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The recognition and separation of polar chiral compounds are important technological challenges in separation science. Taking full advantage of the intrinsically chiral environment and multiple interactions featured by macrocycles, we designed the first example of porous methylated cyclodextrins-containing polymers (MP-CDPs) with three-dimensional (3D) chiral channels. The enantioselective recognition of (R)/(S)-1-phenylethylamine mixtures was realized with enantiomer excess (e.e.) >73% in only 3 min by using MP-CDPs as the adsorbent. The obtained MP-CDPs also serve as highly efficient liquid chromatographic stationary phases for separation of polar chiral compounds. The stationary phase can separate racemic alcohols and acids successfully. These chiral compounds can be separated within 8 min under normal-phase mode, and the resolution (RS) range from 1.76 to 3.00. Molecular simulations suggest that chiral recognition is a cooperative interaction based on multiple effects such as host-guest interaction, H-bond and size selection. These findings will provide novel chiral stationary phases for recognition and separation of polar chiral compounds in the fields of separation science and pharmaceutical industry.We report on a systematic and comprehensive (0.7 ≤ k ≤ 122) experimental study of the effect of the zone retention factor k on eddy dispersion (heddy) in packed bed columns for liquid chromatography. The values for heddy are obtained by subtracting rigorously estimated contributions to the total plate height from longitudinal diffusion (hB) and the mobile (hCm) and stationary zone (hCs) mass transfer resistances. For the first time, hCm-values are calculated using an expression for the Sherwood number (Sh) that has been established and validated in the relevant velocity range. buy Geneticin Experiments were carried out on both a fully-porous and a core-shell particle column. In both cases, the eddy dispersion systematically decreased with increasing retention factor k, dropping 0.5 to 0.8 reduced plate height units when going from the lowest to the highest k. To establish a simple empirical fitting equation that can represent the observed effects, the widely used power law-based Knox model has been extended to express the dependence of its A- and n-parameters on the retention factor.On-spot fixed-charge derivatization has been suggested for the modification of α-amino acids for their analysis by thin layer chromatography/matrix-assisted laser desorption ionization (TLC/MALDI) mass spectrometry. The approach was based on post-chromatographic treatment of separated analytes by tris(2,6-dimethoxyphenyl)methenium salt and triethylamine. The reaction proceeded smoothly in mild conditions and gave rise to pink-red colored derivatives, containing permanent positive charge. Their MALDI mass spectra, recorded directly from TLC plates, revealed intense peaks corresponding to decarboxylated cationic parts. All derivatives are characterized by high ionization efficiency, which indicates the high sensitivity of the developed method for analyzing amino acids. Applicability of the method to analysis of amino acids was demonstrated on artificial mixtures and dietary supplement.The ultra-trace determination of nicotine and its 4 major metabolites (cotinine, nornicotine, norcotinine and anabasine) from rabbit plasma was achieved by a newly developed solid phase microextraction-liquid chromatography-tandem mass spectrometry method. Extraction of the target analytes was performed with hydrophilic/lipophilic balance-polyacrylonitrile SPME fibers. Dual fiber extraction was necessary to guarantee improved recovery at parts-per-trillion levels. Liquid chromatographic analysis was achieved in a 6-min run using a C18 (1.9 µm C18, 50 mm x 2.1 mm) column with a mobile phase flow rate of 0.4 mL/min. Tandem mass spectrometry was used for detection and quantification in positive electrospray ionization (ESI+) mode for all the targeted analytes. Two stable isotope-labeled internal standards were used for signal correction and accurate quantification. The mass spectrometer with laminar flow ion flux transport, guaranteed improved signal stability, minimal contamination of the ion guide and reproducibility into the first quadrupole analyzer. The method was validated in line with the Food and Drug Administration (FDA) guidelines for bioanalytical method validation. The results met the acceptance criteria as proposed by the FDA accuracy was tested at 0.35, 10 and 75 µg L - 1 and ranged between 98.3-112.2% for nicotine, 94.1-101.9% for cotinine, 94.7-107.0% for nornicotine, 81.1-107.2% for norcotinine and 94.3-115.2% for anabasine, with precision up to 14.2%. Stability tests indicated that all the targeted analytes were stable in the desorption solution for at least 1 week. LOQs ranged from 0.05 to 1 µg L-1. The method was successfully applied to analyze plasma samples obtained from rabbits following transdermal application of a smoking cessation formulation loaded with solid lipid nanoparticles containing a nicotine-stearic acid conjugate.Ferric oxide/carbon (Fe2O3@C) was fabricated via direct carbonization of metal-organic framework of iron (MOF-235) under argon atmosphere. The magnetic Fe2O3 nanoparticles are evenly embedded in porous carbon matrix, while original morphology of MOF-235 was well-maintained. The synthesized Fe2O3@C was used as magnetic sorbent for extracting five benzoylurea insecticides (BUs). The materials exhibited excellent extraction performance, which benefited not only from the strong π-π interaction and hydrophobic interaction (π-conjugated system), but also to the abundant adsorption sites and flexible transport channel (the interconnected 3D porous structure). A three-factor-three-level Box-Behnken design (BBD) was selected to optimize three greatly influential parameters amount of adsorbent (A), desorption time (B) and volume of desorption solvent (C) by response surface methodology. The established method coupled to HPLC-UV detection showed wide linearity with the range of 0.2-450 μg•L-1, relatively low limits of detection (0.05-0.10 μg•L-1) with the relative standard deviation (RSD) (n = 7) lower t than 5.47%. Moreover, the proposed method was successfully applied to analyze BUs in tea samples and investigate the removal effect of different washing on BUs residues from tea leaf. These results indicated that the synthesized Fe2O3@C is a promising adsorbent material for magnetic solid phase extraction of BUs at trace concentrations from tea samples.