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Excellent Resolution (excellent + resolution)
Selected AbstractsSESAME-HSQC for simultaneous measurement of NH and CH scalar and residual dipolar couplings,MAGNETIC RESONANCE IN CHEMISTRY, Issue 4 2007Peter Würtz Abstract We present a novel pulse sequence, SESAME-HSQC, for the simultaneous measurement of several NH and CH scalar and residual dipolar couplings in double labeled proteins. The proposed Spin-statE Selective All Multiplicity Edited (SESAME)-HSQC combines gradient selected and sensitivity enhanced 15N- and constant-time 13C-HSQC experiments with the recently introduced spin-state selective method (Nolis et al., J. Magn. Reson. 180 (2006) 39,50) for measuring couplings simultaneously at amide and aliphatic regions. Excellent resolution and high sensitivity is warranted by removing all coupling interactions during the indirectly detected t1 period, and by employing pulsed field gradients for coherence selection and utilizing coherence order selective spin-state selection. The scalar and residual dipolar couplings can be readily measured from a two-dimensional 15N/13C-HSQC spectrum without additional spectral crowding. SESAME-HSQC can be used for epitope mapping by observing chemical shift changes in both amide and aliphatic regions. Simultaneously, potential conversion in protein conformation can be probed by analyzing changes in residual dipolar couplings induced by ligand binding. The pulse sequence is experimentally verified with a sample of 15N/13C enriched human ubiquitin. The internuclear vector directions determined from the residual dipolar couplings are found to be in excellent correlation with those predicted from ubiquitin's refined solution structure. Copyright © 2007 John Wiley & Sons, Ltd. [source] Intracardiac Echocardiography in Patients with Pacing and Defibrillating Leads: A Feasibility StudyECHOCARDIOGRAPHY, Issue 6 2008Maria Grazia Bongiorni M.D. Background: Lead extraction, an important and necessary component of treatment for many common device and lead-related complications, is a procedure that can provoke much anxiety in even the most experienced operators given the potentially serious complications. The principal impediment to lead extraction is the body's response to an intravascular foreign body with matrix intravascular neoformation, which causes the lead to adhere to the endocardium or vascular structure, increasing the risk of vascular or myocardial damage with lead removal. Fluoroscopic visualization, the commonly visualization used tool, has several limits in terms of anatomical structures visualization. The aim of this study was to assess the safety and feasibility of intracardiac echocardiography (ICE) in patients undergoing pacing and defibrillating leads before and during a transvenous device removal, and its potential role in detecting intracardiac leads and areas of fibrous adherence. Methods: ICE interrogation was performed in 25 consecutive patients with pacing and defibrillating implantable cardioverter defibrillators (ICD) leads before and during device removal. Results: A programmed ICE analysis was completed in 23 out of 25 patients with excellent resolution, providing a "qualitative-quantitative" information on anatomical structures, cardiac leads, and related areas of fibrous adherence. No ICE-related complications occurred. Conclusions: ICE evaluation is safe and feasible in patients with pacing and defibrillating leads before and during transvenous lead removal, offering an excellent visualization of cardiac leads and related areas of adherence. ICE can assist pacing and ICD lead removal and could improve procedure efficacy and safety. [source] The effect of co-surfactant-modified micelles on chiral separations in EKCELECTROPHORESIS, Issue 16 2009Adeline B. Kojtari Abstract The use of chiral pseudostationary phases in EKC provides high efficiencies and excellent resolution for enantiomeric separations. The chiral pseudostationary phases of interest in this study are alcohol-modified ("swollen") micelles, in which a co-surfactant (medium chain-length alcohol) is added with the surfactant. In this study, the chiral surfactant, dodecoxycarbonylvaline (DDCV), along with the co-surfactant, 2-hexanol, has been prepared as swollen micelle in order to investigate the chiral separation of enantiomeric pairs. Three sets of experiments were investigated in which swollen micelle systems contained: chiral surfactant and racemic co-surfactant; chiral surfactant and chiral co-surfactant; and phase ratio increases, in which both chiral surfactant and chiral co-surfactant were employed. In the first two sets of experiments, co-surfactant concentration was held constant and the surfactant concentration was increased. In the third set of experiments, both surfactant and chiral surfactant concentrations were increased proportionally. The chromatographic figures of merit for each enantiomeric pair were investigated and compared with various chiral aggregate systems. In swollen micelle compositions using constant racemic 2-hexanol concentration, when DDCV concentration increased, enantioselectivity and resolution increased; whereas, efficiency remained constant for most of the test compounds. Compositions using constant S -2-hexanol concentration reached a maximum in all chromatographic figures of merit when DDCV concentration was increased from 2 to 3%. An increase in both surfactant and co-surfactant concentrations led to noisy baselines and chiral aggregates that were generally unstable in solution. [source] The use of peepers to sample pore water in acid sulphate soilsEUROPEAN JOURNAL OF SOIL SCIENCE, Issue 4 2008P. VanOploo Summary Serious environmental impacts of acidic drainage from acid sulphate soils in coastal areas are the result of the interactions between the hydrologic cycle, land use and drainage management, and pore water chemistry. In this study, in situ, diffusion-controlled dialysis profile samplers, or peepers, were used to examine pore water chemistry of acid sulphate soils in a coastal, sugarcane-producing area in Eastern Australia. The peepers sampled pore water at 20-mm intervals over a 1.0-m length, permitting excellent resolution of the sharp transitions in pore water chemistry that occur around a soil profile's iron sulphide oxidation front. Comparison of peeper profiles with soil water profiles extracted from soil samples by centrifuging, illustrated the advantages of peepers over conventional soil water sampling techniques in