Research Outputs

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Highly sensitive and selective detection of glutathione using ultrasonic aided synthesis of graphene quantum dots embedded over amine-functionalized silica nanoparticles

2022, Kaimal, Reshma, Vinoth, Victor, Shrikrishna Salunke, Amol, Valdes-Morales, Hector, Viswanathan Mangalaraja, Ramalinga, Aljafari, Belqasem, Anandan, Sambandam

Glutathione (GSH) is the most abundant antioxidant in the majority of cells and tissues; and its use as a biomarker has been known for decades. In this study, a facile electrochemical method was developed for glutathione sensing using voltammetry and amperometry analyses. In this study, a novel glassy carbon electrode composed of graphene quantum dots (GQDs) embedded on amine-functionalized silica nanoparticles (SiNPs) was synthesized. GQDs embedded on amine-functionalized SiNPs were physical-chemically characterized by different techniques that included high resolution-transmission electron microscopy (HR-TEM), X-ray diffraction spectroscopy (XRD), UV–visible spectroscopy, Fourier-transform infrared spectroscopy (FTIR), and Raman spectroscopy. The newly developed electrode exhibits a good response to glutathione with a wide linear range (0.5–7 µM) and a low detection limit (0.5 µM) with high sensitivity(2.64 µA µM−1). The fabricated GQDs-SiNPs/GC electrode shows highly attractive electrocatalytic activity towards glutathione detection in the neutral media at low potential due to a synergistic surface effect caused by the incorporation of GQDs over SiNPs. It leads to higher surface area and conductivity, improving electron transfer and promoting redox reactions. Besides, it provides outstanding selectivity, reproducibility, long-term stability, and can be used in the presence of interferences typically found in real sample analysis.

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Synergistic impact of nanoarchitectured GQDs-AgNCs(APTS) modified glassy carbon electrode in the electrochemical detection of guanine and adenine

2023, Dr. Valdes-Morales, Hector, Vinoth, Victor, Kaimal, Reshma, Selvamani, Muthamizh, Michael, Rubina, Pugazhenthiran, Nalandhiran, Viswanathan-Mangalaraja, Ramalinga, Anandan, Sambandam

In this work, a facile green approach for the synthesis of graphene quantum dots (GQDs) embedded on silicate network silver nanocrystals (GQDs-AgNCs(APTS)) is reported. Moreover, glassy carbon-GC electrodes were modified with the prepared nanocomposite containing graphene quantum dots supported on silver nanocrystals (GQDs-AgNCs(APTS)) and applied for simultaneous detection of guanine (GA) and adenine (AD). The chemically modified electrode was assessed during the determination of purine bases by cyclic voltammetry-CV and differential pulse voltammetry-DPV. The incorporation of GQDs-AgNCs(APTS) nanocomposites over the surface of the GC electrode considerably enhances the anodic peak currents and decreases the adenine and guanine peak potentials. Compared to other electrodes, GQDs-AgNCs(APTS)/GC improved the electrochemical behavior towards the detection of adenine and guanine. At optimal conditions, calibration curves were obtained by DPV being linear in the range of 0.1–6.0 μM and 0.1–5.0 μM for guanine and adenine, respectively. The detection limits of both guanine and adenine were estimated as 0.1 μM. Additionally, interferences analyses were performed on the existence of other interferent compounds. Furthermore, the method developed for the identification of GA and AD was proved using fish sperm DNA samples.

