An electrochemical immunosensor based on covalent immobilization of okadaic acid onto screen printed carbon electrode via diazotization-coupling reaction

In this work, an electrochemical method based on the diazonium-coupling reaction mechanism for the immobilization of okadaic acid (OA) on screen printed carbon electrode was developed. At first, 4-carboxyphenyl film was grafted by electrochemical reduction of 4-carboxyphenyl diazonium salt, followed by terminal carboxylic group activation by N-hydroxysuccinimide (NHS), N-(3-dimethylaminopropyle)-N′-ethyle-carbodiimide hydrochloride (EDC). Hexamethyldiamine was then covalently bound by one of its terminal amine group to the activated carboxylic group. The carboxyl group of okadaic acid was activated by EDC/NHS and then conjugated to the second terminal amine group on other side of the hexamethyldiamine through amide bond formation. After immobilization of OA, an indirect competitive immunoassay format was employed to detect OA. The immunosensor obtained using this novel approach allowed detection limit of 1.44 ng/L of OA, and was also validated with certified reference mussel samples.     

Spectrofluorimetric Protocol for Ceftriaxone in Commercial Formulation and Human Plasma After Condensation with Formaldehyde and Ethyl Acetoacetate

A new spectrofluorimetric method has been developed and validated for the quantification of ceftriaxone in bulk powder, pharmaceutical formulations and spiked human plasma. The developed method is reproducible, accurate, sensitive and cost effective. In this method, ceftriaxone was converted into a fluorescent compound by reacting with 0.8 M ethyl acetoacetate and 25% formaldehyde in a buffered medium (pH = 4.2) at 90 °C. The excitation and emission wavelengths of the fluorescent reaction product are 316 nm and 388 nm respectively. Optimization of the experimental conditions affecting the condensation reaction were carefully carried out and the optimum experimental conditions were incorporated in the procedure. The developed method has a broad linear range (0.2–20 μg mL⁻¹) with a correlation coefficient of 0.9992. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 1.94 × 10⁻² μg mL⁻¹ and 6.47 × 10⁻² μg mL⁻¹ respectively. The common excipients and co-administered drugs were investigated for their interferences effect in the assay. The developed method was validated statistically through recovery studies and successfully applied to ceftriaxone determination in bulk powder, pharmaceutical formulations and spiked human plasma samples. The percent recoveries were found to be in the range of 99.04–100.26% for bulk powder, 98.88–99.92% for pharmaceutical formulations and 94.22–98.48% for spiked human plasma. The results were verified by comparing with reference literature HPLC method and were found in good agreement.     

Particle size dependence of the superconductivity and ferromagnetism in YBCO nanoparticles

Magnetic properties of superconducting yttrium barium copper oxide (YBa₂Cu₃O_7-δ) nanoparticles (31–43 nm) prepared by a chemical route have been studied. These nanoparticles have been found to clearly exhibit ferromagnetism at room temperature while superconducting transition is observed at lower temperatures. The low temperature hysteresis loops show evidence suggesting the presence of a large paramagnetic contribution in addition to the superconducting contributions from the particles. Bulk YBCO obtained by pelletizing and heating the same nanoparticles at a high temperature, displays the usual superconducting characteristics and gives no trace of ferromagnetism down to 10 K. The superconducting transition temperature of the nanoparticles is lower than for the bulk YBCO and there is a trend of decreasing T _c with smaller size of the particles. In contrast the ferromagnetic moment increases with decreasing particle size. The development of ferromagnetism is attributed to the presence of surface oxygen vacancies that lead to electron redistribution on the different ions at the surface. The simultaneous decrease of superconducting T _c and the increase of ferromagnetism with decreasing size considered as being reflective of the increased role of finite size and surface defects that weaken the superconductivity and enhance the ferromagnetism. Possible coexistence of surface ferromagnetism and bulk superconductivity at lower temperatures is discussed.     