unconsolidated, sulphidic soils. For conventional sampling, the low permeability, gel-like, unoxidized soil samples had to be frozen then thawed before water could be extracted by centrifuging. Peeper profiles of species not involved in redox reactions agreed well with those from centrifuged soil extracts. Redox sensitive species, however, were in poorer agreement because of the lengthy soil sample preparation and extraction procedures required for extraction by centrifuging. The approximately 6-day equilibration time required for peeper sampling allows them to follow monthly or seasonal changes in pore water chemistry in acid sulphate soils due to variations in climate, and land use and management. [source] Methacrylate ester-based monolithic columns for nano-LC separation of tocopherols in vegetable oilsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 17-18 2010María Jesús Lerma-García Abstract The separation and determination of tocopherols (Ts) in vegetable oils by nano-LC chromatography with UV,vis detection using lauryl methacrylate ester-based monolithic columns has been developed. The separation of Ts was optimized in terms of mobile phase composition on the basis of the best compromise among efficiency, resolution and analysis time. Using a mobile phase composed of ACN/methanol/water, an excellent resolution between Ts was achieved within 18,min. The LODs were lower than 0.26,,g/mL, being repeatability values of retention time and peak area below 0.15 and 3.1%, respectively. The method was applied to the quantification of Ts and tocotrienols present in several vegetable oils from different botanical origins. [source] A review of the background, operating parameters and applications of microemulsion liquid chromatography (MELC)JOURNAL OF SEPARATION SCIENCE, JSS, Issue 15 2005A. Marsh Abstract Microemulsions are dispersions of nanometre-sized droplets of an immiscible liquid within another liquid. Droplet formation is facilitated by the addition of surfactants and often also cosurfactants. Microemulsions are classified as either oil-in-water (O/W) (oil droplets such as octane dispersed throughout aqueous buffer) or water-in-oil (W/O) (aqueous droplets in oil such as hexane). Both microemulsion types have been used as mobile phases for separation in microemulsion HPLC (MELC). There has been a recent increase of interest in this area with new applications and developments such as gradient elution and optimisation of methods using experimental design. O/W microemulsions have been employed as eluents for RP-HPLC while W/O microemulsions have been used for normal phase chromatography. Separations can have superior speed and efficiency to conventional HPLC modes while offering a unique selectivity with excellent resolution. The capability for quantitative and stability-indicating analysis has also been demonstrated. Specific advantages include the ability to operate at low UV wavelengths and elimination of the need for an equilibration rinse between gradients. Operational issues associated with the use of MELC have been identified including the need to add salt to the gradient eluent, relatively high back-pressures and increased need for equipment cleaning compared to conventional RP eluent. This report details the different microemulsion types and compositions used and their reported applications. The use of gradient and isocratic elution is described. The effects on separations of varying operating parameters such as temperature, oil type and concentration, surfactant type and concentration, sample solvent, column type, and organic solvent addition will be discussed and illustrated. [source] Efficient low-power heteronuclear decoupling in 13C high-resolution solid-state NMR under fast magic angle spinningMAGNETIC RESONANCE IN CHEMISTRY, Issue S1 2007Mrignayani Kotecha Abstract The use of a low-power two-pulse phase modulation (TPPM) sequence is proposed for efficient 1H radio frequency (rf) decoupling in high-resolution 13C solid-state NMR (SSNMR) under fast MAS conditions. Decoupling efficiency for different low-power decoupling sequences such as continuous-wave (cw), TPPM, XiX, and ,-pulse (PIPS) train decoupling has been investigated at a spinning speed of 40 kHz for 13C CPMAS spectra of uniformly 13C - and 15N -labeled L -alanine. It was found that the TPPM decoupling sequence, which was originally designed for high-power decoupling, provides the best decoupling efficiency at low power among all the low-power decoupling sequences examined here. Optimum performance of the low-power TPPM sequence was found to be obtained at a decoupling field intensity (,1) of ,,R/4 with a pulse flip angle of ,, and a phase alternation between ± ,(, = ,20° ), where ,R/2, is the spinning speed. The sensitivity obtained for 13CO2,, 13CH, and 13CH3 in L -alanine under low-power TPPM at ,1/2, of 10 kHz was only 5,15% less than that under high-power TPPM at ,1/2, of 200 kHz, despite the fact that only 0.25% of the rf power was required in low-power TPPM. Analysis of the 13CH2 signals for uniformly 13C- and 15N-labeled L -isoleucine under various low-power decoupling sequences also confirmed superior performance of the low-power TPPM sequence, although the intensity obtained by low-power TPPM was 61% of that obtained by high-power TPPM. 13C CPMAS spectra of 13C -labeled ubiquitin micro crystals obtained by low-power TPPM demonstrates that the low-power TPPM sequence is a practical option that provides excellent resolution and sensitivity in 13C SSNMR for hydrated proteins. Copyright © 2007 John Wiley & Sons, Ltd. [source] Direct analysis of pharmaceutical compounds in human plasma with chromatographic resolution using an alkyl-bonded silica rod columnRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 12 2001Robert Plumb Monolithic columns have been successfully used with steep gradient and high flow rates for the direct analysis of a candidate pharmaceutical compound in human plasma. The monolithic columns showed excellent robustness with nearly 300 20-µL injections of plasma (diluted 1:1 with water) being made onto one column without significant deterioration in performance. The system gave excellent sensitivity with a limit of quantification of 5,ng/mL being achieved. Unlike previous methods of direct analysis the monolithic columns showed excellent resolution even after nearly 300 plasma injections. The column performance was measured before and after the analysis of the plasma samples. Copyright © 2001 John Wiley & Sons, Ltd. [source] | ||||||||||