Isolation of a free radical‐scavenging antioxidant from water spinach (Ipomoea aquatica Forsk)

Ipomoea aquatica Forsk, a green leafy vegetable that is a rich source of vitamins and amino acids with many health benefits, has been explored for the isolation and identification of its bioactive compounds. Activity‐guided repeated fractionation of a methanol extract on a silica gel column followed by an XAD column yielded a compound that exhibited antioxidant activity with an EC₅₀ value of 83 ± 1.02 µg ml^?1 reaction mixture. It also showed very strong lipid peroxidation‐inhibitory activity in a liposome model system with an EC₅₀ value of 72.2 ± 0.9 µg ml^?1. However, it showed negligible metal‐chelating activity. Based on UV, 2D nuclear magnetic resonance and gas chromatography/mass spectrometry studies, the compound was tentatively identified to be 7‐O‐β‐D ‐glucopyranosyl‐dihydroquercetin‐3‐O‐α‐D ‐glucopyranoside. This is the first report on the antioxidant properties of I aquatica leaf extracts. Copyright © 2005 Society of Chemical Industry     

Evaluation of phosphoglycolipid elimination from rice bran oil by a nonporous membrane using NMR spectroscopy

The presence of phosphoglycolipids (PGL) in degummed rice bran oil (RBO) affects the color in the subsequent refining process, posing problems in producing a final product of acceptable quality. A nonporous membrane could achieve near complete removal of phospholipids even under hexane‐diluted conditions, including PGL present in RBO. PGL from glycolipid fractions isolated from various membrane process stream samples, analyzed by ¹H, ¹³C and ³¹P NMR spectroscopic techniques, indicated the absence of PGL in the permeate, besides identifying them to be oleates/linoleates of phosphatidic acid. Hence, the efficacy of a nonporous membrane in the removal of PGL suggests its application for effective degumming of crude RBO.     

Eu(3+) doped gadolinium oxysulfide (Gd(2)O(2)S) nanostructures-synthesis and optical and electronic properties

One-dimensional Eu(3+) doped gadolinium oxysulfide (Gd(2)O(2)S:Eu(3+)) nanotubes/nanorods have been synthesized via precursors of Gd(OH)(3) nanostructures using a hydrothermal technique. The blue-shifts in the optical spectra for the Gd(2)O(2)S:Eu(3+) system corresponding to the fundamental absorption and Eu(3+)-X(2-) ligand (X = O/S) charge transfer bands (CTBs) are significant (～0.22-0.36?eV) with respect to the bulk counterpart. The nanotubes are good candidates for investigating the size-induced electrical and optical properties of functional oxysulfides. In order to identify the origin and nature of the electronic transitions observed in the visible region, optical and photo-induced impedance measurements have been extended to the nanotubes in this report.     

Structure–thermomechanical property correlation of moisture cured poly(urethane-urea)/clay nanocomposite coatings

A series of poly(urethane-urea)/clay nanocomposite coatings were prepared by moisture curing of isophorone diisocyanate (IPDI) capped hydroxyl terminated polybutadiene (HTPB)/clay dispersions in a relative humidity (RH) of 50% at 25 °C. The curing progress was studied by periodic measurement of gel fraction of the coating samples. The studies revealed tortuosity effects of clay toward moisture diffusion, thus delaying the induction period of gelation, time for complete cure and rate of gel formation of the nanocomposite coatings. The clay platelets were found to be intercalated in the poly(urethane-urea) matrix, evidenced from wide angle X-ray diffraction (WAXD) and transmission electron microscopy (TEM). Effects of nanoclay on state of the hard and soft segments were investigated by WAXD, differential scanning calorimetry (DSC), temperature modulated DSC (MDSC) and solid-state nuclear magnetic resonance spectroscopy (NMR). WAXD studies revealed unusually ordered hard segment morphology of the moisture cured poly(urethane-urea) and its nanocomposites. Slower soft segment dynamics upon clay addition was evident from concentration dependant broadening of the line widths of the NMR peaks, and decreasing reversible heat capacity changes at soft segment glass transition. The volume fraction of immobilized soft segments of the nanocomposites was determined from MDSC and was found to increase linearly with clay loading. The mechanical property analysis showed simultaneous reinforcement and toughening effect of nanoclay on the MCPU matrix. The increment in mechanical property of the nanocomposites varied proportionately with the volume fraction of immobilized soft segments.     

