综述评论

固体核磁共振魔角旋转条件下的定量交叉极化技术(英文)

  • 梁力鑫 ,
  • 邓风 ,
  • 侯广进
展开
  • 1. 催化基础国家重点实验室, 洁净能源国家实验室, 能源材料化学协同创新中心, 中国科学院 大连化学物理研究所, 辽宁 大连 116023;
    2. 波谱与原子分子物理国家重点实验室, 武汉磁共振中心(中国科学院 武汉物理与数学研究所), 湖北 武汉 430071;
    3. 中国科学院大学, 北京 100049

收稿日期: 2019-08-29

  网络出版日期: 2019-10-16

基金资助

the National Natural Science Foundation of China (21773230); Liaoning Revitalization Talents Program (XLYC1807207); Innovation Foundation of Dalian Institute of Chemical Physics (Y7611105T5).

Quantitative Cross Polarization Magic-Angle Spinning NMR Spectroscopy in Solids

  • LIANG Li-xin ,
  • DENG Feng ,
  • HOU Guang-jin
Expand
  • 1. State Key Laboratory of Catalysis, National Laboratory for Clean Energy, Collaborative Innovation Center of Chemistry for Energy Materials, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;
    2. State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, National Center for Magnetic Resonance in Wuhan(Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences), Wuhan 430071, China;
    3. University of Chinese Academy of Sciences, Beijing 100049, China

Received date: 2019-08-29

  Online published: 2019-10-16

Supported by

the National Natural Science Foundation of China (21773230); Liaoning Revitalization Talents Program (XLYC1807207); Innovation Foundation of Dalian Institute of Chemical Physics (Y7611105T5).

摘要

交叉极化与魔角旋转结合(CP/MAS)的方法已经成为增强固体核磁共振(NMR)检测灵敏度最重要的技术之一.CP/MAS技术的应用大大提高了固体NMR谱图的采集效率.然而,I-S偶极耦合作用、旋转坐标系下的自旋-晶格弛豫、分子运动,以及样品中丰核的分布情况等因素,通常会导致CP/MAS谱图失去定量作用.近年来,多个研究组通过改进或者设计新型固体NMR脉冲序列,获得了基于CP的可用于定量分析的固体NMR谱图.本综述首先简要介绍了CP及CP动力学,随后介绍了一系列基于CP的定量固体NMR信号增强技术,具体包括ramped-amplitude CP(RAMP-CP)、multiple-contact CP、quantification of CP(QCP)、Lee-Goldburg frequency modulated CP(LG-FMCP)和quantitative CP(QUCP).

本文引用格式

梁力鑫 , 邓风 , 侯广进 . 固体核磁共振魔角旋转条件下的定量交叉极化技术(英文)[J]. 波谱学杂志, 2020 , 37(1) : 1 -15 . DOI: 10.11938/cjmr20192779

Abstract

The combination of cross polarization and magic-angle spinning (CP/MAS), is a routine technique for signal enhancement in solid-state nuclear magnetic resonance (NMR) spectrum. With CP/MAS, the acquisition efficiency of solid-state NMR experiments can be improved greatly. However, the enhanced signal is not quantitative according to the different CP dynamics dominated by several factors including heteronuclear dipolar couplings, spin-lattice relaxation times in the rotating frame, molecular motions, number of around abundant spins, and so on. Over the years, numerous efforts have been made to obtain quantitative CP/MAS spectroscopy. This review firstly briefly illustrated the introduction of CP and CP dynamics, and then a series of quantitative NMR methods based on CP were introduced, including ramped-amplitude CP (RAMP-CP), multiple-contact CP, quantification of CP (QCP), Lee-Goldburg frequency modulated CP (LG-FMCP) and quantitative CP (QUCP).

