Browsing by Author "Jaydeep Singh"

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Colorimetric detection of hydrogen peroxide and cholesterol using Fe3O4-brominated graphene nanocomposite
(Springer Science and Business Media Deutschland GmbH, 2022) Jaydeep Singh; Rajshree Singh; Shikha Singh; Kheyanath Mitra; Sourov Mondal; Sambhav Vishwakarma; Biswajit Ray
Fe3O4-brominated graphene (Fe3O4-GBR) nanocomposites were synthesized via an in situ method using the precursors FeSO4.7H2O and GBR in different (1:1, 1:2, 2:1, 1:5, 1:10, 1:20, and 5:1) weight ratios at pH 11.5. The Fe3O4-GBR (1:5) nanocomposite in combination with H2O2 and 3,3′,5,5′-tetramethylbenzidine (TMB) showed swift and superior intrinsic peroxidase mimetic enzyme activity compared with the other Fe3O4-GBR composites, GBR and Fe3O4, as observed by colorimetry. It was characterized using high-resolution scanning electron microscopy (HRSEM), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared (FTIR) spectroscopy, powder X-ray diffraction (PXRD), and thermogravimetric analysis (TGA). Its catalytic activity was optimized by varying different parameters, and the optimum conditions for peroxidase mimetic activity were observed using 100 μL Fe3O4-GBR (1 mg/mL), 50 μL TMB (1 mg/mL), and 200 μL H2O2(1 mM) in 400 μL of acetate buffer of pH 2.3 at 30 °C temperature. Kinetic analysis has revealed the Michaelis–Menten kinetic behavior of peroxidase activity with Michaelis–Menten constants (Km) and maximum initial velocities (Vmax) of 0.082 mM and 14.1 nMs−1 respectively, for H2O2 and 0.086 mM and 5.1 nMs−1, respectively for TMB. The limit of detection and linear range were found to be 49.6 μM and 100–880 μM, respectively, for H2O2 and 41.9 μM and 47.6–952.3 μM, respectively, for cholesterol. On this basis, a simple, swift, sensitive, selective, and reproducible colorimetric assay to detect cholesterol levels in blood serum samples using Fe3O4-GBR nanocomposite has been developed. Thus, Fe3O4-GBR composite as compared to Fe3O4 and GBR has shown better peroxidase mimicking activity for biosensing. Graphical abstract: [Figure not available: see fulltext.] © 2022, Springer-Verlag GmbH Germany, part of Springer Nature.
Highly selective fluorescence 'turn off' sensing of picric acid and efficient cell labelling by water-soluble luminescent anthracene-bridged poly(: N -vinyl pyrrolidone)
(Royal Society of Chemistry, 2019) Rajshree Singh; Kheyanath Mitra; Shikha Singh; Sudipta Senapati; Vijay Kumar Patel; Sambhav Vishwakarma; Archana Kumari; Jaydeep Singh; Susanta K. Sen Gupta; Nira Misra; Pralay Maiti; Biswajit Ray
A novel, water-soluble, luminescent anthracene-bridged AA-type bi-arm poly(N-vinylpyrrolidone) (ATC-PNVP) was synthesized using a click reaction between alkyne-terminated PNVP and 9,10-bis(azidomethyl)anthracene. The resultant anthracene-bridged PNVP (ATC-PNVP) was characterized using 1H NMR, FTIR, UV-Vis, and fluorescence spectroscopic methods and GPC analysis. ATC-PNVP showed effective fluorescence properties in an aqueous medium. It showed highly selective "turn off" sensing behaviour towards picric acid, a common nitro-aromatic explosive, with a wide linear range of detection of 0.01-0.3 mM and LOD value of 0.006 mM in water. ATC-PNVP-based paper sensors also showed very effective detection of picric acid in the concentration range 0.001-1.0 mM. Its binding with bovine serum albumin (BSA) was studied using steady-state, synchronous and 3D fluorescence spectroscopy and this study showed effective quenching of the intrinsic fluorescence of BSA and occurrence of a FRET-type interaction. Furthermore, this luminescent ATC-PNVP was efficiently used as a fluorescence microscopy labelling agent in NIH-3T3 and HeLa cells, and showed greater uptake and hence better fluorescent labelling in the cytosols of the tested cells than free 9,10-bis(azidomethyl) anthracene. The cell viability study also showed a very good biocompatible and non-toxic nature of ATC-PNVP at lower working concentrations towards each of the types of cells tested. © 2019 The Royal Society of Chemistry.
