Rajendra Srivastava

Simultaneous and sensitive determination of ascorbic acid, dopamine, uric acid, and tryptophan with silver nanoparticles-decorated reduced graphene oxide modified electrode.

In this paper, we report the synthesis of silver nanoparticle-decorated reduced graphene oxide composite (AgNPs/rGO) by heating the mixture of graphene oxide and silver nitrate aqueous solution in the presence of sodium hydroxide. This material was characterized by means of X-ray diffraction, UV-vis spectroscopy, and transmission electron microscopy. AgNPs/rGO based electrochemical sensor was fabricated for the simultaneous determination of ascorbic acid, dopamine, uric acid, and tryptophan. Electrochemical studies were carried out by using cyclic voltammetry, linear sweep voltammetry, and chronoamperometry. AgNPs/rGO modified electrode exhibited excellent electrocatalytic activity, stability, sensitivity, and selectivity with well-separated oxidation peaks toward ascorbic acid, dopamine, uric acid, and tryptophan in the simultaneous determination of their quaternary mixture. The analytical performance of this material as a chemical sensor was demonstrated for the determination of ascorbic acid and dopamine in commercial pharmaceutical samples such as vitamin C tablets and dopamine injections, respectively. The applicability of this sensor was also extended in the determination of uric acid in human urine samples.

Hydrothermal synthesis of CuO micro-/nanostructures and their applications in the oxidative degradation of methylene blue and non-enzymatic sensing of glucose/H2O2.

In this paper, we report on the amino acids-/citric acid-/tartaric acid-assisted morphologically controlled hydrothermal synthesis of micro-/nanostructured crystalline copper oxides (CuO). These oxides were characterized by means of X-ray diffraction, nitrogen sorption, scanning electron microscopy, Fourier transform infrared, and UV-visible spectroscopy. The surface area of metal oxides depends on the amino acid used in the synthesis. The formation mechanisms were proposed based on the experimental results, which show that amino acid/citric acid/tartaric acid and hydrothermal time play an important role in tuning the morphology and structure of CuO. The catalytic activity of as-synthesized CuO was demonstrated by catalytic oxidation of methylene blue in the presence of hydrogen peroxide (H(2)O(2)). CuO synthesized using tyrosine was found to be the best catalyst compared to a variety of CuO synthesized in this study. CuO (synthesized in this study)-modified electrodes were used for the construction of non-enzymatic sensors, which displayed excellent electrocatalytic response for the detection of H(2)O(2) and glucose compared to conventional CuO. The high electrocatalytic response observed for the CuO synthesized using tyrosine can be correlated with the large surface area, which enhances the accessibility of H(2)O(2)/glucose molecule to the active site that results in high observed current. The methodology adopted in the present study provides a new platform for the fabrication of CuO-based high-performance glucose and other biosensors.

Direct synthesis of metal oxide incorporated mesoporous SBA-15, and their applications in non-enzymatic sensing of glucose.

One-step direct synthetic route is reported for the preparation of M-SBA-15 materials (M=Cu, Ni, Co, Fe, and Mn) with nSi/nM ratios ranging from 100 to 10 under mild acidic condition than conventionally employed for the synthesis of Si-SBA-15. Materials were characterized by a complementary combination of X-ray diffraction, nitrogen sorption, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared, and UV-visible spectroscopy. Experimental evidences show that metal oxides are incorporated in the pore wall of SBA-15 matrices. A non-enzymatic electrochemical sensor device was fabricated for glucose detection based on M-SBA-15 materials. Cyclic voltammetry and linear sweep voltammetry were used to evaluate the catalytic activity of the M-SBA-15 modified electrode toward glucose. It was found that the Cu-SBA-15 (Si/Cu=20) modified electrode showed enhanced electrocatalytic activity toward the oxidation of glucose in alkaline solution compared to that of the conventional CuO and other M-SBA-15 materials investigated in this study. Under the optimal detection conditions, the Cu-SBA-15 (Si/Cu=20) exhibited linear behavior in the concentration range from 10 μM to 20 mM for the quantification of glucose with a limit of detection of 10 μM. Moreover, the Cu-SBA-15 modified electrode was also relatively insensitive to commonly interfering species such as ascorbic acid, uric acid, and dopamine.

Synthesis of Cyclic Carbonates from Olefins and CO2 over Zeolite-Based Catalysts

Metal phthalocyanine complexes (MPc; M = Cu2+, Co2+, Ni2+ and Al3+) encapsulated in zeolite-Y exhibit high catalytic activity for the cycloaddition of CO2 to epichlorohydrin and propylene oxide yielding the corresponding cyclic carbonates. The catalysts could be separated easily from the reaction mixture and reused with little loss in activity. These environmentally benign catalysts are also more efficient than either the “neat” complexes or those obtained by supporting them on solids like silica.

