SYNTHESIS AND CHARACTERIzATION OF TRIPHENYLANTIMONY (V) (O-ALKYL,O-CYCLOALKYL AND O-ARYLTRITHIOPHOSPHATES)

Triphenylantimony (V) (O-alkyl,O-cycloalkyl and O-aryltrithiophosphates) of the type Ph ₃ Sb[S ₂ (S)P(OR)] (R = Me, Et, Pr ⁿ , Pr ⁱ , Bu ⁿ , Bu ^s , Bu ⁱ , Am ⁱ , Ph and C.h. = cyclohexyl) have been synthesized for the first time by the reaction of triphenylantimony (V) dibromide with potassium trithiophosphates in 1:1 molar ratio in methanol. These new compounds have been characterized by elemental analysis, molecular weight determinations, and spectroscopic (IR,¹³C and ³¹P NMR) studies. On the basis of these data trigonal bipyramidal geometry has been proposed for these compounds.     

Development of New Atom Transfer Radical Polymerization System by Iron (III)‐Metal Salts Without Using any External Initiator and Reducing Agent

Atom transfer radical polymerization (ATRP) catalyzed by high oxidation state metal salts of FeX₃ is developed for the first time in the absence of both external initiator and reducing agent. Methyl methacrylate (MMA) and styrene are polymerized successfully using FeX₃/Phosphorous ligands with well‐controlled molecular weight distributions (=1.5). The molecular weight of the polymers increases with monomer consumption with the progress of time and the polymerization behaviors show a decent ATRP trend. Activators and initiators are suggested to generate in situ by the addition reaction of MMA and one equivalent of FeX₃. The PMMA synthesized from without‐initiator system is characterized by ¹H, ¹³C and DEPT (distortionless enhancement by polarization transfer nuclear magnetic resonance) nuclear magnetic resonance spectroscopy. Chain extension and copolymerization experiments prove the livingness of the obtained polymer.

     

Comparison of HPLC and MEEKC for Miconazole Nitrate Determination in Pharmaceutical Formulation

A simple solid phase extraction (SPE) method coupled with high performance liquid chromatography (HPLC) using UV detector and microemulsion electrokinetic chromatography (MEEKC) has been developed and compared for the quantitative determination of miconazole nitrate in pharmaceutical formulation. For HPLC method, two parameters were optimized, namely, the wavelength and the mobile phases. The optimized condition was at the 225 nm wavelength and the mobile phase of ACN:MeOH (90:10 v/v). There are seven MEEKC parameters that were optimized, in this research, which were applied to voltage, temperature, wavelength, sodium dodecyl sulfate (SDS) concentration, buffer pH, buffer concentration and butan-1-ol concentration. The optimum MEEKC condition was obtained using 86.35 % (w/w) 2.5 mM borate buffer pH 9, 0.25 % (w/w) SDS, 0.8 % (w/w) ethyl acetate, 6.6 % w/w butan-1-ol and 6.0 % (w/w) acetonitrile. The combination of SPE using a diol column with HPLC–UV and the MEEKC methods were successfully applied for the determination of miconazole nitrate in a pharmaceutical formulation with the recovery percentage of 98.35 and 92.50 %, respectively.     

Modelling and measuring the thermal conductivity of multi-metallic Zn/Cu nanofluid

A metallic nanofluid is a suspension of metallic nanoparticles in a base fluid. Multi-metallic nanoparticles are a combination of two or more types of metallic particles. Such multi-metallic nanoparticles were suspended in water using an ultrasonic vibrator for different total volume fractions and different ratios of metallic/metallic nanoparticles. A transient hot wire setup was built to measure the thermal conductivity of the nanofluid at different temperatures. The experimental results were in good agreement with the results in the literature. Then, the experimental results were used as input data for an adaptive neural fuzzy inference system (ANFIS) to predict the thermal conductivity of the multi-metallic nanofluid. The maximum deviation between the ANFIS results and experimental measurements was 1 %. The predicted results and the experimental data were compared with other models. The ANFIS model was found to have good ability to predict the thermal conductivity of the multi-metallic nanofluid over the range of the experimental results.     

Adsorption and Micellization Behavior of Cationic Surfactants (Gemini and Conventional)—Amphiphilic Drug Systems

In the present work, the behavior of mixed drug–surfactant systems has been studied by surface tension measurements. The drug used in this work is adiphenine hydrochloride (ADP) and the surfactants are of m-s-m type geminis, i.e., alkanediyl-α,ω-bis(dimethylalkylammonium bromide), with m = (14, 16), s = (4, 5, 6), and conventional alkyltrimethylammonium bromides (CTAB, TTAB). The excess surface concentration (Γ _max ) increases and the minimum head group area at the air/water interface (A _min) decreases with increasing concentration of surfactant in the drug solution. Both the critical micelle concentration (cmc) and ideal cmc (cmc*) values decrease with mole fraction of surfactants. Also, the cmc values are lower than cmc*, indicating attractive interactions are present in the mixed micelles. The mole fractions of surfactant in the micelles $ \left( {X_{1}^{m} } \right) $ and monolayers $ \left( {X_{1}^{\sigma } } \right) $ , as well as the respective interaction parameters ( $ \beta^{m} $ , $ \beta^{\sigma } $ ), indicate that monolayer formation is easier than micelle formation due to the rigid hydrophobic part of the drug.     