L-menthol-based initiators for atom transfer radical polymerization of styrene
(John Wiley and Sons Inc., 2019) Sambhav Vishwakarma; Archana Kumari; Kheyanath Mitra; Shikha Singh; Rajshree Singh; Jaydeep Singh; Susanta K. Sen Gupta; Biswajit Ray
Two new atom transfer radical polymerization (ATRP) initiators, 2-isopropyl-5-methylcyclohexyl 2-bromopropanoate (1) and 2-Isopropyl-5-methylcyclohexyl 2-bromo-2-methylpropanoate (2), have been synthesized by the reaction of 2-bromopropanoyl bromide and 2-bromo-2-methylpropanoyl bromide, respectively, with L-menthol and characterized by 1H and 13C NMR and FTIR spectroscopic studies. ATRP of styrene has successfully been carried out in a control manner using these initiators along with catalyst/ligand system consisting of Cu(I)Br/N,N,N/,N/,N//-pentamethyldiethylenetriamine. Polymerizations have yielded polystyrenes (PSts) of controlled molecular weight with low polydispersity index having a menthyl end group, as confirmed by 1H NMR and gel permeation chromatography [GPC]. The controlled nature of the polymerization has also been confirmed by kinetic study of the polymerization process monitored via 1H NMR and GPC. Initiator 2 has evolved as most efficient among the two. The obtained end-functional PSt has also been used as a macroinitiator for homochain extension with styrene and heterochain extension with methyl methacrylate to produce PSt-b-PMMA, showing the living nature of the polymerization process. In comparison with the PSt sample prepared using widely used initiator ethyl-2-bromo-isobutyrate with almost the same molecular weight and polydispersity, initiator 2-made L-menthyl-capped PSt has shown higher light transmission properties of its dichloromethane solution at ~259 nm, higher thermal stability, lower glass transition temperature, a broad melting temperature, and higher surface roughness over its film. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019, 136, 47964. © 2019 Wiley Periodicals, Inc.
L-menthol-based xanthate mediator for RAFT polymerization of vinyl acetate
(Taylor and Francis Inc., 2020) Sambhav Vishwakarma; Archana Kumari; Kheyanath Mitra; Shikha Singh; Rajshree Singh; Jaydeep Singh; Susanta K. Sen Gupta; Biswajit Ray
A xanthate RAFT agent 2-isopropyl-5-methylcyclohexyl 2-(ethoxycarbonothioyl)thio) propanoate has been synthesized via the reactions of L-menthol with 2-bromo-propionyl bromide in THF in the presence of triethylamine leading to the formation of 2-isopropyl-5-methylcyclohexyl 2-bromopropanoate followed by its reaction with potassium-O-ethyl xanthate in ethanol at room temperature and characterized by 1H, 13C NMR and FTIR. RAFT polymerization of vinyl acetate (VAc) using it has resulted in the formation of well-defined polyVAc in controlled manner. This is evidenced by (i) the observation of the pseudo first order kinetics upto ∼90% conversion, (ii) linear increment of molecular weight (unimodal GPC chromatogram) of the polymer keeping its PDI low with the progress of the reaction upto ∼90% conversion, (iii) the linear increment of the molecular weight of the polymers with low PDI on increasing monomer loading, (iv) chain-end analysis of the polymer using 1H NMR confirming the presence of the RAFT agent fragment at the polymer chain-ends, and (v) successful homo- and hetero-chain extension with VAc and NVP, respectively. L-Menthyl-capped polyvinyl acetate has shown higher (i) light transmission properties of its dichloromethane solution at ∼277 nm, (ii) thermal stability, and (iii) glass transition temperature in comparison to its non-L-Menthyl-capped homolog. © 2019, © 2019 Taylor & Francis Group, LLC.