参考文献

[1] ENRST R R. Sensitivity enhancement in magnetic resonance[J]. Advances in Magnetic and Optical Resonance, 1966, 2:1-135.
[2] PINES A, GIBBY M G, WAUGH J S. Proton-enhanced NMR of dilute spins in solids[J]. J Chem Phys, 1973, 59(2):569-590.
[3] WU X L, ZHANG S M. Polarization transfer in solid state CPMAS NMR[J]. Chinese J Magn Reson, 1995, 12(4):429-438. 吴肖令, 张善民. 固态交叉极化魔角旋转NMR中的极化转移[J]. 波谱学杂志, 1995, 12(4):429-438.
[4] DING S W, FU R Q, YE C H. Effects of non-secular terms in heteronuclear dipolar interaction on cross polarization relaxation rate[J]. Chinese J Magn Reson, 1993, 10(2):123-130. 丁尚武, 傅日强, 叶朝辉. 异核偶极相互作用非久期项对交叉极化弛豫速率的影响[J]. 波谱学杂志, 1993, 10(2):123-130.
[5] LEVITT M H, SUTER D, ERNST R R. Spin dynamics and thermodynamics in solid-state NMR cross polarization[J]. J Chem Phys, 1986, 84(8):4243.
[6] SHEKAR S C, LEE D K, RAMAMOORTHY A. Chemical shift anisotropy and offset effects in cross polarization solid-state NMR spectroscopy[J]. J Magn Reson, 2002, 157(2):223-234.
[7] PAULSON E K, MARTIN R W, ZILM K W. Cross polarization, radio frequency field homogeneity, and circuit balancing in high field solid state NMR probes[J]. J Magn Reson, 2004, 171(2):314-323.
[8] ZHANG S M, WU X L, MEHRING M. Successive polarization under mismatched hartmann-hahn condition[J]. Chem Phys Lett, 1990, 166(1):92-94.
[9] ZHANG S M, WU X L, ZHANG H P, et al. Quantitative measurement of rare spins in solid state cross polarization NMR[J]. Chem Phys Lett, 1990, 165(6):465-468.
[10] METZ G, ZILIOX M, SMITH S O. Towards quantitative CP-MAS NMR[J]. Solid State Nucl Magn Reson, 1996, 7(3):155-160.
[11] FU R Q, HU J, CROSS T A. Towards quantitative measurements in solid-state CPMAS NMR:A Lee-Goldburg frequency modulated cross-polarization scheme[J]. J Magn Reson, 2004, 168(1):8-17.
[12] HOU G J, DENG F, DING S W, et al. Quantitative cross-polarization NMR spectroscopy in uniformly 13C-labeled solids[J]. Chem Phys Lett, 2006, 421(4-6):356-360.
[13] HOU G J, DENG F, YE C H, et al. Towards uniform enhancement in solid-state cross polarization magic[corrected] angle spinning NMR:a scheme incorporating cross polarization with rotational resonance[J]. J Chem Phys, 2006, 124(23):234512.
[14] SHU J, CHEN Q, ZHANG S M. Quantification of cross polarization with relaxation compensated reciprocity relation in NMR[J]. Chem Phys Lett, 2008, 462(1-3):125-128.
[15] HOU G J, DING S W, ZHANG L M, et al. Breaking the T1 constraint for quantitative measurement in magic angle[J]. J Am Chem Soc, 2010, 132(16):5538-5539.
[16] TANG W X, NEVZOROV A A. Repetitive cross-polarization contacts via equilibration-re-equilibration of the proton bath:Sensitivity enhancement for NMR of membrane proteins reconstituted in magnetically aligned bicelles[J]. J Magn Reson, 2011, 212(1):245-248.
[17] TAKEDA K, NODA Y, TAKEGOSHI K, et al. Quantitative cross-polarization at magic-angle spinning frequency of about 20 kHz[J]. J Magn Reson, 2012, 214(1):340-345.
[18] JOHNSON R L, SCHMIDT-ROHR K. Quantitative solid-state 13C NMR with signal enhancement by multiple cross polarization[J]. J Magn Reson, 2014, 239:44-49.
[19] LIU H W, ZHOU X Y, CHEN Q, et al. Accurate quantitative and maximum cross polarization via multiple ramped contacts[J]. Chem Phys Lett, 2017, 679(1):233-236.
[20] LIU H W, ZHANG S M. Quantitative analysis of a labeled 13C system in NMR[J]. Chem Phys Lett, 2015, 621:199-202.
[21] PEERSON O B, WU X L, KUSTANOVICH I, et al. Variable-amplitude cross-polarization MAS NMR[J]. J Magn Reson, Series A, 1993, 104(3):334-339.
[22] METZ G, WU X L, SMITH S O. Ramped-amplitude cross polarization in magic-angle-spinning NMR[J]. J Magn Reson, Series A, 1994, 110(2):219-227.
[23] COOK R L, LANGFORD C H, YAMDAGNI R, et al. A modified cross-polarization magic angle spinning 13C NMR procedure for the study of humic materials[J]. Anal Chem, 1996, 68(22):3979-3986.
[24] WU X L, ZHANG S M. Selective polarization inversion and depolarization of 13C in cross relaxation in NMR[J]. Chem Phys Lett, 1989, 156(1):79-81.
[25] GERSTEIN B C, DYBOWSKI C R. Transient techniques in NMR of solids:an introduction to theory and practice[M]. San Diego:Academic Press, 1985.