Micelle-Catalyzed Interaction Between [Ni(II)-Gly-Gly]+ and Ninhydrin

The effect of cationic micelles of cetyltrimethyl ammonium bromide (CTAB) on the observed pseudo-first-order rate constant for the interaction of nickel dipeptide complex [Ni(II)-Gly-Gly]⁺ with ninhydrin has been studied spectrophotometrically. At constant temperature and pH, increase in the [CTAB] from 0.0 to 60.0 × 10^?3 mol dm^?3 caused nearly three-fold increase of the rate constant. The micellar catalysis is explained in terms of the pseudophase model. From the observed kinetic data, binding constants of micelle–[Ni(II)-Gly-Gly]⁺ (K _S), and micelle–ninhydrin (K _N) are evaluated, respectively, to be 5.3 mol^?1 dm³ and 84.0 mol^?1 dm³. The role of added inorganic (NaCl, NaBr, Na₂SO₄) and organic salts (NaBenz, NaSal) on the reaction rate has also been examined.     

Ultra Moisturizing Anti-Wrinkle Lotion Enriched with Tocotrienols

A stable palm-based anti-wrinkle lotion enriched with tocotrienols was successfully prepared. The stability of the product was due to the presence of liquid crystalline structure in the emulsion system. It helps in bringing the active to the dermis layer. Functionality active ingredients such as tocotrienols and anti-wrinkle were added in the formulation. A commercial plant extract was used to strengthen the collagen seated at the dermis layer. The product was formulated to pH 5.5 which is suitable for the skin. The mean droplet size is 10.2 µm with a monomodal distribution pattern which prevents agglomeration. This will decrease Brownian motion, thus prolonging its stability. Long-term acute moisturizing tests show a significant increase of between 24% and 17% hydration for five and six weeks respectively. The efficacy testing on 12 subjects confirmed a reduction in natural fine wrinkles on faces during aging or premature aging at ?7.6%.     

Synthesis of a cyclic peptide containing norlanthionine: effect of the thioether bridge on peptide conformation

Two diastereomeric analogues of ring C of nisin incorporating a novel norlanthionine residue have been synthesized via a triply orthogonal protecting group strategy. A full structural study was carried out by NMR, which elucidated the conformational properties of the two peptides and enabled the identity of each diastereoisomer to be proposed.     

Wurtzite CuGaS2 with an In-Situ-Formed CuO Layer Photocatalyzes CO2 Conversion to Ethylene with High Selectivity

We present surface reconstruction-induced C−C coupling whereby CO₂ is converted into ethylene. The wurtzite phase of CuGaS_2. undergoes in situ surface reconstruction, leading to the formation of a thin CuO layer over the pristine catalyst, which facilitates selective conversion of CO₂ to ethylene (C₂H₄). Upon illumination, the catalyst efficiently converts CO₂ to C₂H₄ with 75.1 % selectivity (92.7 % selectivity in terms of R_electron) and a 20.6 μmol g⁻¹ h⁻¹ evolution rate. Subsequent spectroscopic and microscopic studies supported by theoretical analysis revealed operando-generated Cu²⁺, with the assistance of existing Cu⁺, functioning as an anchor for the generated *CO and thereby facilitating C−C coupling. This study demonstrates strain-induced in situ surface reconstruction leading to heterojunction formation, which finetunes the oxidation state of Cu and modulates the CO₂ reduction reaction pathway to selective formation of ethylene.     

Indium-doped ZnOas efficient photosensitive material for sunlight driven hydrogen generation and DSSC applications: integrated experimental and computational approach

Electricity generation using simple and cheap dye-sensitized solar cells and photocatalytic water splitting to produce future fuel, hydrogen, directly under natural sunlight fascinated the researchers worldwide. Herein, synthesis of indium-doped wurtzite ZnO nanostructures with varying molar percentage of indium from 0.25 to 3.0% with concomitant characterization indicating wurtzite structure is reported. The shift of (002) reflection plane to higher 2θ degree with increase in indium-doping thus is a clear evidence of doping of indium in zinc oxide nanoparticles. Surface morphological as well as microstructural studies of In@ZnO exhibited generation of ZnO nanoparticles and nanoplates of diameter 10–30 nm. The structures have been correlated well using computational density functional (DFT) studies. Diffuse reflectance spectroscopy depicted the extended absorbance of these materials in the visible region. Hence, the photocatalytic activity towards hydrogen generation from water under natural sunlight as well as efficient DSSC fabrication of these newly synthesized materials has been demonstrated. In-doped ZnO exhibited enhanced photocatalytic activity towards hydrogen evolution (2465 μmol/h/g) via water splitting under natural sunlight. DSSC fabricated using 2% In-doped ZnO exhibited an efficiency of 3.46% which is higher than other reported In-doped ZnO based DSSCs.