A Novel Synthesis and Characterization of Titanium Superoxide and its Application in Organic Oxidative Processes

A novel, exceptionally stable titanium superoxide radical ion was prepared and its structure determined by FTIR, ESR, Raman spectroscopy, X-ray diffraction, thermogravimetric/differential thermal analysis and elemental analysis. This heterogeneous catalyst has been found to be effective for the selective oxidation of aromatic amines and phenols to the corresponding nitro aromatics and p-quinones, respectively. In addition, this non-toxic, inexpensive and reusable catalyst has also been used in aminobromination of olefins, which proceed to give the 1, 2-bromoaminated anti-Markovnikov product. A brief account of these results is summarized in this review.     

Antimicrobial investigation of Linum usitatissimum for the treatment of acne

Light petroleum, dichloromethane and methanolic extracts of Linum usitatissimum were investigated using GC/MS. The main components of three sequential extracts were methyl linolenate (11.9-33.9%) and methyl linoleate (3.4-9.1%). Components possessing antimicrobial activity against acne causing bacteria, namely alpha-linolenic acid (7.0 -7.1%), alpha-terpinene (1.7-3.1%), terpinen-4-ol (1.3-4.6%), 4-cymene (1.6-7.1%) and alpha-pinene (1.1%), were found in varying amounts. Antimicrobial screening indicated that the light petroleum extract was more active against aerobic and anaerobic test strains with a MIC value of 1.25 mg/mL and a MBC of 2.5 mg/mL against S. aureus and P. acnes. A MIC of 2.5 mg/mL was observed against S. epidermidis.     

Synthesis of Metal‐Free Phthalocyanines in Functionalized Ammonium Ionic Liquids

A convenient, fast, efficient, and ecofriendly synthesis of metal‐free phthalocyanines from various substituted phthalonitriles in different hydroxyalkylammonium ionic liquids in the presence of 1,8‐diazabicyclo‐[5,4,0]‐undec‐7‐ene (DBU) is reported in moderate yields. The effect of concentration of DBU and temperature on the synthesis of phthalocyanine in N‐(2‐hydroxyethyl)‐N,N‐dimethylbutylammonium bromide ionic liquid has been examined, and the ionic liquid has been recovered and reused conveniently.     

Determination of the active and inactive metabolites of prasugrel in human plasma by liquid chromatography/tandem mass spectrometry

Two fast and sensitive liquid chromatography/tandem mass spectrometry (LC/MS/MS)-based bioanalytical assays were developed and validated to quantify the active and three inactive metabolites of prasugrel. Prasugrel is a novel thienopyridine prodrug that is metabolized to the pharmacologically active metabolite in addition to three inactive metabolites, which directly relate to the formation and elimination of the active metabolite. After extraction and separation, the analytes were detected and quantified using a triple quadrupole mass spectrometer using positive electrospray ionization. The validated concentration range for the inactive metabolites assay was from 1 to 500 ng/mL for each of the three analytes. Additionally, a 5x dilution factor was validated. The interday accuracy ranged from -10.5% to 12.5% and the precision ranged from 2.4% to 6.6% for all three analytes. All results showed accuracy and precision within +/-20% at the lower limit of quantification and +/-15% at other levels. The validated concentration range for the active metabolite assay was from 0.5 to 250 ng/mL. Additionally, a 10x dilution factor was validated. The interbatch accuracy ranged from -7.00% to 5.98%, while the precision ranged from 0.98% to 3.39%. Derivatization of the active metabolite in blood with 2-bromo-3'-methoxyacetophenone immediately after collection was essential to ensure the stability of the metabolite during sample processing and storage. These methods have been applied to determine the concentrations of the active and inactive metabolites of prasugrel in human plasma.     

Identification and structural characterization of major degradation products of tapentadol by using liquid chromatography–tandem mass spectrometry

Tapentadol, a centrally acting analgesic was subjected to hydrolysis (acidic, alkaline, and neutral), oxidation, photolysis, humidity, and thermal stress conditions as per International Conference on Harmonization prescribed guidelines. Tapentadol was found susceptible to oxidative stress that produced two major degradation products DP-I and DP-II. However, it was stable to hydrolysis, photolysis, and thermal stress conditions. A simple, sensitive, and accurate high-performance liquid chromatography stability-indicating assay method (liquid chromatography–mass spectrometer compatible) was developed and validated for identification and characterization of stressed degradation products of Tapentadol. The chromatographic separation of the drug and its degradation products were achieved on Inertsil ODS, C18 (250 × 4.6 mm, i.d., 5 µm) column using a 12.5 mM aqueous ammonium acetate buffer (with 0.2% triethyl amine and final pH of buffer was adjusted to 3.60 with glacial acetic acid): acetonitrile (75:25, v/v) as a mobile phase. The degradation products were characterized by liquid chromatography mass spectrometry and subsequently its fragmentation pathway as well as plausible mechanism for generation of degradation products was also proposed. The stability indicating high-performance liquid chromatographic method was validated with respect to linearity, precision, and accuracy.     

