Simple, Sensitive, and Rapid Voltammetric Detection of Alloxan on Glassy Carbon Electrodes.

Alloxan is a chemical generally administered to rats to induce diabetes mellitus, and pharmaceutical industries test the efficacy of their diabetic products on these rats. Alloxan is in a redox cycle with dialuric acid; hence, direct estimation of alloxan may not represent the actual concentration of the same in a given matrix. Also, in recent times, alloxan is added to food materials, especially to the all-purpose flour (maida) to bring softness and white color to the flour. Hence, consumption of food items made from such flour could induce diabetic mellitus in individuals, making it imperative to develop an accurate estimation of alloxan in food items. Herein, a voltammetric-based technique is developed to quantify the alloxan in refined wheat flour (maida) using an unmodified glassy carbon electrode (GCE). The electrochemical method offers rapid sensing while the use of an unmodified GCE surface offers repeatability and reproducibility between measurements. First, alloxan is converted to its stable adduct alloxazine by the reaction with o-phenylenediamine. The alloxazine adduct is electrochemically active, and the concentration of alloxan is estimated as a function of alloxazine formed using the voltammetric technique. The common shortfall in alloxan detection mainly involves its short half-life (∼a minute) whereas the alloxazine adduct formed is stable over a period of time. Using the current approach, alloxan concentration ranging from 10 to 600 µM is detected with a sensitivity of 0.0116 µA/µM. A low limit of detection of 1.95 µM with a precision of 1.2% is achieved using the above method. Real sample analysis revealed the presence of alloxan in all-purpose flour (maida-refined wheat flour) and bread purchased from the local market to the values of 35.76 and 25.03 µM, respectively. The same is confirmed using the gold-standard colorimetric technique.

A Robust strategy enabling addressable porous 3D carbon-based functional nanomaterials in miniaturized systems.

3D-porous carbon nanomaterials and their hybrids are ideal materials for energy storage and conversion, biomedical research, and wearable sensors, yet today's fabrication methods are too complicated and inefficient to implement into miniaturized systems. Instead, it is shown here that 3D-carbon nanofibrous electrodes of various designs, shapes and sizes, on flexible substrates, under ambient conditions and without complicated equipment and procedures can simply be "written" via a one-step laser-induced carbonization on electrospun nanofibers. Analytical functionalities are realized as full control over native polymer chemistry doping of the polymer (e.g. with metals) is provided. Similarly, being able to control mat morphology and its impact on the electroanalytical performance was studied. Ultimately, optimized writing conditions were harnessed for superior (bio)analytical sensing of important biomarkers (NADH, dopamine). The new procedure hence paves the way for future controlled studies on this 3D nanomaterial, for a multitude of functionalization and design possibilities, and for mass production capabilities necessary for their application in the real world.

PAMAM Dendrimer Modified Reduced Graphene Oxide Postfunctionalized by Horseradish Peroxidase for Biosensing H2O2.

In this chapter, we describe the tethering of horseradish peroxidase (HRP) to reduced graphene oxide (RGO) for sensing H2O2 in serum. To accomplish this, RGO was synthesized through a green route by reducing graphene oxide (GO) prepared by Hummers method with carrot extract. The RGO was then covalently functionalized by electrochemical amination using fourth generation, amine-terminated PAMAM dendrimers. Subsequently, HRP was postfunctionalized through glutaraldehyde linkage. The synthesized RGO and the functionalization steps were well characterized by spectroscopic, microscopic, and electrochemical techniques. The application of HRP tethered RGO was demonstrated for H2O2 sensing in blood serum. This work provides scope for extending this functionalization strategy for other carbonaceous materials as well.

2D MoSe2 sheets embedded over a high surface graphene hybrid for the amperometric detection of NADH.

