{"title":"碳检测氘固态核磁共振旋转框架弛豫测量魔角旋转下的蛋白质甲基基团","authors":"Liliya Vugmeyster , Dmitry Ostrovsky , Riqiang Fu","doi":"10.1016/j.ssnmr.2024.101922","DOIUrl":null,"url":null,"abstract":"<div><p>Deuterium rotating frame solid-state NMR relaxation measurements (<sup>2</sup>H <span><math><mrow><msub><mi>R</mi><mrow><mn>1</mn><mi>ρ</mi></mrow></msub></mrow></math></span>) are important tools in quantitative studies of molecular dynamics. We demonstrate how <sup>2</sup>H to <sup>13</sup>C cross-polarization (CP) approaches under 10–40 kHz magic angle spinning rates can be combined with the <sup>2</sup>H <span><math><mrow><msub><mi>R</mi><mrow><mn>1</mn><mi>ρ</mi></mrow></msub></mrow></math></span> blocks to allow for extension of deuterium rotating frame relaxation studies to methyl groups in biomolecules. This extension permits detection on the <sup>13</sup>C nuclei and, hence, for the achievement of site-specific resolution. The measurements are demonstrated using a nine-residue low complexity peptide with the sequence GGKGMGFGL, in which a single selective −<sup>13</sup>CD<sub>3</sub> label is placed at the methionine residue. Carbon-detected measurements are compared with the deuterium direct-detection results, which allows for fine-tuning of experimental approaches. In particular, we show how the adiabatic respiration CP scheme and the double adiabatic sweep on the <sup>2</sup>H and <sup>13</sup>C channels can be combined with the <sup>2</sup>H <span><math><mrow><msub><mi>R</mi><mrow><mn>1</mn><mi>ρ</mi></mrow></msub></mrow></math></span> relaxation rates measurement. Off-resonance <sup>2</sup>H <span><math><mrow><msub><mi>R</mi><mrow><mn>1</mn><mi>ρ</mi></mrow></msub></mrow></math></span> measurements are investigated in addition to the on-resonance condition, as they extent the range of effective spin-locking field.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":1.8000,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Carbon-detected deuterium solid-state NMR rotating frame relaxation measurements for protein methyl groups under magic angle spinning\",\"authors\":\"Liliya Vugmeyster , Dmitry Ostrovsky , Riqiang Fu\",\"doi\":\"10.1016/j.ssnmr.2024.101922\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>Deuterium rotating frame solid-state NMR relaxation measurements (<sup>2</sup>H <span><math><mrow><msub><mi>R</mi><mrow><mn>1</mn><mi>ρ</mi></mrow></msub></mrow></math></span>) are important tools in quantitative studies of molecular dynamics. We demonstrate how <sup>2</sup>H to <sup>13</sup>C cross-polarization (CP) approaches under 10–40 kHz magic angle spinning rates can be combined with the <sup>2</sup>H <span><math><mrow><msub><mi>R</mi><mrow><mn>1</mn><mi>ρ</mi></mrow></msub></mrow></math></span> blocks to allow for extension of deuterium rotating frame relaxation studies to methyl groups in biomolecules. This extension permits detection on the <sup>13</sup>C nuclei and, hence, for the achievement of site-specific resolution. The measurements are demonstrated using a nine-residue low complexity peptide with the sequence GGKGMGFGL, in which a single selective −<sup>13</sup>CD<sub>3</sub> label is placed at the methionine residue. Carbon-detected measurements are compared with the deuterium direct-detection results, which allows for fine-tuning of experimental approaches. In particular, we show how the adiabatic respiration CP scheme and the double adiabatic sweep on the <sup>2</sup>H and <sup>13</sup>C channels can be combined with the <sup>2</sup>H <span><math><mrow><msub><mi>R</mi><mrow><mn>1</mn><mi>ρ</mi></mrow></msub></mrow></math></span> relaxation rates measurement. Off-resonance <sup>2</sup>H <span><math><mrow><msub><mi>R</mi><mrow><mn>1</mn><mi>ρ</mi></mrow></msub></mrow></math></span> measurements are investigated in addition to the on-resonance condition, as they extent the range of effective spin-locking field.</p></div>\",\"PeriodicalId\":21937,\"journal\":{\"name\":\"Solid state nuclear magnetic resonance\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":1.8000,\"publicationDate\":\"2024-02-22\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Solid state nuclear magnetic resonance\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0926204024000080\",\"RegionNum\":3,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"CHEMISTRY, PHYSICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Solid state nuclear magnetic resonance","FirstCategoryId":"92","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0926204024000080","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CHEMISTRY, PHYSICAL","Score":null,"Total":0}
Carbon-detected deuterium solid-state NMR rotating frame relaxation measurements for protein methyl groups under magic angle spinning
Deuterium rotating frame solid-state NMR relaxation measurements (2H ) are important tools in quantitative studies of molecular dynamics. We demonstrate how 2H to 13C cross-polarization (CP) approaches under 10–40 kHz magic angle spinning rates can be combined with the 2H blocks to allow for extension of deuterium rotating frame relaxation studies to methyl groups in biomolecules. This extension permits detection on the 13C nuclei and, hence, for the achievement of site-specific resolution. The measurements are demonstrated using a nine-residue low complexity peptide with the sequence GGKGMGFGL, in which a single selective −13CD3 label is placed at the methionine residue. Carbon-detected measurements are compared with the deuterium direct-detection results, which allows for fine-tuning of experimental approaches. In particular, we show how the adiabatic respiration CP scheme and the double adiabatic sweep on the 2H and 13C channels can be combined with the 2H relaxation rates measurement. Off-resonance 2H measurements are investigated in addition to the on-resonance condition, as they extent the range of effective spin-locking field.
期刊介绍:
The journal Solid State Nuclear Magnetic Resonance publishes original manuscripts of high scientific quality dealing with all experimental and theoretical aspects of solid state NMR. This includes advances in instrumentation, development of new experimental techniques and methodology, new theoretical insights, new data processing and simulation methods, and original applications of established or novel methods to scientific problems.