OPTIMIZATION OF THE SYNTHESIS OF ACRYLAMIDE HYDROGEL BY γ-RAY IRRADIATION

Hydrogels have been synthesized from 10%, 20%, 30%, 40%, 50% and 60% aqueous solutions of acrylamide monomer by gamma radiation employing doses in the range of 0.2-30 kGy from a Co-60 source. The effect of solution concentration, γ-ray dose, pH and time was studied in order to observe the optimizing conditions in the characterization of hydrogels. Gel fraction increases with dose for all concentrations indicating hundred-percentage conversion of gel at doses ≥5 kGy for homogenous solutions in the range of 20%-50% concentration. On the other hand, 10% solution provides conversion less than 86% even at 30 kGy, whereas 60% monomer makes an inhomogeneous solution which stile gives about 100% gel fraction. Swelling of hydrogels under water with respect to time varies with both the doses and concentrations due to the change of crosslinking density in the gels. The maximum volume change of hydrogels during swelling and water desorption mainly occurs within 24 h. Swelling is also enhanced with the rise of pH due to change of ionic content of the solvent. Considering the amount of gel fraction and the properties of hydrogel, the samples prepared from 20% solution at 5kGy show better results. Moreover, the effect of bacteria on hydrogel was found to be nil, suggesting a prohibition of growth of microorganism in it.     

Physical, electrical and dielectric properties of Ca-substituted strontium hexaferrite (SrFe12O19) nanoparticles synthesized by co-precipitation method

Calcium substituted strontium hexaferrite Ca_xSr_1−xFe₁₂O₁₉ (x=0.0−0.6) nanoparticles are synthesized by chemical co-precipitation method. The synthesized samples are characterized by Fourier Transform Infrared (FTIR), X-ray diffraction (XRD), Scanning Electron Microscopy, Transmission Electron Microscopy, DC electrical resistivity and dielectric measurements. FTIR data of uncalcined sample shows that nitrate ions are present which disappeared on calcination at 920 °C. The XRD data shows that a single hexagonal magnetoplumbite phase is formed in samples in which the calcium content, x, is ≤0.20. However, a nonmagnetic phase (α-Fe₂O₃) in addition to the hexagonal phase is also present in samples with x>0.20. The average crystallite size is found between 17 and 29 nm. The DC electrical resistivity increases with increase of calcium content up to level of x=0.2 but decreased on further addition of calcium. The enhanced resistivity of the calcium doped material has potential applications in microwave devices. The variations of dielectric constant and dielectric loss angle are explained on the basis of Maxwell-Wagner and Koops models.     

Polarity Directed Appraisal of Pharmacological Potential and HPLC-DAD Based Phytochemical Profiling of Polygonum glabrum Willd

The present study was designed to evaluate polarity-dependent extraction efficiency and pharmacological profiling of Polygonum glabrum Willd. Crude extracts of leaves, roots, stems, and seeds, prepared from solvents of varying polarities, were subjected to phytochemical, antioxidant, antibacterial, antifungal, antidiabetic, and cytotoxicity assays. Maximum extraction yield (20.0% w/w) was observed in the case of an acetone:methanol (AC:M) root extract. Distilled water:methanol (W:M) leaves extract showed maximum phenolic contents. Maximum flavonoid content and free radical scavenging potential were found in methanolic (M) seed extract. HPLC-DAD quantification displayed the manifestation of substantial quantities of quercetin, rutin, gallic acid, quercetin, catechin, and kaempferol in various extracts. The highest ascorbic acid equivalent total antioxidant capacity and reducing power potential was found in distilled water roots and W:M leaf extracts, respectively. Chloroform (C) seeds extract produced a maximum zone of inhibition against Salmonella typhimurium. Promising protein kinase inhibition and antifungal activity against Mucor sp. were demonstrated by C leaf extract. AC:M leaves extract exhibited significant cytotoxic capability against brine shrimp larvae and α-amylase inhibition. Present results suggest that the nature of pharmacological responses depends upon the polarity of extraction solvents and parts of the plant used. P. glabrum can be considered as a potential candidate for the isolation of bioactive compounds with profound therapeutic importance.     