Delaminated 2D sheets of MoSe2 were prepared by liquid phase exfoliation and were embedded over high surface area hydrogen exfoliated graphene (HEG) by a simple technique. The MoSe2/HEG hybrid composite exhibits fast heterogeneous electron-transfer (HET) and a high electrochemically active surface area compared to only HEG. When employed for detection of NADH, it exhibits electrooxidation at a low potential of 150 mV (vs. Ag/AgCl) with high sensitivity of 0.0814 µA⋅µM-1⋅cm2 over a wide linear range (1-280 µM), good selectivity, and a low limit of detection (1 µM). The good performance of the composite is due to the homogeneously dispersed 2D sheets of MoSe2 over large-surface area HEG, which retain its electrochemical activity, prevents restacking, and acts as an electron transfer channel. On the basis of the above analytical requirements and its easy synthesis, the hybrid composite represents a robust material for electrochemical sensing. Graphical abstract Schematic of the 2D MoSe2/HEG composite for electrochemical detection of NADH.

Tactical tuning of the surface and interfacial properties of graphene: A Versatile and rational electrochemical approach.

Designing a versatile and rational method for the tactical tuning of the surface and interfacial properties of graphene is an essential yet challenging task of many scientific areas including health care, sensors, energy, and the environment. A method was designed herein to tackle the challenge and tune the surface and interfacial properties of graphene using a simple electrochemical tethering of arylamines that provides diverse reactive end groups to graphene. This method resulted in the preparation of graphenes with thiol, hydroxy, amine, carboxyl, and sulfonate surface functionalities respectively. X-ray photoelectron spectroscopy, scanning electron microscopy, and cyclic voltammetry were used to study the chemical, morphological, and electrochemical properties of the modified graphenes. The results show the promising scope of the reported method towards the tactical tuning of the surface and interfacial properties of graphene. Also, this method can give fundamental insights of the surface tuning of graphene and its structurally similar materials. Hence, this approach can be used to advantageously tune the surface properties of the other structurally similar nanocarbons and their hybrid materials to make them potential candidates for many applications.

Nitric oxide releasing photoresponsive nanohybrids as excellent therapeutic agent for cervical cancer cell lines.

Gold nanoparticles (GNPs) that can release nitric oxide (NO) on visible-light irradiation were prepared using 2-mercapto-5-nitro benzimidazole (MNBI) as stabilizer. These nanoparticles meet overall prerequisites for biomedical applications like small sizes, water solubility, and stability. It was found that even a very low dosage of MNBI-stabilized GNPs exhibit appreciable tumor cell mortality against cervical cancer cell lines, demonstrating the role of NO in killing cancer cells.

Synthesis of gold nanoparticles: an ecofriendly approach using Hansenula anomala.

This work describes a bioassisted approach for the preparation of metal nanoparticles using yeast species Hansenula anomala. Gold nanoparticles were prepared using gold salt as the precursor, amine-terminated polyamidoamine dendrimer as the stabilizer, and the extracellular material from H. anomala as the bioreductant. It could also be demonstrated that, using our approach, small molecules such as cysteine can act as stabilizers as well. This synthetic approach offers a greener alternative route to the preparation of gold sols that are devoid of cellular and toxic chemical components. The ability of as-synthesized gold sol to function as biological ink for producing patterns for the analysis of fingerprints and to act as an antimicrobial reagent is evaluated. The generality of this toxin-free synthetic approach to other metals was assessed using palladium and silver.

Self-assembly and cross-linking of FePt nanoparticles at planar and colloidal liquid-liquid interfaces.

Terpyridine thiol functionalized FePt and Au NPs were self-assembled and cross-linked at the liquid-liquid interfaces using Fe(II) metal ion. Complexation of terpyridine with Fe(II) metal ion leads to NP network and affords stable membranes and colloidal shells at the liquid-liquid interfaces.

From ribbons to nanodot arrays: nanopattern design through reductive annealing.

A new approach to the generation of nanoparticle arrays in periodic as well as non-periodic fashions has been discovered based on reduction of oxidized nanoscroll/nanoribbon precursors in the transmission electron microscope (carbothermal reduction) or by hydrogen annealing. Arrays consisting of nickel arsenide nanoparticles of size 3-4 nm have been generated.