Chinese Journal of Magnetic Resonance >
Two-Dimensional Homonuclear Orthogonal-Pattern Phase-Sensitive J-Resolved NMR Spectroscopy Based on Pure Shifts
Received date: 2021-06-29
Online published: 2021-08-26
Two-dimensional J-resolved (2D JRES) nuclear magnetic resonance (NMR) experiments provide a simple and user-friendly spectral representation, in which J couplings and chemical shifts are separated into two orthogonal frequency dimensions. The 2D JRES experiments have attracted wide attention in fundamental pulse sequence developments and practical applications, since they were first proposed 40 years ago. In this paper, we review the recent advances in the development of novel 2D JRES pulse sequences and 2D J-edited methods for accurate measurements of J coupling, mainly focusing on pure shift based 2D orthogonal-pattern and phase-sensitive 2D JRES spectroscopy and their applications in overcoming strong coupling effects and field inhomogeneities.
Xiao-qing LIN , Shi-jia DU , Hao-lin ZHAN , Yu-qing HUANG , Zhong CHEN . Two-Dimensional Homonuclear Orthogonal-Pattern Phase-Sensitive J-Resolved NMR Spectroscopy Based on Pure Shifts[J]. Chinese Journal of Magnetic Resonance, 2021 , 38(4) : 448 -459 . DOI: 10.11938/cjmr20212929
| 1 | DI CARO D , LIGUORI C , PIETROSANTO A , et al. Quality assessment of the inshell hazelnuts based on TD-NMR analysis[J]. IEEE Trans Instrum Meas, 2020, 69 (6): 3770- 3779. |
| 2 | EVANGELIDIS T , NERLI S , NOVACEK J , et al. Automated NMR resonance assignments and structure determination using a minimal set of 4D spectra[J]. Nature Commun, 2018, 9 (1): 1- 13. |
| 3 | TOYAMA Y , KANO H , MASE Y , et al. Dynamic regulation of GDP binding to g proteins revealed by magnetic field-dependent NMR relaxation analyses[J]. Nature Commun, 2017, 8 (1): 1- 15. |
| 4 | HUANG Y Q , ZHAN H L , YOU X Q , et al. A pure shift-based NMR method for transverse relaxation measurements on complex samples[J]. IEEE Trans Instrum Meas, 2020, 69 (1): 201- 211. |
| 5 | DU G F , LIN J , ZHANG J , et al. Study on shortening the dead time of surface nuclear magnetic resonance instrument using bipolar phase pulses[J]. IEEE Trans Instrum Meas, 2020, 69 (4): 1268- 1274. |
| 6 | FU R Q , MIAO Y M , QIN H J , et al. Probing hydronium ion histidine NH exchange rate constants in the m2 channel via indirect observation of dipolar-dephased 15N signals in magic-angle-spinning NMR[J]. J Amer Chem Soc, 2016, 138 (49): 15801- 15804. |
| 7 | FRYDMAN L , SCHERF T , LUPULESCU A . The acquisition of multidimensional NMR spectra within a single scan[J]. Proc Nat Acad Sci USA, 2020, 99 (25): 15858- 15862. |
| 8 | CHEN X L , LV W , SU Q C . Conversion of lignocellulose studied by nuclear magnetic resonance[J]. Chinese J Magn Reson, 2021, 38 (2): 277- 290. |
| 8 | 陈晓丽, 吕微, 苏秋成, 等. 核磁共振技术在生物质转化中的应用[J]. 波谱学杂志, 2021, 38 (2): 277- 290. |
| 9 | ZANGGER K . Pure shift NMR[J]. Prog Nucl Magn Reson Spectrosc, 2015, 86-87, 1- 20. |
