biosensor.