Pyrene-tagged poly(N-vinyl pyrrolidone) as efficient nano-carrier for anticancer drug delivery
(Taylor and Francis Ltd., 2024) Kheyanath Mitra; Swapan Maity; Archismita Hajra; Shikha Singh; Sourov Mondal; Jaydeep Singh; Pralay Maiti; Biswajit Ray
Herein, we report the use of self-assembled amphiphilic pyrene-tagged poly(N-vinyl pyrrolidone) (PyPNVP) micelles as effective anticancer delivery vehicle. Self-assembly phenomenon of PyPNVP has been studied in aqueous medium. Anticancer drug doxorubicin has been encapsulated in the hydrophobic micellar core and in vitro release profiles have been explored in four different pH values (pH 7.4 − 1.4). The drug-loaded construct has shown pH-responsive higher drug release at lower pH. Anticancer activity of the construct has been studied against human squamous cell carcinoma of the cervix uteri cell line. The in vitro study has shown the highly effective tumoricidal activity. © 2023 Taylor & Francis Group, LLC.
Selective nitration of phenol to: O -nitrophenol in the presence of metal-free reduced graphene oxide at room temperature
(Royal Society of Chemistry, 2020) Sourov Mondal; Jaydeep Singh; Shikha Singh; Sambhav Vishwakarma; Kheyanath Mitra; Archana Kumari; Rajshree Singh; Susanta K. Sen Gupta; Biswajit Ray
We report here a reduced graphene oxide (RGO)-catalyzed ultra-efficient, highly selective and low temperature synthesis of o-nitrophenol using phenol and nitric acid in an equimolar ratio. The effects of various parameters such as concentration of reactants, type of catalyst, weight of the catalyst, solvent, temperature and time of reaction on the catalytic reaction have been explored. The optimum conditions for the catalytic nitration reaction have been observed using a 1 : 1 molar ratio of nitric acid to phenol in the presence of 50 mg RGO in dichloroethane at room temperature for 3 h with a turn over frequency (TOF) of 10.96 × 1017 molecules g-1 s-1 and a reaction rate of 12.17 × 1014 molecules mL-1 s-1. In order to explore the decrease in efficiency of the catalyst during reuse, both the parent catalyst and used catalyst have been characterized by XRD, Raman, SEM, EDX, BET and FT-IR. The large surface area of RGO promotes the catalytic activity of aromatic compounds via smooth and high conversion of products with fine regioselectivity. So this protocol opens up a new avenue for the selective synthesis of o-nitrophenol using reduced graphene oxide at room temperature. This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique.
Study of the fluorescence based applications of water soluble (N, P) doped carbon dots synthesized via microwave assisted green pyrolysis
(Bentham Science Publishers, 2020) Rajshree Singh; Shikha Singh; Sudipta Senapati; Kheyanath Mitra; Jaydeep Singh; Susanta K.S. Gupta; Nira Misra; Pralay Maiti; Biswajit Ray
Background: Water soluble nitrogen and phosphorus doped carbon dots (CD) have been synthesized using citric acid, tris(2-aminoethyl)amine and orthophosphoric acid via one step microwave assisted pyrolytic method. Methods: The CD synthesized has been characterized using FTIR, UV-Vis, fluorescence spectroscopy and EDAX coupled with SEM techniques. Results: SEM study has shown the formation of nanosized CD with an average size of ~18 nm. Elemental analysis via EDAX has confirmed successful incorporation of nitrogen (30.8% wt) and phosphorus (5.7% wt) atoms in it. The steady state and 3D fluorescence spectroscopic studies have shown its efficient fluorescence emission with emission maxima in the region of ~450 nm. It has shown efficient “turn off” fluorescence behaviour towards transition metal ions like Fe2+ and Co2+ ions and toxic nitrophenolic compounds like p-nitrophenol and picric acid. Its efficient interaction with BSA has been revealed in terms of fluorescence quenching of BSA by steady state, synchronous and 3D fluorescence spectroscopy. It has shown very good in vitro biocompatibility and enhanced cell adhesion properties towards NIH 3T3 fibroblast cells. Moreover, fluorescence microscopy has shown significant uptake of CD by the tested cell line. Conclusion: Such bio-compatible nitrogen and phosphorous doped CD can be potentially useful to estimate metal ions, p-nitrophenol and picric acid using fluorescence spectroscopy and for fluorescence based bio-imaging. © 2020 Bentham Science Publishers.