Mccullochrivers5402

The solvent mixtures that were eligible for practical application in these respects were used to construct a screening sequence, including identical compositions combined with different column pretreatment. The gain achievable by using the proposed sequence was then evaluated using 15 enantiomer pairs with focus on resolution, enantiomer elution order and chemoselectivity.A fast, non-invasive, high-performance liquid chromatographic screening method with electrospray ionization mass spectrometric detection was developed for the analysis of three major glycine-conjugated bile acids in human saliva. Using a mobile phase composed of 80% methanol and 0.1% formic acid, glycocholic, glycodeoxycholic, and glycochenodeoxycholic acids were separated in less than 4 minutes with sensitivity in the low nM range. Bile acids are thought to contribute to the pathology of various complications in gastroesophageal reflux disease, for instance, Barrett's esophagus, which may eventually lead to esophageal carcinoma. In this pilot study, samples of saliva obtained from 15 patients with Barrett's esophagus of various severities were compared to saliva samples from 10 healthy volunteers. Glycochenodeoxycholic acid was significantly elevated in the patients and principal component analysis of all bile acids could distinguish the most severe Barrett's esophagus patients. selleck products We also reported on the detection of glycochenodeoxycholic acid in exhaled breath condensate for the first time. The promising results of this pilot study warrant future investigation, aiming at non-invasive diagnostics of Barrett's esophagus susceptibility in patients with gastroesophageal reflux disease.The influence of impregnation the chromatographic plate adsorbent layer, silica, with hen's egg white albumin (OVA) or bovine serum albumin (BSA) on the retention of some popular medicines (paracetamol, aminophenazone, theophylline, caffeine, acetanilide, ciprofloxacin, tramadol, acetylsalicylic acid, acebutolol) is investigated. The effect of composition and buffer pH of the mobile phase on solute separation selectivity is also studied. The chromatographic systems with and without above mentioned albumins and their influence on investigated drug retention are compared. In general, it has been turned out that retention of tested medicines in systems with the sorbent impregnated with albumin significantly increase relative to those with non-impregnated.The monodisperse pillar[5]arene-based polymeric sub-microsphere was prepared by polycondensation of hydroxylated pillar[5]arene and cyanuric chloride through a one-pot reaction in mild condition. The preparation was realized by a simple two-step temperature-programmed process without heating operation. The obtained polymeric sub-microsphere exhibited monodisperse and regular spherical structure with uniform particle size distribution of 220-320 nm accounting for 94%. The prominent adsorption capacity of the polymeric sub-microsphere for antioxidants was demonstrated and attributed to the synergistic effect of the cladding interaction with the π-electron rich cavity and hydrophilic interaction with terminal hydroxyl on pillar[5]arene. Then the pillar[5]arene sub-microsphere was packed into a micro-column to realize effective on-line enrichment of antioxidants coupling with high-performance liquid chromatography (HPLC). The flow rate of extraction and desorption solvent, clean-up and desorption volume were assessed to optimize the method. The method showed wide linear ranges with R2 greater than 0.9926, low limits of detection (0.030-0.20 μg/L) and limits of quantification (0.10-0.67 μg/L). The developed method was successfully applied to determine trace antioxidants in the migration of food contact materials with simulated solution, which demonstrated the promising potential of this method for practical analysis. Furthermore, the migration behavior of antioxidants from food packaging materials into different food matrix was also investigated.Efficient extraction of polar sulfonamides antibiotics from aqueous samples and food is very challenging, because they are hydrophilic, their concentration is very low, and the matrix is complex. Covalent organic frameworks (COFs), a novel porous organic material, have attracted great attention. In this work, the spherical triphenylbenzene-dimethoxyterephthaldehyde-COFs (TPB-DMTP-COFs) were synthesized by a simple room temperature method, and due to their attractive properties, such as high outstanding acid-base stability, large specific surface area, low skeletal density, inherent porosity and high crystallinity, so TPB-DMTP-COFs as ideal solid phase extraction adsorbents showed excellent adsorption performance for trace polar sulfonamides in food and water. TPB-DMTP-COFs were characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, powder X-ray diffraction, and so on. The important parameters were optimized to improve the extraction efficiency of TPB-DMTP-COFs toward sulfonamides. Analysis of sulfonamides was performed by liquid chromatography-tandem mass spectrometry. The developed method based on TPB-DMTP-COFs material achieved low limits of detection (0.5-1.0 ng L-1), wide linearity (5-1000 ng L-1), and good repeatability (2.5%-8.7%). The possible extraction mechanism was also discussed. Finally, the method was successfully applied to the enrichment and detection of sulfonamides in environmental water samples and food samples. The present study indicated that TPB-DMTP-COFs had splendid prospects in highly sensitive analysis of other pollutants in complex matrix.An ultra-high-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC-QTOF/MS) method was employed for chemical identification in a commercial polyvinyl chloride/polyethylene (PVC/PE) multilayer film. Over 30 chemicals from different layers (PE layer, PVC layer, and adhesive layer) of the film were identified and were classified into 6 groups, including antioxidants, plasticizers, slip agents, antistatic agents, adhesive components, etc. Special attention was placed on the analysis of some non-intentionally added substances and oligomers in adhesive. Based on the identification results, six additives (all from PE layer) were selected and their migration behaviors were investigated via one-sided contact migration test. The migration test was performed by exposing the PE side of the film to different simulating solutions (water, 40% ethanol, and 95% ethanol) at 40°C, as well as recording the migration level as a function of time. No obvious migration was found into water for all additives, while the migration into 40% and 95% ethanol followed Fickian diffusion behavior, and could be described by Fick's diffusion equation.