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Non-enzymatic glucose sensor and photocurrent performance of zinc oxide quantum dots supported multi-walled carbon nanotubes

2021, Dr. Valdes-Morales, Hector, Vinoth, Victor, Subramaniyam, Gowrishankar, Anandan, Sambandam, Manidurai, Paulraj

Hybrid nanocomposites consisting of carbon nanotubes (CNT)/nanomaterial heterostructure play a key part in the excellent performance of nano-devices by coupling different functionalities. In this study, a glucose sensor was fabricated by immobilizing zinc oxide quantum dots (ZnO QDs) on multiwall carbon nanotubes (MWCNTs) nanocomposites using ultrasonication in an ease and economical method. ZnO QDs with ~ 3–8 nm diameters were grown and anchored on the surface of MWCNTs. These nanocomposites were characterized using different spectroscopy and microscopy techniques. XRD reveals the wurtzite structure of ZnO. TEM confirmed that ZnO QDs were anchored onto MWCNTs. The synthesized nanocomposites were applied as a sensor for electrochemical detection of glucose and as a photoelectric effect for photoelectric current measurements. The electrochemical properties of the MWCNT/ZnO QDs nanocomposite were enhanced significantly for glucose sensing when compared to pristine ZnO and MWCNTs. Results showed that ZnO QDs anchored over MWCNTs have a sensitivity of 9.36 µA µM− 1 with repeatable results. The detection limit was found to be 0.208 µM. By applying nanocomposites on the sensor, the linear range could be extended from 0.1 to 2.5 µM, which increases the response time to less than 3 s. Experimental results also indicate that the sensor response is unaffected by the common interference agents during glucose-sensing such as sucrose, ascorbic acid, dopamine and uric acid. The proposed sensor was successfully employed to detect glucose levels in human urine samples with satisfactory outcomes.

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Ferrihydrite âˆ’ Graphene oxide foams as an efficient adsorbent for Arsenic(III) removal from an aqueous solution

2023, Dr. Valdes-Morales, Hector, Shanmugaraj, Krishnamoorthy, Vinoth, Victor, Pugazhenthiran, Nalandhiran, Salvo, Christopher, SepĂºlveda, Erwin, Viswanathan-Mangalaraja, Ramalinga

We report the synthesis of a new range of ferrihydrite-graphene oxide (FH-GO) foams using chitosan as cross linker, with varying iron content (5 wt%, 10 wt%, and 20 wt% of FH) as highly efficient adsorbents for the removal of arsenic (III) (As(III)) in an aqueous solution. The sonochemical methods were adopted to synthesize various FH-GO foams and were further characterized by XRD, SEM, TEM, FTIR, Raman, and XPS techniques. The synthesized materials were used for the removal of As(III) in both batch and fixed bed absorbent column methods. The adsorption isotherm results showed that the 10 wt% of FH-GO foams demonstrated a superior adsorbent for the As(III) with high adsorption capacities than that of the other two FH-GO foams (5 wt% and 20 wt% of FH). Moreover, 10 wt% of FH-GO foams was also demonstrated to be nearly a complete (>98.4%) removal of As(III) ions at neutral pH 7. The adsorption isotherm fitted very well with the Langmuir model with the highest accuracy data for all the synthesized adsorbent materials. In addition, the fixed bed absorbent column method was also adopted for the removal of As(III) ions in the water sample, which showed > 99.2% of removal efficiency. The outstanding adsorption capabilities, along with their easy and low-cost synthesis, make these kinds of adsorbents extremely capable for commercial applications in wastewater treatment and drinking water purification.

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Development of an electrochemical enzyme-free glucose sensor based on self-assembled Pt–Pd bimetallic nanosuperlattices

2020, Dr. Valdes-Morales, Hector, Vinoth, Victor, Pugazhenthiran, Nalenthiran, Viswanathan-Mangalaraja, Ramalinga, Syed, Asad, Marraiki, Najat, Anandan, Sambandam

