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Peak Resolution (peak + resolution)
Selected AbstractsOrganic solvents in CEELECTROPHORESIS, Issue S1 2009Ernst Kenndler Abstract In this contribution some fundamental aspects are discussed serving for a critical reflection and elucidation of the role of organic solvents in CE. The implications of the solvent on the parameters governing peak resolution are discussed based on the concepts describing migration and zone broadening in capillary zone electrophoresis. This discussion includes the solvent-dependent influence of the ionic strength on the mobility. The role of the solvent on the plate number in case of the inevitable diffusional peak dispersion is outlined, and its effect on other peak broadening contributions is briefly examined. This paper also deals with the problems of conductance, applicable voltage and analysis time upon application of organic solvents, and tries to clarify some misunderstandings common in the literature. [source] Urtica dioica agglutinin: Separation, identification, and quantitation of individual isolectins by capillary electrophoresis and capillary electrophoresis,mass spectrometryELECTROPHORESIS, Issue 9 2005Markus Ganzera Abstract With benign prostatic hyperplasia (BPH) being a major health problem in ageing men, alternative therapeutic approaches (e.g., with phytopharmaceuticals) are of great interest. Based on pharmacological evidences, one of the most promising options in that respect are the lectins found in Urtica dioica (stinging nettle) roots. In this study the qualitative and quantitative analysis of individual isolectins in U. dioica extracts is described, which is the first report on using capillary electrophoresis (CE) for the analysis of lectins in plant material at all. By utilizing a 200 mM sodium acetate buffer (pH 3.75) a baseline separation and determination of four closely related isolectins was feasible within 20 min in the aqueous plant extracts. The individual compounds were identified based on reference compounds as well as data obtained from CE-mass spectrometry (MS) experiments. After modifying the optimized CE conditions to 100 mM ammonium formate buffer with pH 3.75 and a voltage of 15 kV, the isolectins were clearly assignable in positive electrospray ionization (ESI) mode. The quantitative results obtained by CE (the total lectin content varied from 0 to 0.42% in the samples) were accurate (recovery rates of spiked samples between 92.5 and 96.2%), precise (relative standard deviation < 5%) and in good agreement to those obtained by High-performance liquid chromatography (HPLC). As for peak resolution, assignable compounds and required separation time the newly developed CE method was clearly advantageous over the determination achieved by LC. [source] Evaluation of use of a very short polar microbore column segment in high-speed gas chromatography analysisJOURNAL OF SEPARATION SCIENCE, JSS, Issue 14 2008Peter Quinto Tranchida Abstract Very fast GC analyses are commonly carried out by using 10 m×0.1 mm id capillaries. In order to achieve rapid elution times (1,3 min), the latter are operated under suboptimum conditions. The present research is focused on the evaluation of use of a 0.1 mm id polar column segment (2 m), operated under near-to-optimum conditions, in very fast GC analysis. The results attained are compared with those derived from using a 10 m microbore column in very fast GC experiments. Prior to method development, the effects of gas velocity, temperature program rate, and sample amounts on analytical performance were evaluated. Following these preliminary applications, a complex lipidic sample, cod liver oil, was subjected to rapid separation (,2.1 min) on the 10 m capillary through the application of a 50°C/min temperature rate and a 130 cm/s gas velocity. The same matrix was analyzed on the 2 m capillary using the same temperature program rate and range, but with a close-to-ideal linear velocity. The results observed were of interest, as the separation was achieved in less time (1.45 min) with improved peak resolution. Finally, both methods were validated in terms of retention time and peak area repeatability, LOQ, and linearity. [source] Microstructure and Molecular Interaction in Glycerol Plasticized Chitosan/Poly(vinyl alcohol) Blending FilmsMACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 10 2009Songmiao Liang Abstract Exploring some basic interactions in blending systems is of great significance for designing a blend with controlled structure and properties. This work attempts to analyze microstructure and molecular interaction in glycerol plasticized chitosan/poly(vinyl alcohol) blends by atomic force microscopy, differential scanning calorimetry and ATR-FTIR spectroscopy. Our results show that the blending films are aggregated by spherical chitosan/poly(vinyl alcohol) blending nanoparticles. The size and aggregation behavior