A Step-Forward Method of Quantitative Analysis of Enzymatically Produced Isomaltooligosaccharide Preparations by AEC-PAD

In this paper, anion exchange chromatography coupled with pulsed amperometric detection has been successfully applied for the fine analysis of isomaltooligosaccharides (IMO) syrups where previous reported methods suffered from a lack of homologue oligosaccharides resolution. These syrups are made of a very complex mixture of glucose oligosaccharides characterized at the same time by their DP value (from 2 to ~15) and linkage types [α-(1–2, 3 or 6) and non-IMO α-(1–4)] and position. A mix of available commercial standards (17 species) was completely separated on a CarboPac PA-100 column at a flow rate of 1 mL min^?1 and with a gradient of sodium acetate in 100 mM sodium hydroxide. The method was validated according to calibration curve, precision, recovery tests, limits of detection and quantitation. Calibration curves presented correlation coefficients greater than 0.98. The analytical method has been applied on real syrups, keeping a high performance separation of structurally close molecules and giving, for six determinations, very low relative SD for the available standard molecules (0.3–5.8%). The accuracy of the proposed method was tested by recovery measurements: first by spiking maltose on three different syrups and then by spiking six different sugar standards (20, 50 and 75% of the initial content) on a single syrup. Good recovery results (respectively, 96.5–99.7 and 97.1–102.7%) were found. The method was found sensible with limits of detection (signal-to-noise ratio of 3) between 0.048 and 0.124 μg mL^?1 and limits of quantification (signal-to-noise ratio of 10) between 0.159 and 0.412 μg mL^?1.     

The first synthesis of 2-amino-1,4-dihydroquinolines

A versatile strategy is described for the synthesis of new 2-amino-1,4-dihydroquinolines. It involved a Knoevenagel condensation of N-protected-2-amino-5-bromobenzaldehyde with ethylcyanoacetate, followed by a cyclization and protection of the NH group to afford the key intermediates 7 or 19. Then various 1,4 addition reactions have been performed to introduce substituents on the upper part of the 2-amino-1,4-dihydroquinolines.     

Phase equilibria of (water + levulinic acid + dibasic esters) ternary systems

Liquid–liquid equilibrium (LLE) data of the solubility (binodal) curves and tie-line end compositions were examined for mixtures of {(water (1) + levulinic acid (2) + dimethyl succinate or dimethyl glutarate or dimethyl adipate (3)} at 298.15 K and 101.3 ± 0.7 kPa. The reliability of the experimental tie-line data was confirmed by using the Othmer–Tobias correlation. The LLE data of the ternary systems were predicted by UNIFAC method. The LLE data were correlated fairly well with UNIQUAC and NRTL models, indicating the reliability of the UNIQUAC and NRTL equations for these ternary systems. The best results were achieved with the NRTL equation, using non-randomness parameter (α = 0.3) for the correlation. Distribution coefficients and separation factors were measured to evaluate the extracting capability of the solvents.     

Chemoenzymatic synthesis of highly enantiomerically enriched secondary alcohols with a thiazolic core

Stereoselective preparative enzymatic acylation and hydrolysis/methanolysis of various C-substituted rac-thiazol-2-yl-methanols were achieved for the preparation of enantiopure or enantiomerically enriched, naturally occurring 2-hydroxymethylthiazoles. The absolute configurations of the resulting secondary alcohols were determined by a detailed ¹H NMR study of Mosher’s derivatives.     

The Molecular-Kinetic Approach to Hydrolysis of Boron Hydrides for Hydrogen Production

Kinetics and Catalysis - In this study, Langmuir–Hinshelwood and Michaelis–Menten kinetic models are applied to describe the kinetic behaviour of the Co–B catalyst in the...     

Synthesis and photophysical properties of some 6,6″-functionalized terpyridine derivatives

The synthesis and photophysical properties of several 6,6″ symmetrically substituted 4′-aryl-2,2′:6′,2″-terpyridine derivatives are reported herein. The UV-Vis spectra in acetonitrile as well as in dichloromethane show two intense bands in the UV areas 252–262 nm and 275–290 nm while the fluorescence emission spectra are only slightly influenced by chemical derivatization.     

A mononuclear, mixed (salicylato) (nicotinamide) complex of Zn(II) with penta- and hexa-coordination sites: a novel framework structure

The title compound, diaqua(bissalicylato-??O)(bisnicotinamide-??N)zinc(II)][bis(triaqua (monosalicylato-??O)(mononicotinamide-??N)zinc(II)salicylate, includes three Zn(II) ions, four nicotinamide ligands, six salicylate ligands and eight coordinated aqua ligands in the asymmetric unit in complex structure. The geometry around one of the Zn(II) ions is a slightly distorted octahedron, of which the equatorial plane is formed by two carboxylate oxygens and two aqua oxygens, while the axial positions are occupied by two pyridyl nitrogen atoms. The other Zn(II) ions adopt fivefold coordinations with one carboxylate oxygen atom from salicylate ligand, one N atom from nicotinamide ligand and three oxygen atoms from aqua ligands. In addition, there are two salicylate anions in the unit cell that are not coordinated. They provide charge balance as counter-ions in the complex framework.