[26] RAYA J, PERRONE B, HIRSCHINGER J. Chemical shift powder spectra enhanced by multiple-contact cross-polarization under slow magic-angle spinning[J]. J Magn Reson, 2013, 227:93-102.
[27] BROWNBILL N J, SPRICK R S, BONILLO B, et al. Structural elucidation of amorphous photocatalytic polymers from dynamic nuclear polarization enhanced solid state NMR[J]. Macromolecules, 2018, 51(8):3088-3096.
[28] KING C, STEIN R S, SHAMSHINA J L, et al. Measuring the purity of chitin with a clean, quantitative solid-state NMR method[J]. ACS Sustainable Chem Eng, 2017, 5(9):8011-8016.
[29] SMET S, VERLOOY P, SAIDI F, et al. Solid-state NMR tools for the structural characterization of POSiSils:(29) Si sensitivity improvement with MC-CP and 2D (29) Si-(29) Si DQ-SQ at natural abundance[J]. Magn Reson Chem, 2019, 57(5):224-229.
[30] WU X L, SHANMIN Z, XUEWEN W. Two-stage feature of Hartmann-Hahn cross relaxation in magic-angle sample spinning[J]. Phys Rev B Condens Matter, 1988, 37(16):9827-9829.
[31] SHU W F, ZHANG S M. Relaxation compensated and intensity recovered dynamics of cross polarization in the frame of reciprocity relation[J]. Chem Phys Lett, 2011, 511(4-6):424-426.
[32] LU X Y, GUO C M, HOU G J, et al. Combined zero-quantum and spin-diffusion mixing for efficient homonuclear correlation spectroscopy under fast MAS:broadband recoupling and detection of long-range correlations[J]. J Biomol NMR, 2015, 61(1):7-20.
[33] FU R Q, TIAN C L, CROSS T A. NMR spin locking of proton magnetization under a frequency-switched Lee-Goldburg pulse sequence[J]. J Magn Reson, 2002, 154(1):130-135.
[34] LEE M, GOLDBURG I W. Nuclear-magnetic-resonance line narrowing by a rotating RF field[J]. Phys Rev, 1965, 140(4A):1261-1271.
[35] TAKEGOSHI K, NAKAMURA S, TERAO T. 13C-1H dipolar-assisted rotational resonance in magic-angle spinning NMR[J]. Chem Phys Lett, 2001, 344(5):634-637.
[36] RALEIGH D P, LEVITT M H, GRIFFIN R G. Rotational resonance in solid state NMR[J]. Chem Phys Lett, 1988, 146(1,2):71-76.
[37] OAS T G, GRIFFIN R G, LEVITT M H. Rotary resonance recoupling of dipolar interactions in solid-state nuclear magnetic resonance spectroscopy[J]. J Chem Phys, 1988, 89(2):692-695.
[38] ZHANG R C, MROUE K H, RAMAMOORTHY A. Proton-based ultrafast magic angle spinning solid-state NMR spectroscopy[J]. Acc Chem Res, 2017, 50(4):1105-1113.
[39] CHEN L, WANG Q, HU B W, et al. Measurement of hetero-nuclear distances using a symmetry-based pulse sequence in solid-state NMR[J]. Phys Chem Chem Phys, 2010, 12(32):9395-9405.
[40] TEYMOORI G, PAHARI B, VISWANATHAN E, et al. Multiple-quantum spin counting in magic-angle-spinning NMR via low-power symmetry-based dipolar recoupling[J]. J Magn Reson, 2013, 236:31-40.
[41] HOU G J, YAN S, TREBOSC J, et al. Broadband homonuclear correlation spectroscopy driven by combined R2(n)(v) sequences under fast magic angle spinning for NMR structural analysis of organic and biological solids[J]. J Magn Reson, 2013, 232:18-30.
[42] SHEN M, HU B W, LAFON O, et al. Broadband finite-pulse radio-frequency-driven recoupling (fp-RFDR) with (XY8)4(1) super-cycling for homo-nuclear correlations in very high magnetic fields at fast and ultra-fast MAS frequencies[J]. J Magn Reson, 2012, 223:107-119.
[43] HU B W, LAFON O, TREBOSC J, et al. Broad-band homo-nuclear correlations assisted by 1H irradiation for bio-molecules in very high magnetic field at fast and ultra-fast MAS frequencies[J]. J Magn Reson, 2011, 212(2):320-329.
[44] WEINGARTH M, DEMCO D E, BODENHAUSEN G, et al. Improved magnetization transfer in solid-state NMR with fast magic angle spinning[J]. Chem Phys Lett, 2009, 469(4-6):342-348.
[45] HOU G J, YAN S, SUN S J, et al. Spin diffusion driven by R-symmetry sequences:applications to homonuclear correlation spectroscopy in MAS NMR of biological and organic solids[J]. J Am Chem Soc, 2011, 133(11):3943-3953.
[46] JAYANTHI S, AKBEY U, ULUCA B, et al. A floquet description of phase alternated sequences for efficient homonuclear recoupling in solid perdeuterated systems[J]. J Magn Reson, 2013, 234:10-20.
文章导航

/