Synthesis of Dicationic Ionic Liquids and their Application in the Preparation of Hierarchical Zeolite Beta

Piperidine- and imidazole-based dicatoinic ionic liquids have been developed for the synthesis of zeolite Beta. Hierarchical Beta has a larger surface area and pore volume than conventional Beta. Beta derived from a dicationic ionic liquid exhibited remarkably higher catalytic activity than the conventional Beta. Experimental evidence and DFT calculations suggest that only a suitable conformation of such dicationic ionic liquids is able to form zeolite Beta (see scheme).

Synthesis of NiCo2O4/Nano-ZSM-5 nanocomposite material with enhanced electrochemical properties for the simultaneous determination of ascorbic acid, dopamine, uric acid and tryptophan

NiCo2O4/Nano-ZSM-5 nanocomposite materials were prepared by the calcination of a physical mixture of NiCo2O4 and Nano-ZSM-5. The materials were characterized by the complementary combination of X-ray diffraction, N2-adsorption and electron microscopic techniques. An electrochemical sensor based on NiCo2O4/Nano-ZSM-5 nanocomposite was constructed for the simultaneous determination of ascorbic acid, dopamine, uric acid, and tryptophan. Among the materials investigated in this study, the NiCo2O4 (30%)/Nano-ZSM-5 modified glassy carbon electrode exhibited the highest electrocatalytic activity with excellent stability, sensitivity, and selectivity. Under the optimum conditions, wide linear ranges were obtained from 1–1200 μM for ascorbic acid, 0.6–900 μM for dopamine, 0.9–1000 μM for uric acid, and 0.9–1000 μM for tryptophan. The detection limits were found to be 0.8, 0.5, 0.7 and 0.7 μM for ascorbic acid, dopamine, uric acid, and tryptophan, respectively. The analytical performance of the developed sensor was demonstrated in the determination of ascorbic acid and dopamine in commercial pharmaceutical preparations (vitamin C tablets and dopamine injections) and uric acid in human urine samples.

Synthesis of mesostructured polyaniline using mixed surfactants, anionic sodium dodecylsulfate and non-ionic polymers and their applications in H2O2 and glucose sensing

Mesostructured polyaniline was prepared by the self-assembly of a mixture of an anionic surfactant, sodium dodecylsulfate and a non-ionic polymeric surfactant (polyethylene glycol, and block-co-polymers such as Pluronic P123 and Brij-35). Materials were characterized by a complementary combination of X-ray diffraction, Scanning electron microscopy, Fourier-transform infrared spectrometer and UV-visible spectrophotometer. Mesostructured polyaniline was used for construction of biosensor, which displayed excellent electrocatalytic response for the detection of H(2)O(2) and glucose compared to conventional polyaniline. The electrocatalytic response observed in the case of mesostructured polyaniline can be correlated with the large surface area and nanopores which enhances the accessibility of H(2)O(2)/glucose molecule to the active site that result in high observed current. The methodology adopted in the present study provides a new platform for the fabrication of polyaniline based high-performance glucose and other biosensors.

Mesoporous materials with zeolite framework: remarkable effect of the hierarchical structure for retardation of catalyst deactivation

Hierarchical MFI zeolite was synthesized following a synthesis route using organic-inorganic hybrid surfactants; the resultant zeolite with mesoporous/microporous hierarchical structure exhibited remarkably high resistance to deactivation in catalytic activity of various reactions such as isomerization of 1,2,4-trimethylbenzene, cumene cracking, and esterification of benzyl alcohol with hexanoic acid, as compared with conventional MFI and mesoporous aluminosilicate MCM-41.

Facile preparation of Ni(OH)2-MnO2 hybrid material and its application in the electrocatalytic oxidation of hydrazine.

A surfactant-free synthetic methodology is reported for the preparation of Ni(OH)2-MnO2 hybrid nanostructures. For comparative study, MnO2 and Ni(OH)2 were also synthesized. Materials were characterized by X-ray diffraction, nitrogen sorption, scanning electron microscopy, and transmission electron microscopy. Ni(OH)2-MnO2 modified electrode is fabricated for the determination of hydrazine. The electrochemical oxidation of hydrazine was investigated using cyclic, linear sweep voltammetries, and chronoamperometry methods. The Ni(OH)2-MnO2 modified electrode showed hydrazine oxidation with decrease in the over voltage and increase in the oxidation peak current, when compared to MnO2, Ni(OH)2, and bare GCE. pH was optimized to obtain the best peak potential and current sensitivity. Chronoamperometry was used to estimate the diffusion coefficient of hydrazine. The kinetic parameters such as overall number of electrons involved in the catalytic oxidation of hydrazine and the rate constant (k) for the oxidation of hydrazine at Ni(OH)2-MnO2 modified electrode were determined. The Ni(OH)2-MnO2 modified electrode exhibited good sensitivity, stability, and reproducibility in hydrazine sensing.

Pd-SAPO-31, an efficient, heterogeneous catalyst for Heck reactions of aryl chlorides

Pd-SAPO-31 exhibits high activity for Heck reactions of aryl chlorides. These catalysts with activities superior to most known solid catalysts can be recovered and reused with negligible loss in activity.