{"title":"非共振13C-2H REDOR核磁共振用于分子运动的位点分辨研究","authors":"Martin D. Gelenter, Kelly J. Chen, Mei Hong","doi":"10.1007/s10858-021-00377-7","DOIUrl":null,"url":null,"abstract":"<div><p>We introduce a <sup>13</sup>C–<sup>2</sup>H Rotational Echo DOuble Resonance (REDOR) technique that uses the difference between on-resonance and off-resonance <sup>2</sup>H irradiation to detect dynamic segments in deuterated molecules. By selectively inverting specific regions of the <sup>2</sup>H magic-angle spinning (MAS) sideband manifold to recouple some of the deuterons to nearby carbons, we distinguish dynamic and rigid residues in 1D and 2D <sup>13</sup>C spectra. We demonstrate this approach on deuterated GB1, H/D exchanged GB1, and perdeuterated bacterial cellulose. Numerical simulations reproduce the measured mixing-time and <sup>2</sup>H carrier-frequency dependence of the REDOR dephasing of bacterial cellulose. Combining numerical simulations with experiments thus allow the extraction of motionally averaged quadrupolar couplings from REDOR dephasing values.</p></div>","PeriodicalId":613,"journal":{"name":"Journal of Biomolecular NMR","volume":"75 8-9","pages":"335 - 345"},"PeriodicalIF":1.3000,"publicationDate":"2021-08-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10858-021-00377-7.pdf","citationCount":"2","resultStr":"{\"title\":\"Off-resonance 13C–2H REDOR NMR for site-resolved studies of molecular motion\",\"authors\":\"Martin D. Gelenter, Kelly J. Chen, Mei Hong\",\"doi\":\"10.1007/s10858-021-00377-7\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>We introduce a <sup>13</sup>C–<sup>2</sup>H Rotational Echo DOuble Resonance (REDOR) technique that uses the difference between on-resonance and off-resonance <sup>2</sup>H irradiation to detect dynamic segments in deuterated molecules. By selectively inverting specific regions of the <sup>2</sup>H magic-angle spinning (MAS) sideband manifold to recouple some of the deuterons to nearby carbons, we distinguish dynamic and rigid residues in 1D and 2D <sup>13</sup>C spectra. We demonstrate this approach on deuterated GB1, H/D exchanged GB1, and perdeuterated bacterial cellulose. Numerical simulations reproduce the measured mixing-time and <sup>2</sup>H carrier-frequency dependence of the REDOR dephasing of bacterial cellulose. Combining numerical simulations with experiments thus allow the extraction of motionally averaged quadrupolar couplings from REDOR dephasing values.</p></div>\",\"PeriodicalId\":613,\"journal\":{\"name\":\"Journal of Biomolecular NMR\",\"volume\":\"75 8-9\",\"pages\":\"335 - 345\"},\"PeriodicalIF\":1.3000,\"publicationDate\":\"2021-08-03\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://link.springer.com/content/pdf/10.1007/s10858-021-00377-7.pdf\",\"citationCount\":\"2\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Biomolecular NMR\",\"FirstCategoryId\":\"99\",\"ListUrlMain\":\"https://link.springer.com/article/10.1007/s10858-021-00377-7\",\"RegionNum\":3,\"RegionCategory\":\"生物学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"BIOCHEMISTRY & MOLECULAR BIOLOGY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Biomolecular NMR","FirstCategoryId":"99","ListUrlMain":"https://link.springer.com/article/10.1007/s10858-021-00377-7","RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"BIOCHEMISTRY & MOLECULAR BIOLOGY","Score":null,"Total":0}
Off-resonance 13C–2H REDOR NMR for site-resolved studies of molecular motion
We introduce a 13C–2H Rotational Echo DOuble Resonance (REDOR) technique that uses the difference between on-resonance and off-resonance 2H irradiation to detect dynamic segments in deuterated molecules. By selectively inverting specific regions of the 2H magic-angle spinning (MAS) sideband manifold to recouple some of the deuterons to nearby carbons, we distinguish dynamic and rigid residues in 1D and 2D 13C spectra. We demonstrate this approach on deuterated GB1, H/D exchanged GB1, and perdeuterated bacterial cellulose. Numerical simulations reproduce the measured mixing-time and 2H carrier-frequency dependence of the REDOR dephasing of bacterial cellulose. Combining numerical simulations with experiments thus allow the extraction of motionally averaged quadrupolar couplings from REDOR dephasing values.
期刊介绍：
The Journal of Biomolecular NMR provides a forum for publishing research on technical developments and innovative applications of nuclear magnetic resonance spectroscopy for the study of structure and dynamic properties of biopolymers in solution, liquid crystals, solids and mixed environments, e.g., attached to membranes. This may include:
Three-dimensional structure determination of biological macromolecules (polypeptides/proteins, DNA, RNA, oligosaccharides) by NMR.
New NMR techniques for studies of biological macromolecules.
Novel approaches to computer-aided automated analysis of multidimensional NMR spectra.
Computational methods for the structural interpretation of NMR data, including structure refinement.
Comparisons of structures determined by NMR with those obtained by other methods, e.g. by diffraction techniques with protein single crystals.
New techniques of sample preparation for NMR experiments (biosynthetic and chemical methods for isotope labeling, preparation of nutrients for biosynthetic isotope labeling, etc.). An NMR characterization of the products must be included.
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