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Selected AbstractsFast multidimensional localized parallel NMR spectroscopy for the analysis of samplesMAGNETIC RESONANCE IN CHEMISTRY, Issue 10 2010Marino Vega-Vazquez Abstract A parallel localized spectroscopy (PALSY) method is presented to speed up the acquisition of multidimensional NMR (nD) spectra. The sample is virtually divided into a discrete number of nonoverlapping slices that relax independently during consecutive scans of the experiment, affording a substantial reduction in the interscan relaxation delay and the total experiment time. PALSY was tested for the acquisition of three experiments 2D COSY, 2D DQF-COSY and 2D TQF-COSY in parallel, affording a time-saving factor of 3,4. Some unique advantages are that the achievable resolution in any dimension is not compromised in any way: it uses conventional NMR data processing, it is not prone to generate spectral artifacts, and once calibrated, it can be used routinely with these and other combinations of NMR spectra. Copyright © 2010 John Wiley & Sons, Ltd. [source] Toward multipurpose NMR experimentsMAGNETIC RESONANCE IN CHEMISTRY, Issue 1 2010Judith Schlagnitweit Abstract Standard phase cycled NMR pulse sequences were generalized such that for each individual step of the pulse phase cycle the free induction decay is stored separately without phase correction. This is in contrast to the usual practice, where pulse responses are phase shifted immediately (by applying a ,receiver phase') and co-added as they are stored. The approach used here allows one to extract different types of NMR information, which are usually referred to as different ,experiments', from the same raw data set a posteriori by using complex linear combinations. Storing the free induction decays of individual phase cycle steps separately and using specific linear combinations of these data to obtain a particular type of information increase the overall efficiency of a given set of NMR experiments substantially, because all information can be derived from a single multiplexed data set. This ,super-experiment' requires only as much time as the most complex of the derived specific experiments alone. The principle of this multipurpose approach was demonstrated by performing different multiple-quantum filtered COSY experiments. It also becomes possible to generate linear combinations, which differ from the conventionally acquired spectra a posteriori. For example, we implemented diagonal peak reduction by using zero- and single-quantum filtered COSY contributions without requiring additional experiment time. Copyright © 2009 John Wiley & Sons, Ltd. [source] Fast 1H,13C correlation data for use in automatic structure confirmation of small organic compoundsMAGNETIC RESONANCE IN CHEMISTRY, Issue 2 2005Adrian J. Dunn Abstract A method of speeding up the acquisition of 1H,13C correlation data has been developed. It is applicable in situations where the experiment time is determined by the need to sample the second dimension adequately rather than by signal-to-noise ratio requirements. Two spectra with different, reduced, 13C sweep widths are measured, time being saved by reducing the number of increments in line with the reduction in the sweep width. Rules are presented for the selection of the two reduced sweep widths so that the correct 13C chemical shifts can be easily and unambiguously calculated. The benefits and limitations of this approach, in the context of the structure confirmation of small (MW , 450) organic compounds, is discussed. The use of a third spectrum to resolve problems that may be encountered when proton signals overlap is demonstrated. Copyright © 2004 John Wiley & Sons, Ltd. [source] Investigating DNA migration in pulsed fields using a miniaturized FIGE systemELECTROPHORESIS, Issue 23 2008Xiaojia Chen Abstract PFGE is a well-established technique for fractionation of DNA fragments ranging from kilobases to megabases in length. But many of these separations require an undesirable combination of long experiment times (often approaching tens of hours) and application of high voltages (often approaching tens of kV). Here, we present a simple miniaturized FIGE apparatus capable of separating DNA fragments up to 32.5,kb in length within 3,h using a modest applied potential of 20,V. The device is small enough to be imaged under a fluorescence microscope, permitting the migrating DNA bands to be observed during the course of the separation run. We use this capability to investigate how separation performance is affected by parameters including the ratio of forward and backward voltage, pulse time, and temperature. We also characterize the dependence of DNA mobility on fragment size N, and observe a scaling in the vicinity of N,0.5 over the size range investigated. The high speed, low power consumption, and simple design of this system may help enable future studies of DNA migration in PFGE to be performed quickly and inexpensively. [source] Can the choice of endpoint lead to contradictory results of mixture-toxicity experiments?ENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 7 2005Nina Cedergreen Abstract Theoretically, the effect of two independently acting compounds in a mixture will depend on the slope of the dose-response curves of the individual compounds if evaluated in relation to the model of concentration addition (CA). In the present study, we explored development of the shape of the dose-response relationship for four different recommended endpoints (surface area, frond number, fresh weight-specific, and dry weight-specific relative growth rates [RGRA, RGRF, RGRFW, and RGRDW, respectively]) and for two differently acting herbicides (metsulfuron-methyl and terbuthylazine) over time (3,15 d) on the standard test plant Lemna minor to identify endpoints and experiment times for which predictions of independent action (IA) would depart the most from those of CA. After a test time of 6 d, predictions of IA based on RGRA and RGRFW showed antagonism in relation to CA. Based on RGRDW, synergy was predicted, whereas IA based on RGRF was indistinguishable from CA. To test the prediction of choice of endpoint giving different results in mixture-toxicity experiments, three endpoints and six combinations of independently acting herbicides were evaluated using isobolograms. The experiments showed that in four of six herbicide combinations, different conclusions were reached depending on endpoint. The contradictory isoboles did not follow the theory of IA and, therefore, are more likely to be related to differences in susceptibility of the physiological processes affecting each endpoint than to the shape of the dose-response curve. [source] |