Robust Heteronuclear Correlations for Sub-milligram Protein in Ultrafast Magic-Angle Spinning Solid-State NMR

doi:10.1021/jacs.5c00191

	Robust Heteronuclear Correlations for Sub-milligram Protein in Ultrafast Magic-Angle Spinning Solid-State NMR
	Xiao, Hang 1; Wang, Jian2 ; Tan, Huan 1; Gan, Yuefang 1; Liu, Wenjing 1; Zhang, Yan 1; Zhang, Zhengfeng 3; Yang, Jun 1,3
	2025
发表期刊	JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (IF:14.4[JCR-2023],14.8[5-Year])
ISSN	0002-7863
EISSN	1520-5126
卷号	147 期号:8 页码:6384-6389
发表状态	已发表
DOI	10.1021/jacs.5c00191
摘要	Proton-detected solid-state nuclear magnetic resonance (ssNMR) under ultrafast magic-angle spinning (MAS) has become a powerful tool for elucidating the structures of proteins with sub-milligram quantities, where establishing 13C-15N correlations is essential. However, traditional 13C-15N cross-polarization (CP), effective at lower MAS frequencies, suffers diminished efficiency under ultrafast MAS conditions. To overcome this limitation, we developed a robust method for selective polarization between insensitive nuclei (SPINE). This approach significantly enhances the heteronuclear 13C-15N correlation efficiency over CP, with gain factors of 1.75 for 13CA-15N and 1.9 and 13CO-15N transfers. SPINE’s efficacy was validated on four diverse proteins: the microcrystalline β1 immunoglobulin binding domain of protein G (GB1), the large-conductance mechanosensitive ion channel from Methanosarcina acetivorans (MaMscL), fibrillar septum-forming protein (SepF), and the vertex protein of the β-carboxysome shell (CcmL). This enhancement can reduce the duration of current multidimensional experiments to about one-third of that using a single 13C-15N CP and to about one-tenth with dual 13C-15N transfers. Our findings underscore the practical utility and versatility of SPINE in ssNMR spectroscopy, making it a valuable approach for advancing structural biology studies of sub-milligram protein. © 2025 American Chemical Society.
关键词	Atomic emission spectroscopy Binding energy Nuclear magnetic resonance spectroscopy Polarization Cross polarizations Heteronuclear Heteronuclear correlation Magic-angle spinning Robust methods Solid state NMR Solid-state nuclear magnetic resonance Spinning conditions Spinning frequency Ultra-fast
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收录类别	EI ; SCI
语种	英语
资助项目	National Natural Science Foundation of China["22074153","22104091","21927801","22434003","21921004"] ; National Natural Science Foundation of China["YJKYYQ20190032","XDB0540000"]
WOS研究方向	Chemistry
WOS类目	Chemistry, Multidisciplinary
WOS记录号	WOS:001422604700001
出版者	American Chemical Society
EI入藏号	20250717883391
EI主题词	Magic angle spinning
EI分类号	1301.1.2 Physical Properties of Gases, Liquids and Solids ; 1301.1.3.1 Spectroscopy ; 801.3 Physical Chemistry
原始文献类型	Article in Press
文献类型	期刊论文
条目标识符	https://kms.shanghaitech.edu.cn/handle/2MSLDSTB/490315
专题	生命科学与技术学院生命科学与技术学院_公共科研平台_高性能计算平台
通讯作者	Zhang, Zhengfeng; Yang, Jun
作者单位	1.National Center for Magnetic Resonance in Wuhan, Key Laboratory of Magnetic Resonance in Biological Systems, State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics and Mathematics, Innovation Academy for Precision Measurement Science and Technology, Chinese Academy of Sciences, Wuhan; 430071, China; 2.School of Life Science and Technology, ShanghaiTech University, Shanghai; 201210, China; 3.Interdisciplinary Institute of NMR and Molecular Sciences, School of Chemistry and Chemical Engineering, The State Key Laboratory of Refractories and Metallurgy, Wuhan University of Science and Technology, Wuhan; 430081, China
推荐引用方式 GB/T 7714	Xiao, Hang,Wang, Jian,Tan, Huan,et al. Robust Heteronuclear Correlations for Sub-milligram Protein in Ultrafast Magic-Angle Spinning Solid-State NMR[J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY,2025,147(8):6384-6389.
APA	Xiao, Hang.,Wang, Jian.,Tan, Huan.,Gan, Yuefang.,Liu, Wenjing.,...&Yang, Jun.(2025).Robust Heteronuclear Correlations for Sub-milligram Protein in Ultrafast Magic-Angle Spinning Solid-State NMR.JOURNAL OF THE AMERICAN CHEMICAL SOCIETY,147(8),6384-6389.
MLA	Xiao, Hang,et al."Robust Heteronuclear Correlations for Sub-milligram Protein in Ultrafast Magic-Angle Spinning Solid-State NMR".JOURNAL OF THE AMERICAN CHEMICAL SOCIETY 147.8(2025):6384-6389.