The huge demand for the clinical diagnosis of diabetes mellitus has prompted the development of great-performance sensing platforms for glucose detection. Non-enzymatic glucose sensors are getting closer to their use in realistic applications. In this work, polyvinylpyrrolidone (PVP)-conjugated bimetallic Pt–Pd nanosuperlattices were synthesized precisely through a simple synthesis procedure, leading to controllable spherical morphologies with significantly fine and precise nanostructures in a size range of ∼3–5 nm by the reduction of Pt and Pd precursors in ethylene glycol, using an ultrasonic method. High-resolution transmission electron microscopy (HRTEM) measurements evidenced the formation of Pt–Pd bimetallic nanosuperlattices (BMNSLs). The superlattice-fringe patterns (111) of bimetallic Pt–Pd NSLs were identified in the HRTEM images, clearly showing their crystalline nature. The prepared material was used in the electrochemical oxidation of glucose using voltammetry analyses. The experimental evidence indicates that the Pt–Pd BMNSL modified glassy carbon electrode is effective for the selective amperometric detection of glucose in the presence of galactose, sucrose, fructose, lactose, and ascorbic acid. Moreover, its application in the detection of glucose in real serum and urine samples was assessed and good recoveries are achieved. The results show that a Pt–Pd bimetallic nanosuperlattice with high surface area, catalytic activity, and superior selectivity could be a promising material in the generation of novel electrodes for low-cost non-enzymatic glucose sensors.

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Novel MoSe2–Ni(OH)2 nanocomposite as an electrocatalyst for high efficient hydrogen evolution reaction

2021, Dr. Valdes-Morales, Hector, Vinoth, Victor, Rameshbabu, R., Pecchi, Gina, Delgado, Eduardo, Mangalaraja, R.

Nowadays, there is a great demand for low-cost and highly active electrocatalyst for the production of clean renewable energy. However, most of the electrocatalysts are noble metal-based which are very costly and unstable. To counter this, electrochemical water splitting in energy storage systems is been widely applied, using non-noble metal-based nanostructured electrocatalysts. In this work, a novel noble metal-free MoSe2eNi(OH)2 nanocomposite electrocatalyst is synthesized using a multi-step hydrothermal technique for efficient hydrogen evolution reaction (HER). The morphology, structural, chemical composition, and functional features of the synthesized nanomaterials were characterized using different techniques that include scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction analysis (XRD), X-ray photoelectron spectroscopy (XPS), and Raman analysis. The new developed MoSe2eNi(OH)2 nanocomposite combines a high active surface area with a high chemical stability, generating a novel material with a synergistic effect that enhances water splitting process performance. Thus, an outstanding low Tafel slope of 54 mV dec1 is accomplished in the hydrogen evolution reaction.

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Goethite (α-FeOOH) nanoparticles wrapped on reduced graphene oxide nanosheet for sensitive electrochemical detection of arsenic(III)

2023, Dr. Valdes-Morales, Hector, Vinoth, Victor, Shanmugaraj, Krishnamoorthy, Pugazhenthiran, Nalandhiran, Salvo, Christopher, Anandan, Sambandam, Mangalaraja, Ramalinga

The goethite (α-FeOOH) nanoparticles were wrapped on the reduced graphene oxide (rGO) to synthesize the α-FeOOH/rGO nanocomposites. The nanocomposites (NCs) were initially examined for their optical, structural, and morphological properties. The XRD data obtained the crystallite size of the α-FeOOH, showed that the average crystal size for pristine α-FeOOH and α-FeOOH/rGO nanocomposites were about 85 and 90 nm, respectively. The transmission electron microscope confirmed the nanoparticles (NPs) were evenly distributed throughout the reduced graphene oxide sheets. The nanocomposites improved glassy carbon electrodes (GCE), making them efficient sensors for detecting the arsenic(III) (As+3) in a pH 5 phosphate buffer solution with an Ag/AgCl reference electrode. The detection limit for As+3 was 0.07 μgL−1 and the resulting sensitivity was 0.39 μA−1 μgL−1 in the linear dynamic range of 0.1–10 μgL−1. The α-FeOOH/rGO/GCE was more sensitive than its original and showed a synergistic effect due to the influence of α-FeOOH on the properties of rGO. The α-FeOOH/rGO NCs-modified GCE electrode performed as a promising sensor, by separating the common interfering ions. Moreover, the modified electrode exhibited remarkable stability, repeatability, and potential real-time application towards the detection of arsenic(III). Additionally, the proposed approach has been successfully applied to the detection of As+3 in the real water sample.