of these particles are closely related to glycerol content. The presence of glycerol gives rise to a continuous closing in Tg of poly(vinyl alcohol) and chitosan components, suggesting an improved miscibility of the blend. Strong hydrogen bonding interaction in the blend is observed and further distinguished by peak resolution. Moreover, more interesting evidence on the effect of glycerol in the blends is provided by monitoring the structure evolution of the blend at different blending steps using atomic force microscopy. The formation of strong hydrogen bonding network among glycerol molecules and polymer matrix was considered as the main driving force to result in the changes in the microstructure and miscibility of the blend. [source] Cell-free expression and selective isotope labelling in protein NMRMAGNETIC RESONANCE IN CHEMISTRY, Issue S1 2006David Staunton Abstract Isotope labelling is a very powerful tool in NMR studies of proteins and has been employed in various ways for over 40 years. 15N and 13C incorporation, using recombinant expression systems, is now commonplace because heteronuclear experiments assist with the fundamental problems of peak resolution and assignment. The use of selective labelling for peak assignment has been restricted by the scrambling of isotope label through metabolic pathways within the expression host organism. The availability of efficient cell-free expression systems with low levels of metabolic conversion allow the increasing use of selective isotope labelling as a tool in protein NMR. We describe two examples, one where a selective labelling scheme can identify backbone amide peaks from unassigned 1H15N HSQC and HNCO spectra of a 84 residue protein, and another where a specific backbone amide in a 198 residue construct of the ninth and tenth Type III repeats from human fibronectin can be labelled and rapidly identified using a simple HSQC experiment. Copyright © 2006 John Wiley & Sons, Ltd. [source] The design of a multi-dimensional LC-SPE-NMR system (LC2 -SPE-NMR) for complex mixture analysis,MAGNETIC RESONANCE IN CHEMISTRY, Issue 1 2006A. J. Alexander Abstract In this communication, we describe the design of an online multi-chromatographic approach to the routine NMR analyses of low-level components (,0.1%) in complex mixtures. The technique, termed LC2 -SPE-NMR, optimally combines multi-dimensional liquid chromatography with SPE technology for isolating, enriching and delivering trace analytes to the NMR probe. The fully automated LC2 -SPE-NMR system allows for maximal loading capacity (in the first, preparative LC dimension), close to optimal peak resolution (in the second, analytical LC dimension) and enhanced sample concentration (through SPE). Using this system, it is feasible to conveniently conduct a wide range of NMR experiments on, for example, drug impurities at the low microgram per milliliter level, even for components poorly resolved in the first dimension. Such a sensitivity gain significantly elevates the analytical power of online NMR technology in terms of the level at which substances of pharmaceutical significance can be structurally characterized. Copyright © 2006 John Wiley & Sons, Ltd. [source] Sample preparation effects in matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry of partially depolymerised methyl celluloseRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 11 2003Dane Momcilovic Methyl cellulose (MC) was partially depolymerised and the oligomers thus obtained were studied by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOFMS). The depolymerisation was either enzymatic or acidic. Fractions of enzymatically depolymerised MC were collected from size-exclusion chromatography and subjected to a sample preparation investigation. Several MALDI matrices and solvents were evaluated. The results showed that the solvent choice had a significant effect on the measured degree of substitution (DS). Aprotic solvents produced higher DS values, which was most likely due to poor solubility of species with low DS. The obtained signal intensity, however, did not correlate with the solubility but seemed to be more dependent on certain matrix/solvent combinations. All the matrices attempted produced mass spectra with sufficient signal intensity for accurate peak area calculation. The choice of matrix did not have any significant effect on the measured DS. Sample spots obtained from organic solvents had a more homogeneous distribution of the analyte and smaller crystals than those obtained from water. This increased both the reproducibility and peak resolution and in addition the analysis time was shorter. DS measurements were performed on two acidically depolymerised MCs with different nominal DS values. It was easy to distinguish between the two MCs, and the measured DS values agreed well with the values supplied by the manufacturers. Copyright © 2003 John Wiley & Sons, Ltd. [source] | ||||||||||