DNP 增强的细菌视紫红质中频率选择 TEDOR 实验。
DNP enhanced frequency-selective TEDOR experiments in bacteriorhodopsin.
机构信息
Department of Chemistry, Massachusetts Institute of Technology, Cambridge, MA 02139, USA.
出版信息
J Magn Reson. 2010 Jan;202(1):9-13. doi: 10.1016/j.jmr.2009.09.005. Epub 2009 Sep 9.
Abstract
We describe a new approach to multiple (13)C-(15)N distance measurements in uniformly labeled solids, frequency-selective (FS) TEDOR. The method shares features with FS-REDOR and ZF- and BASE-TEDOR, which also provide quantitative (15)N-(13)C spectral assignments and distance measurements in U-[(13)C,(15)N] samples. To demonstrate the validity of the FS-TEDOR sequence, we measured distances in [U-(13)C,(15)N]-asparagine which are in good agreement with other methods. In addition, we integrate high frequency dynamic nuclear polarization (DNP) into the experimental protocol and use FS-TEDOR to record a resolved correlation spectrum of the Arg-(13)C(gamma)-(15)N(epsilon) region in [U-(13)C,(15)N]-bacteriorhodopsin. We resolve six of the seven cross-peaks expected based on the primary sequence of this membrane protein.
摘要
我们描述了一种在均标记固体中进行多个（13）C-（15）N 距离测量的新方法，即频率选择（FS）TEDOR。该方法与 FS-REDOR 和 ZF- 和 BASE-TEDOR 具有共同的特点，这两种方法也可在 U-[(13)C,（15）N]样品中提供定量（15）N-（13）C 光谱分配和距离测量。为了证明 FS-TEDOR 序列的有效性，我们测量了 [U-（13）C，（15）N]-天冬酰胺中的距离，这些距离与其他方法非常吻合。此外，我们将高频动态核极化（DNP）集成到实验方案中，并使用 FS-TEDOR 记录 [U-（13）C，（15）N]-细菌视紫红质中 Arg-（13）C（γ）-（15）N（ε）区域的分辨相关谱。我们根据该膜蛋白的一级序列解析了七个预期的交叉峰中的六个。
相似文献
1
DNP enhanced frequency-selective TEDOR experiments in bacteriorhodopsin.DNP 增强的细菌视紫红质中频率选择 TEDOR 实验。
J Magn Reson. 2010 Jan;202(1):9-13. doi: 10.1016/j.jmr.2009.09.005. Epub 2009 Sep 9.
2
3D TEDOR NMR experiments for the simultaneous measurement of multiple carbon-nitrogen distances in uniformly (13)C,(15)N-labeled solids.用于同时测量均匀（13）C、（15）N标记固体中多个碳-氮距离的3D TEDOR NMR实验。
J Am Chem Soc. 2002 Sep 11;124(36):10728-42. doi: 10.1021/ja026385y.
3
Functional and shunt states of bacteriorhodopsin resolved by 250 GHz dynamic nuclear polarization-enhanced solid-state NMR.通过250吉赫兹动态核极化增强固态核磁共振解析细菌视紫红质的功能和分流状态。
Proc Natl Acad Sci U S A. 2009 Jun 9;106(23):9244-9. doi: 10.1073/pnas.0900908106. Epub 2009 May 27.
4
Optimization of N-C double-resonance NMR experiments under low temperature magic angle spinning dynamic nuclear polarization conditions.低温魔角旋转动态核极化条件下 N-C 双共振 NMR 实验的优化。
J Magn Reson. 2024 Nov;368:107783. doi: 10.1016/j.jmr.2024.107783. Epub 2024 Oct 2.
5
Measurement of dipolar couplings in a uniformly (13)C,(15)N-labeled membrane protein: distances between the Schiff base and aspartic acids in the active site of bacteriorhodopsin.均匀（13）C、（15）N标记膜蛋白中偶极耦合的测量：细菌视紫红质活性位点中席夫碱与天冬氨酸之间的距离
J Am Chem Soc. 2001 Dec 26;123(51):12929-30. doi: 10.1021/ja016923r.
