The effect of solvent on the crystal structure and size distribution of cadmium sulfide nanocrystals

CdS nanocrystals with different structures were synthesized by the method of solution precipitation using thiourea and cadmium acetate as starting materials in different solvents: water, methanol and N,N-dimethylformamide (DMF). Our results show that the solvent has direct effect on the structure and size of the final nanoparticles. It was found that using DMF, as a solvent, results in producing smaller nanoparticles with the cubic structures, while using the other solvents gives rise to larger nanoparticles with the hexagonal structure. It was also found that using heat during washing the precipitate results in a more homogenous size distribution of CdS nanocrystals. On the basis of our experimental results we also suggest a critical structure transformation size.     

Fluorimetric Determination of Histamine in Fish Using Micellar Media and Fluorescamine as Labelling Reagent

An analytical method based on the use of fluorescamine to produce a fluorescent derivative with histamine and combined with micellar-enhanced fluorescence detection of the formed complex is developed for the sensitive and rapid determination of histamine in fishes. The fluorescence properties of the obtained complex in water and micellar solutions of sodium dodecyl sulfate (SDS), cetyltrimethylammonium chloride (CTAC) and brij-700 are reported. Physicochemical variables influencing the sensitivity of the method (pH, micellar, fluorescamine and NaCl relative concentrations) have been optimized. The stability of the formed complex, as shown by kinetic study, depends on the pH of the solution. Linear calibration curves allowing an effective histamine determination were established with large linear dynamic range (LDR), and low limits of detection (LOD) between 0.5 and 33 ng mL⁻¹, according to the solvent. Application to the analysis of fish samples (sardines) yielded satisfactory results. The method seems to be suitable for environmental fish quality control. Presented in part, at the 39th IUPAC Congress and the 86th Conference of the Canadian Society for Chemistry, August, 10–15, 2003, Ottawa (Canada).     

Fragmentation energetics of the phenol(+)···Ar(3) cation cluster

The various dissociation thresholds of phenol(+)···Ar(3) complexes for the consecutive loss of all three Ar ligands were measured in a molecular beam using resonant photoionization efficiency and mass analyzed threshold ionization spectroscopy via excitation of the first excited singlet state (S(1)). The adiabatic ionization energy is derived as 68077 ± 15 cm(-1). The analysis of the dissociation thresholds demonstrate that all three Ar ligands in the neutral phenol···Ar(3) tetramer are attached to the aromatic ring via π-bonding, denoted phenol···Ar(3)(3π). The value of the dissociation threshold for the loss of one Ar ligand from phenol(+)···Ar(3)(3π), ～190 cm(-1), is significantly lower than the binding energy measured for the π-bonded Ar ligand in the phenol(+)···Ar(π) dimer, D(0) = 535 ± 3 cm(-1). This difference is rationalized by an ionization-induced π → H isomerization process occurring prior to dissociation, that is, one Ar atom in phenol(+)···Ar(3)(3π) moves to the OH binding site, leading to a structure with one H-bonded and 2 π-bonded ligands, denoted phenol(+)···Ar(3)(H/2π). The dissociation thresholds for the loss of two and three Ar atoms are also reported as 860 and 1730 cm(-1). From these values, the binding energy of the H-bound Ar atom can be estimated as 870 cm(-1).     

Asymmetric Cycloaddition: An Efficient Synthesis of Enantiopure Isoxazolines Substituted with Carbohydrate Analogues

A simple and convenient method for the synthesis of heterocycles substituted with carbohydrate analogs is described. The chiral optically pure five‐membered glycoconjugates containing the isoxazoline unit were obtained by an aromatic nitrile oxides cycloaddition with 1‐phenyl‐1,2‐dihydro‐pyridazine‐3,6‐dionyl N‐glycoside derivatives.     

New Analytical Method using Coupled Enzymes for Determination of Polyunsaturated Fatty Acid Content in Olive Oil

A new, simple, and original method is described for specific measurement of polyunsaturated fatty acid content in olive oil. This analytical system uses coupled enzymes, lipase and lipoxygenase. The system consists of lipase-catalyzed hydrolysis of triacylglycerol and subsequent lipoxygenation of liberated polyunsaturated fatty acids. The hydroperoxy-fatty acids formed were easily monitored by spectrophotometry at 234 nm. After being optimized, the method was validated in terms of linearity, precision sensitivity, and recovery. Linear calibration graph was obtained in the range 50–500 µg mL^?1, with a correlation coefficient higher than 0.921 and a detection limit (S/N?=?3) of 15 µg mL^?1. The precision of the method (relative standard deviation) for within and between days is better than 7% and 12%, respectively. The proposed method was successfully applied to the estimation of polyunsaturated fatty acids level in olive oil samples and results obtained were in excellent agreement with those obtained by the classical official method. The proposed method is accurate, simple, cheap, and can be satisfactorily used for routine analysis of edible oils.     

Transformations de N-acylaziridines catalysées par des supports à base de silice et d’alumine : une élucidation mécanistique

The silica gel, neutral alumina and acid activated clays transform the N-acyl-2,2-dimethylaziridines 1 into a mixture of N-methallylamides 2, oxazolines 3 and amidoalcohols 4. The reaction of N-benzoyl-2,2-dimethylaziridine with benzylcyanid anion leads to a mixture of amidopyrroline 5 and iminopyrrolidine 6. The product 5 was converted into its tautomer 6 by chromatogaphy on silica gel. Ionic mechanisms were then proposed to explain the formation of products 2–6 resulting from the regioselective ring opening on the more substituted C2 carbon side.     

Two Optimal General Classes of Iterative Methods with Eighth-Order

Two new three-step classes of optimal iterative methods to approximate simple roots of nonlinear equations, satisfying the Kung-Traub’s conjecture, are designed. The development of the methods and their convergence analysis are provided joint with a generalization of both processes. In order to check the goodness of the theoretical results, some concrete methods are extracted and numerical and dynamically compared with some known methods.     

On the Symmetric H q -Semiclassical Polynomial Sequences of Even Class. Some Examples from the Class Two

In the present work, we deal with the quadratic decomposition of symmetric H _q -semiclassical polynomial sequences of even class. Some examples from class two are settled. We give an integral and discrete measure representations for each of considered symmetric forms.     

Synthesis and evaluation of new phosphonated δ-lactam and glutarimide derivatives as angiotensin converting enzyme inhibitors

An efficient synthesis of new γ,δ-insaturated δ-lactam and glutarimide derivatives bearing a phosphonomethyl group from a common allylphosphonate precursor is described. Our approach is based on a two-step procedure involving the preparation of phosphonated-1,5-ketoester and −1,5-diester followed by an amidation–heterocyclization sequence. The first step proceeds via Michael's addition of ethyl acetoacetate and diethyl malonate on an allylphosphonate starting material. The second step consists of a base-promoted intramolecular amidation-cyclization sequence with primary amines, which accounts for the construction of δ-lactams and glutarimide skeletons. We performed the evaluation of angiotensin I-converting enzyme (ACE) inhibition using an in vitro enzyme assay on six new compounds. Five compounds showed potent ACE inhibitory activity, with IC₅₀ values ranging from 0.02 to 0.27 mg/ml. Compared with Captopril, used as a reference drug, two new glutarimide derivatives exhibited higher efficiency ACE inhibition activity.