Tribological studies of polymer based ceramic–metal composites processed at ambient temperature

Use of composite material is increasing due to economical processing of complicated shapes in large quantities. Addition of fiber/particulates improves the composite strength. In the current study, the tribological characterization of polymer based particulate composites which are processed at room temperature are investigated. The friction and wear behavior of polystyrene reinforced with steel powder (polymer–metal), alumina powder (polymer–ceramic) and a mix of steel and alumina powders (polymer–metal–ceramic) have been investigated under dry sliding conditions using a pin-on-disc tribometer. Tests were conducted at different normal loads and sliding velocities at room temperature. Coefficient of friction and wear loss during the wear tests are determined. Presence of metal and ceramic particulates affects the tribological behavior of the composite. The rise in temperature of the pin during sliding was measured. The rise in contact temperature is influenced by the composition which in turn influences the wear behaviour. The polymer–ceramic composite exhibits the lowest wear rate among the materials investigated.     

Amyloglucosidase-catalysed synthesis of curcumin-bis-α-d-glucoside—a response surface methodological study

Response surface methodology (RSM) was employed to optimize amyloglucosidase-catalyzed synthesis of curcumin-bis-α-d-glucoside. A central composite rotatable design (CCRD) was employed involving five variables (enzyme concentration, curcumin concentration, incubation period, buffer concentration and pH) at five levels. A second-order polynomial equation with a R ² value 0.9 showed good correspondence between experimental and predicted yields. Three-dimensional surface and contour plots generated described the catalytic efficiency of amyloglucosidase under the reaction conditions employed. A maximum conversion of 35% was predicted for curcumin concentrations above 0.55 mmol at 35–60% (w/w d-glucose) amyloglucosidase concentrations. While lower (<35%) amyloglucosidase concentrations converted less, concentrations >60% could be inhibitory to curcumin. Extent of glucosylation was governed by a critical buffer (0.95–1.0 ml of 0.01 M pH 6.0) to enzyme ratio (15–45% w/w d-glucose). Experiments under optimum predicted conditions of 16.9% (w/w d-glucose) amyloglucosidase, 0.33 mmol curcumin, 120 h incubation period, 0.1 mM (1.0 ml of 0.01 M) buffer concentration at pH 7.5 gave a conversion yield of 56.3%. Validation experiments carried out under selected random conditions also showed good correspondence between experimental and predicted yields.     

Measurement of ultrasonic wave velocity in a solid under gas pressures up to 0·4 GPa

A set-up is described for the measurement of longitudinal and transverse wave velocities in a solid under gas pressures up to 0·4 GPa. To check the performance of the set-up, the elastic constants of Se and As₂Se₃ glasses and their pressure derivatives were obtained from the wave velocity data and compared with the data available in the literature.     

Barium Holmium Zirconate, A New Perovskite Oxide: II, Synthesis as Nanoparticles through a Modified Combustion Process

Nanoparticles of barium holmium zirconate, a new complex perovskite ceramic oxide, has been synthesized using a modified self-propagating combustion process. The solid combustion products obtained were characterized by X-ray diffraction (XRD), electron diffraction, differential thermal analysis, thermogravimetric analysis, infrared spectroscopy, particle size analysis, surface area determination, and high-resolution transmission electron microscopy. The XRD and electron diffraction studies have shown that the as-prepared powder is phase pure Ba₂HoZrO_5.5 and has a complex cubic perovskite (A₂BB'O₆) structure with a lattice constant a = 8.428 Å. The transmission electron microscopic investigation has shown that the particle size of the as-prepared powder was in the range 4–16 nm with a mean grain size of 8.2 nm. The nanoparticles of Ba₂HoZrO_5.5 obtained by the present method could be sintered to 98% theoretical density at 1500°C.