6
Efficient resonance assignment of proteins in MAS NMR by simultaneous intra- and inter-residue 3D correlation spectroscopy.利用 MAS NMR 中同时的内残基和间残基 3D 相关光谱技术实现蛋白质的高效共振分配。
J Biomol NMR. 2013 Mar;55(3):257-65. doi: 10.1007/s10858-013-9707-0. Epub 2013 Jan 19.
7
Atomic resolution protein structure determination by three-dimensional transferred echo double resonance solid-state nuclear magnetic resonance spectroscopy.通过三维转移回波双共振固态核磁共振波谱学测定原子分辨率蛋白质结构。
J Chem Phys. 2009 Sep 7;131(9):095101. doi: 10.1063/1.3211103.
8
Advances towards resonance assignments for uniformly--13C, 15N enriched bacteriorhodopsin at 18.8 T in purple membranes.在紫色膜中对均匀富集13C、15N的细菌视紫红质在18.8 T磁场下进行共振归属的进展。
J Biomol NMR. 2008 May;41(1):1-4. doi: 10.1007/s10858-008-9235-5. Epub 2008 Apr 22.
9
A robust heteronuclear dipolar recoupling method comparable to TEDOR for proteins in magic-angle spinning solid-state NMR.一种在魔角旋转固态核磁共振中与TEDOR相当的用于蛋白质的强大异核偶极重耦合方法。
J Magn Reson. 2017 Dec;285:79-85. doi: 10.1016/j.jmr.2017.10.012. Epub 2017 Oct 31.
10
Selective measurements of long-range homonuclear J-couplings in solid-state NMR.固态 NMR 中长程同核 J 耦合的选择测量。
J Magn Reson. 2013 Jun;231:90-4. doi: 10.1016/j.jmr.2013.03.010. Epub 2013 Apr 4.
引用本文的文献
1
Highly efficient heteronuclear polarization transfer using dipolar-echo edited R-symmetry sequences in solid-state NMR.在固态核磁共振中使用偶极回波编辑的R-对称序列进行高效异核极化转移。
Chem Sci. 2024 Dec 21;16(5):2251-2257. doi: 10.1039/d4sc07965e. eCollection 2025 Jan 29.
2
Cross polarization stability in multidimensional NMR spectroscopy of biological solids.生物固体多维 NMR 光谱学中的交叉极化稳定性。
J Magn Reson. 2024 Aug;365:107724. doi: 10.1016/j.jmr.2024.107724. Epub 2024 Jun 23.
3
Resolution in cryogenic solid state NMR: Challenges and solutions.低温固态 NMR 中的分辨率：挑战与解决方案。
Protein Sci. 2024 Jul;33(7):e4803. doi: 10.1002/pro.4803.
4
H detection and dynamic nuclear polarization-enhanced NMR of Aβ fibrils.Aβ 纤维的 H 检测和动态核极化增强 NMR。
Proc Natl Acad Sci U S A. 2022 Jan 4;119(1). doi: 10.1073/pnas.2114413119.
5
Probing the photointermediates of light-driven sodium ion pump KR2 by DNP-enhanced solid-state NMR.通过动态核极化增强的固态 NMR 探测光驱动钠离子泵 KR2 的光中间产物。
Sci Adv. 2021 Mar 12;7(11). doi: 10.1126/sciadv.abf4213. Print 2021 Mar.
6
Characterization of photonic band resonators for DNP NMR of thin film samples at 7 T magnetic field.用于7T磁场下薄膜样品动态核极化核磁共振的光子带谐振器特性研究
J Magn Reson. 2021 Feb;323:106893. doi: 10.1016/j.jmr.2020.106893. Epub 2020 Dec 13.
7
Modular, triple-resonance, transmission line DNP MAS probe for 500 MHz/330 GHz.用于 500 MHz/330 GHz 的模块化、三共振、传输线 DNP MAS 探头。
J Magn Reson. 2019 Oct;307:106573. doi: 10.1016/j.jmr.2019.106573. Epub 2019 Aug 14.