Synthesis, spectroscopic and cytotoxic studies of biologically active new schiff bases derived from p-nitrobenzaldehyde

Thirteen new Schiff bases derived from p-nitrobenzaldehyde were synthesized by condensation with the appropriate amines. An unusual reduction of the p-nitrobenzaldehyde to the corresponding alcohol was also observed in one of the reactions. The structures of the compounds were identified using spectroscopic techniques. Cytotoxicity for the titled compounds was studied against Brine Shrimp, used as the test animal.     

Highly efficient,economic, and recyclable glutathione decorated magnetically separable nanocomposite for uranium(VI) adsorption from aqueous solution

A green and environment-friendly magnetically separable nanocomposite, glutathione@magnetite was fabricated sonochemically through the functionalization of Fe₃O₄ by glutathione which was well characterized using Fourier-transform infrared spectroscopy, ultravoilet-visible spectroscopy, scanning electron microscope, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction, thermogravimetric analysis, vibrating sample magnetometer, Brunauer-Emmett-Teller, and high-resolution transmission electron microscope. The parameters affecting adsorption including pH, temperature, contact time, initial adsorbate concentration, and adsorbent amount were optimized by batch experiments. The magnetic glutathione@magnetite was applied for the removal of uranium(VI) in water with maximum adsorption capacity found to be 333.33 mg/g in 120 min at a neutral pH at 25 °C showing high efficiency for U(VI) ions. Furthermore, adsorption results obtained from UV-vis spectroscopy were validated by inductively coupled plasma optical emission spectroscopy. The thermodynamic parameters, viz Gibbs free energy (ΔGº), standard enthalpy change (ΔHº), and standard entropy change (ΔSº) of the process were calculated using the Langmuir constants. The pseudo-second-order kinetics model is seen to be applicable for describing the uptake process using a kinetics test. Moreover, desorption studies reveals that glutathione@magnetite can be used repeatedly, and removal efficiency shows only a small decrease after six cycles. Thus, glutathione@magnetite acts as a potential adsorbent for the removal of U(VI) from the water with great adsorption performance.     

Biocompatibility of gold nanoparticles and their endocytotic fate inside the cellular compartment: a microscopic overview

Macrophages are one of the principal immune effector cells that play essential roles as secretory, phagocytic, and antigen-presenting cells in the immune system. In this study, we address the issue of cytotoxicity and immunogenic effects of gold nanoparticles on RAW264.7 macrophage cells. The cytotoxicity of gold nanoparticles has been correlated with a detailed study of their endocytotic uptake using various microscopy tools such as atomic force microscopy (AFM), confocal-laser-scanning microscopy (CFLSM), and transmission electron microscopy (TEM). Our findings suggest that Au(0) nanoparticles are not cytotoxic, reduce the production of reactive oxygen and nitrite species, and do not elicit secretion of proinflammatory cytokines TNF-alpha and IL1-beta, making them suitable candidates for nanomedicine. AFM measurements suggest that gold nanoparticles are internalized inside the cell via a mechanism involving pinocytosis, while CFLSM and TEM studies indicate their internalization in lysosomal bodies arranged in perinuclear fashion. Our studies thus underline the noncytotoxic, nonimmunogenic, and biocompatible properties of gold nanoparticles with the potential for application in nanoimmunology, nanomedicine, and nanobiotechnology.     

Heat transfer for laminar flow through parallel porous disks of different permeability

The problem of temperature distribution and heat transfer for laminar flow through two parallel porous disks of different permeability, has been investigated when the flow is entirely due to injection and/or suction at the two disks. Viscous dissipation terms have been included in the energy equation and the injection and/or suction velocities at the two disks are assumed to be small. The boundaries are kept at constant temperatures. The variation of temperature and Nusselt numbers at the two disks has been graphically depicted for various values of the injection and suction velocities.     

Completeness properties of the pseudocompact-open topology on <Emphasis Type="Italic">C</Emphasis>(<Emphasis Type="Italic">X</Emphasis>)

This is a study of the completeness properties of the space C _ps (X) of continuous real-valued functions on a Tychonoff space X, where the function space has the pseudocompact-open topology. The properties range from complete metrizability to the Baire space property. Dedicated to Professor Robert A. McCoy