SOGGY: solvent-optimized double gradient spectroscopy for water suppression. A comparison with some existing techniques.
ABSTRACT Excitation sculpting, a general method to suppress unwanted magnetization while controlling the phase of the retained signal [T.L. Hwang, A.J. Shaka, Water suppression that works. Excitation sculpting using arbitrary waveforms and pulsed field gradients, J. Magn. Reson. Ser. A 112 (1995) 275-279] is a highly effective method of water suppression for both biological and small molecule NMR spectroscopy. In excitation sculpting, a double pulsed field gradient spin echo forms the core of the sequence and pairing a low-power soft 180 degrees (-x) pulse with a high-power 180 degrees (x) all resonances except the water are flipped and retained, while the water peak is attenuated. By replacing the hard 180 degrees pulse in the double echo with a new phase-alternating composite pulse, broadband and adjustable excitation of large bandwidths with simultaneous high water suppression is obtained. This "Solvent-Optimized Gradient-Gradient Spectroscopy" (SOGGY) sequence is a reliable workhorse method for a wide range of practical situations in NMR spectroscopy, optimizing both solute sensitivity and water suppression.
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ABSTRACT: The complementary use of liquid chromatography (LC) and nuclear magnetic resonance (NMR) has shown high utility in a variety of fields. While the significant benefit of spectral simplification can be achieved for the analysis of complex samples, other limitations remain. For example, 1H LC-NMR suffers from pH dependent chemical shift variations, especially during urine analysis, owing to the high physiological variation of urine pH. Additionally, large solvent signals from the mobile phase in LC can obscure lower intensity signals and severely limit the number of metabolites detected. These limitations, along with sample dilution, hinder the ability to make reliable chemical shift assignments. Recently, stable isotopic labeling has been used to detect quantitatively specific classes of metabolites of interest in biofluids. Here we present a strategy that explores the combined use of two-dimensional hydrophilic interaction chromatography (HILIC) and isotope tagged NMR for the unambiguous identification of carboxyl containing metabolites present in human urine. The ability to separate structurally related compounds chromatographically, in off-line mode, followed by detection using 1H-15N 2D HSQC (two-dimensional heteronuclear single quantum coherence) spectroscopy, resulted in the assignment of low concentration carboxyl-containing metabolites from a library of isotope labeled compounds. The quantitative nature of this strategy is also demonstrated.09/2013; 3(3):575-591. DOI:10.3390/metabo3030575
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ABSTRACT: Aberrant energy metabolism is a hallmark of cancer. To fulfill the increased energy requirements, tumor cells secrete cytokines/factors inducing muscle and fat degradation in cancer patients, a condition known as cancer cachexia. It accounts for nearly 20% of all cancer-related deaths. However, the mechanistic basis of cancer cachexia and therapies targeting cancer cachexia thus far remain elusive. A ketogenic diet, a high-fat and low-carbohydrate diet that elevates circulating levels of ketone bodies (i.e., acetoacetate, β-hydroxybutyrate, and acetone), serves as an alternative energy source. It has also been proposed that a ketogenic diet leads to systemic metabolic changes. Keeping in view the significant role of metabolic alterations in cancer, we hypothesized that a ketogenic diet may diminish glycolytic flux in tumor cells to alleviate cachexia syndrome and, hence, may provide an efficient therapeutic strategy.09/2014; 2:18. DOI:10.1186/2049-3002-2-18