8
Multi-resonant photonic band-gap/saddle coil DNP probehead for static solid state NMR of microliter volume samples.用于微升体积样品静态固态核磁共振的多共振光子带隙/鞍形线圈动态核极化探头。
J Magn Reson. 2018 Dec;297:113-123. doi: 10.1016/j.jmr.2018.10.010. Epub 2018 Oct 23.
9
Direct amide N to C transfers for solid-state assignment experiments in deuterated proteins.用于氘代蛋白质固态归属实验的直接酰胺氮到碳的转移
J Biomol NMR. 2018 Oct;72(1-2):69-78. doi: 10.1007/s10858-018-0207-0. Epub 2018 Sep 11.
10
New NMR tools for protein structure and function: Spin tags for dynamic nuclear polarization solid state NMR.用于蛋白质结构与功能研究的新型核磁共振工具：用于动态核极化固态核磁共振的自旋标记
Arch Biochem Biophys. 2017 Aug 15;628:102-113. doi: 10.1016/j.abb.2017.06.010. Epub 2017 Jun 13.
本文引用的文献
1
Rotational-echo double-resonance NMR. 1989.旋转回波双共振核磁共振。1989年。
J Magn Reson. 2011 Dec;213(2):413-7. doi: 10.1016/j.jmr.2011.09.003.
2
Dynamic nuclear polarization at 9T using a novel 250 GHz gyrotron microwave source. 2003.2003年，利用新型250吉赫兹回旋管微波源在9特斯拉下进行动态核极化。
J Magn Reson. 2011 Dec;213(2):404-9. doi: 10.1016/j.jmr.2011.09.010.
3
Functional and shunt states of bacteriorhodopsin resolved by 250 GHz dynamic nuclear polarization-enhanced solid-state NMR.通过250吉赫兹动态核极化增强固态核磁共振解析细菌视紫红质的功能和分流状态。
Proc Natl Acad Sci U S A. 2009 Jun 9;106(23):9244-9. doi: 10.1073/pnas.0900908106. Epub 2009 May 27.
4
Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization.用于魔角旋转动态核极化的低温样品交换核磁共振探头。
J Magn Reson. 2009 Jun;198(2):261-70. doi: 10.1016/j.jmr.2009.03.003. Epub 2009 Mar 17.
5
Dipolar truncation in magic-angle spinning NMR recoupling experiments.魔角旋转核磁共振再耦合实验中的偶极截断
J Chem Phys. 2009 Mar 21;130(11):114506. doi: 10.1063/1.3089370.
6
BioMagResBank (BMRB) as a partner in the Worldwide Protein Data Bank (wwPDB): new policies affecting biomolecular NMR depositions.生物磁共振数据库（BMRB）作为全球蛋白质数据银行（wwPDB）的合作伙伴：影响生物分子核磁共振沉积的新政策。
J Biomol NMR. 2008 Mar;40(3):153-5. doi: 10.1007/s10858-008-9221-y. Epub 2008 Feb 21.
7
Determination of methyl 13C-15N dipolar couplings in peptides and proteins by three-dimensional and four-dimensional magic-angle spinning solid-state NMR spectroscopy.通过三维和四维魔角旋转固态核磁共振光谱法测定肽和蛋白质中的甲基13C-15N偶极耦合。
J Chem Phys. 2008 Feb 7;128(5):052314. doi: 10.1063/1.2817638.
8
Energy transformations early in the bacteriorhodopsin photocycle revealed by DNP-enhanced solid-state NMR.动态核极化增强固态核磁共振揭示的细菌视紫红质光循环早期的能量转换
Proc Natl Acad Sci U S A. 2008 Jan 22;105(3):883-8. doi: 10.1073/pnas.0706156105. Epub 2008 Jan 14.
9
BioMagResBank.生物磁共振数据库
Nucleic Acids Res. 2008 Jan;36(Database issue):D402-8. doi: 10.1093/nar/gkm957. Epub 2007 Nov 4.
10
250GHz CW gyrotron oscillator for dynamic nuclear polarization in biological solid state NMR.用于生物固态核磁共振动态核极化的250GHz连续波回旋管振荡器。
J Magn Reson. 2007 Dec;189(2):251-79. doi: 10.1016/j.jmr.2007.09.013. Epub 2007 Sep 20.
Zotero 插件