Fluorescein Hydrazide-Appended Metal–Organic Framework as a Chromogenic and Fluorogenic Chemosensor for Mercury Ions

In this work, we prepared a fluorescein hydrazide-appended Ni(MOF) (Metal–Organic Framework) [Ni₃(BTC)₂(H₂O)₃]·(DMF)₃(H₂O)₃ composite, FH@Ni(MOF). This composite was well-characterized by PXRD (powder X-ray diffraction), FT-IR (Fourier transform infrared spectroscopy), N₂ adsorption isotherm, TGA (thermogravimetric analysis), XPS (X-ray photoelectron spectroscopy), and FESEM (field emission scanning electron microscopy). This composite was then tested with different heavy metals and was found to act as a highly selective and sensitive optical sensor for the Hg²⁺ ion. It was found that the aqueous emulsion of this composite produces a new peak in absorption at 583 nm, with a chromogenic change to a pink color visible to the naked eye upon binding with Hg²⁺ ions. In emission, it enhances fluorescence with a fluorogenic change to green fluorescence upon complexation with the Hg²⁺ ion. The binding constant was found to be 9.4 × 10⁵ M⁻¹, with a detection limit of 0.02 μM or 5 ppb. This sensor was also found to be reversible and could be used for seven consecutive cycles. It was also tested for Hg²⁺ ion detection in practical water samples from ground water, tap water, and drinking water.     

Enhanced bactericidal and in vivo wound healing potential of biosynthesized zinc oxide nanoparticles from psyllium mucilage

The multifunctional zinc oxide nanoparticles are synthesized using a cost-effective, efficient, eco-friendly, simple, and clean synthesis approach. Herein, we reported the antibacterial and wound healing potential of zinc oxide nanoparticles (ZnO-NPs) prepared using psyllium gel (PG) as the reducing and stabilizing agent. The PG-mediated zinc oxide nanoparticles (PG-ZnO-NPs) were characterized using UV–Vis, photoluminescence (PL), FTIR, XRD, Raman, and SEM. UV–Vis spectral studies confirmed the surface plasmonic resonance (SPR) band at 364 nm. PL results demonstrated the fluorescent or emission nature of PG-ZnO-NPs. FTIR analysis confirmed characteristic peaks at 873.82 and 619.88 cm⁻¹ due to the tetrahedral coordination of zinc and the formation of the Zn-O bond. XRD and Raman confirm the formation of PG-ZnO-NPs, whereas SEM analysis revealed PG-ZnO-NPs are rod-shaped, having hexagonal prism-like bases, and EDX exhibited the elemental composition of PG-ZnO-NPs. The as-synthesized PG-ZnO-NPs possessed prominent microbicidal potential against gram-positive (Bacillus subtilis and Bacillus licheniformis) and gram-negative (Escherichia coli and Salmonella shigella) bacterial strains in terms of zone of inhibition (ZOI), minimum inhibitory concentration (MIC), and minimum bactericidal concentration (MBC). In vivo biological investigations with mice show that the synthesized PG-ZnO-NPs possess outstanding biocompatibility and wound healing potential. PG-ZnO-NPs dressing significantly speeds up full-thickness wound repair by triggering a decrease in MMP-1 and MMP-2 and escalating the mRNA levels of collagen types (I & III) and fibronectin. Thus, our work validates that the inclusion of PG-ZnO-NPs in dressing shows excellent potential for acute wound management.     

Excited-state nonadiabatic dynamics simulations on the heptazine and adenine in a water environment: A mini review

Studying the excited-state decay process is crucial for materials research because what happens to the excited states determines how effective the materials are for many applications, such as photoluminescence and photocatalysis. The high computational cost, however, limits the use of high-accuracy theoretical approaches for analyzing research systems containing a significant number of atoms. Time-dependent density functional theory is a practical approach to investigate the photorelaxation processes in these systems, as demonstrated in the studies of the excited-state decays of heptazine-water clusters and adenine in water described in this review. Here, we highlight the importance of conical intersections in the excited-state decay processes of these systems using the aforementioned examples. In the heptazine-water and adenine-water systems, these intersections are associated with the photocatalytic water splitting reaction, caused by a barrierless reaction called water to adenine electron-driven proton transfer. We expect the result would be helpful for researching the excited-state decays of graphitic carbon nitride materials and DNA nucleotides.