Chiral Capillary Electrokinetic Chromatography: Principle and Applications, Detection and Identification, Design of Experiment, and Exploration of Chiral Recognition Using Molecular Modeling

This work reviews the literature of chiral capillary electrokinetic chromatography from January 2016 to March 2021. This is done to explore the state-of-the-art approach and recent developments carried out in this field. The separation principle of the technique is described and supported with simple graphical illustrations, showing migration under normal and reversed polarity modes of the separation voltage. The most relevant applications of the technique for enantioseparation of drugs and other enantiomeric molecules in different fields using chiral selectors in single, dual, or multiple systems are highlighted. Measures to improve the detection sensitivity of chiral capillary electrokinetic chromatography with UV detector are discussed, and the alternative aspects are explored, besides special emphases to hyphenation compatibility to mass spectrometry. Partial filling and counter migration techniques are described. Indirect identification of the separated enantiomers and the determination of enantiomeric migration order are mentioned. The application of Quality by Design principles to facilitate method development, optimization, and validation is presented. The elucidation and explanation of chiral recognition in molecular bases are discussed with special focus on the role of molecular modeling

Spherical-shaped Y2O3:Eu3+ nanoparticles with intense photoluminescence emission

Herein we report on the crystallized nanoparticles based on Eu3+-doped Y2O3 with 5 mol% using citric acid as precursor. The heating temperatures were evaluated in order to obtain the best crystallized nanoparticles with size around 12 nm and with highest red intense photoluminescence emission. Nanocrystallite size was calculated by Scherrer's equation based on diffractogram of the material heated at 750 degrees C for 4 h, obtaining size around 8 nm. The low photoluminescence intense emissions were attributed to the presence of quenchers remaining from precursors used in the synthesis. In general the photoluminescence properties were evaluated based on emission and excitation spectra profile. Rietveld refinement was performed based on the diffractogram of the material annealed at 750 degrees C for 4 h, and the visualization of the cubic structure was obtained. The centered cubic crystalline structure of Y2O3 was obtained and the photoluminescence properties of Eu3+ ion in Y2O3 host lattice was verified as being dependent on the temperature of heating and C-2 and S-6 site of symmetry present in the cubic structure. CIE chromaticity diagram was obtained with x and y being 0.682 and 0.316, respectively, for material with the highest relative photoluminescence intensity. (C) 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

Theoretical and experimental study of inclusion complexes formed by isoniazid and modified β-Cyclodextrins: 1H NMR structural determination and antibacterial activity evaluation

Me-β-cyclodextrin (Me-βCD) and HP-β-cyclodextrin (HP-βCD) inclusion complexes with isoniazid (INH) were prepared with the aim of modulating the physicochemical and biopharmaceutical properties of the guest molecule, a well-known antibuberculosis drug. The architectures of the complexes were initially proposed according to NMR data Job plot and ROESY followed by density functional theory (DFT) calculations of (1)H NMR spectra using the PBE1PBE functional and 6-31G(d,p) basis set, including the water solvent effect with the polarizable continuum model (PCM), for various inclusion modes, providing support for the experimental proposal. An analysis of the (1)H NMR chemical shift values for the isoniazid (H6',8' and H5',9') and cyclodextrins (H3,5) C(1)H hydrogens, which are known to be very adequately described by the DFT methodology, revealed them to be extremely useful, promptly confirming the inclusion complex formation. An included mode which describes Me-βCD partially enclosing the hydrazide group of the INH is predicted as the most favorable supramolecular structure that can be used to explain the physicochemical properties of the encapsulated drug. Antibacterial activity was also evaluated, and the results indicated the inclusion complexes are a potential strategy for tuberculosis treatment