Rajat Garg , Barry DeZonia , Alexander L. Paterson , Chad M. Rienstra
{"title":"Low power supercycled TPPM decoupling","authors":"Rajat Garg , Barry DeZonia , Alexander L. Paterson , Chad M. Rienstra","doi":"10.1016/j.jmr.2024.107726","DOIUrl":null,"url":null,"abstract":"<div><p>Improving the spectral sensitivity and resolution of biological solids is one of the long-standing problems in nuclear magnetic resonance (NMR) spectroscopy. In this report, we introduce low-power supercycled variants of two-pulse phase-modulated (TPPM) sequence for heteronuclear decoupling. The utility of the sequence is shown by improvements in the transverse relaxation time of observed nuclei (with <sup>1</sup>H decoupling) with its application to different samples (uniformly <sup>13</sup>C, <sup>15</sup>N, <sup>2</sup>H-labeled GB1 back-exchanged with 25% H<span><math><msub><mrow></mrow><mrow><mn>2</mn></mrow></msub></math></span>O and 75% D<span><math><msub><mrow></mrow><mrow><mn>2</mn></mrow></msub></math></span>O, uniformly <sup>13</sup>C, <sup>15</sup>N, <sup>2</sup>H-labeled human derived Asyn fibril back-exchanged with 100% H<span><math><msub><mrow></mrow><mrow><mn>2</mn></mrow></msub></math></span>O and uniformly <sup>13</sup>C, <sup>15</sup>N -labeled human derived Asyn fibril) at fast MAS using low radiofrequency (RF) fields. To understand the effect of spinning speed, the transverse relaxation time is monitored under different spinning frequencies. In comparison to existing heteronuclear decoupling sequences, the supercycled TPPM (sTPPM) sequence significantly improves the spectral sensitivity and resolution and is robust towards <span><math><msub><mrow><mi>B</mi></mrow><mrow><mn>1</mn></mrow></msub></math></span> inhomogeneity and decoupler offset.</p></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":null,"pages":null},"PeriodicalIF":2.0000,"publicationDate":"2024-07-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of magnetic resonance","FirstCategoryId":"92","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S1090780724001101","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
引用次数: 0
Abstract
Improving the spectral sensitivity and resolution of biological solids is one of the long-standing problems in nuclear magnetic resonance (NMR) spectroscopy. In this report, we introduce low-power supercycled variants of two-pulse phase-modulated (TPPM) sequence for heteronuclear decoupling. The utility of the sequence is shown by improvements in the transverse relaxation time of observed nuclei (with 1H decoupling) with its application to different samples (uniformly 13C, 15N, 2H-labeled GB1 back-exchanged with 25% HO and 75% DO, uniformly 13C, 15N, 2H-labeled human derived Asyn fibril back-exchanged with 100% HO and uniformly 13C, 15N -labeled human derived Asyn fibril) at fast MAS using low radiofrequency (RF) fields. To understand the effect of spinning speed, the transverse relaxation time is monitored under different spinning frequencies. In comparison to existing heteronuclear decoupling sequences, the supercycled TPPM (sTPPM) sequence significantly improves the spectral sensitivity and resolution and is robust towards inhomogeneity and decoupler offset.
期刊介绍:
The Journal of Magnetic Resonance presents original technical and scientific papers in all aspects of magnetic resonance, including nuclear magnetic resonance spectroscopy (NMR) of solids and liquids, electron spin/paramagnetic resonance (EPR), in vivo magnetic resonance imaging (MRI) and spectroscopy (MRS), nuclear quadrupole resonance (NQR) and magnetic resonance phenomena at nearly zero fields or in combination with optics. The Journal''s main aims include deepening the physical principles underlying all these spectroscopies, publishing significant theoretical and experimental results leading to spectral and spatial progress in these areas, and opening new MR-based applications in chemistry, biology and medicine. The Journal also seeks descriptions of novel apparatuses, new experimental protocols, and new procedures of data analysis and interpretation - including computational and quantum-mechanical methods - capable of advancing MR spectroscopy and imaging.