| 10 | ZHOU Q J , XIANG J F , TANG Y L , et al. Pure shift proton NMR spectroscopy and its application[J]. Chinese J Magn Reson, 2016, 33 (3): 502- 513. |
| 10 | 周秋菊, 向俊峰, 唐亚林, 等. 纯位移核磁共振氢谱及其应用[J]. 波谱学杂志, 2016, 33 (3): 502- 513. |
| 11 | LIN X Q , LI H , ZHAN H L , et al. High-resolution pure shift NMR spectroscopy and its applications[J]. Chinese J Magn Reson, 2019, 36 (4): 425- 436. |
| 11 | 林晓晴, 李弘, 詹昊霖, 等. 高分辨率核磁共振纯化学位移谱新方法及其应用[J]. 波谱学杂志, 2019, 36 (4): 425- 436. |
| 12 | HUNG I , GAN Z H . High-resolution NMR of S=3/2 quadrupole nuclei by detection of double-quantum satellite transitions via protons[J]. J Phys Chem Lett, 2020, 11 (12): 4734- 4740. |
| 13 | BIFULCO G , DAMBRUOSO P , GOMEZ-PALOMA L , et al. Determination of relative configuration in organic compounds by NMR spectroscopy and computational methods[J]. Chem Rev, 2007, 107 (9): 3744- 3779. |
| 14 | THOMAS W A . Unravelling molecular structure and conformation-the modern role of coupling constants[J]. Prog Nucl Magn Reson Spectrosc, 1997, 30, 183- 207. |
| 15 | REIF B , HENNIG M , GRIESINGER C . Direct measurement of angles between bond vectors in high-resolution NMR[J]. Science, 1997, 276 (5316): 1230- 1233. |
| 16 | LI Y J , YANG H J , LIU J H , et al. Assignments of NMR spectral data of a novel carbazole-triazinoindole based N-acylhydrazone derivative[J]. Chinese J Magn Reson, 2020, 37 (4): 496- 504. |
| 16 | 李英俊, 杨鸿境, 刘季红, 等. 基于咔唑-三嗪并吲哚的N-酰腙衍生物的NMR数据归属[J]. 波谱学杂志, 2020, 37 (4): 496- 504. |
| 17 | AUE W P , KARHAN J , ERNST R R . Homonuclear broad band decoupling and two-dimensional J-resolved NMR spectroscopy[J]. J Chem Phys, 1976, 64, 4226- 4227. |
| 18 | KIKUCHI J , TSUBOI Y , KOMATSU K , et al. Spin couple: development of a web tool for analyzing metabolite mixtures via two-dimensional J-resolved NMR database[J]. Anal Chem, 2016, 88 (1): 659- 665. |
| 19 | LUPULESCU A , AHARON H , FRYDMAN L . Two-dimensional RF pulses: A new approach to selectively exciting J-coupled spins in nuclear magnetic resonance[J]. J Chem Phys, 2013, 139 (14): 144204. |
| 20 | ESPINDOLA A P D M , CROUCH R , DEBERGH J R , et al. Deconvolution of complex NMR spectra in small molecules by multi frequency homonuclear decoupling (MDEC)[J]. J Amer Chem Soc, 2009, 131 (44): 15994- 15995. |
| 21 | YILMAZ A , NYBERG N T , JAROSZEWSKI J W . Metabolic profiling based on two-dimensional J-resolved 1H NMR data and parallel factor analysis[J]. Anal Chem, 2011, 83 (21): 8278- 8285. |
| 22 | LUDWIG C , VIANT M R . Two-dimensional J-resolved NMR spectroscopy: review of a key methodology in the metabolomics toolbox[J]. Phytochem Anal, 2010, 21 (1): 22- 32. |
| 23 | RACHINENI K , KAKITA V M R , DAYAKA S , et al. Precise determination of enantiomeric excess by a sensitivity enhanced two-dimensional band-selective pure-shift NMR[J]. Anal Chem, 2015, 87 (14): 7258- 7266. |
| 24 | KIRALY P , FOROOZANDEH M , NILSSON M , et al. Anatomising proton NMR spectra with pure shift 2D J-spectroscopy: A cautionary tale[J]. Chem Phys Lett, 2017, 683, 398- 403. |
| 25 | BAX A , FREEMAN R , MORRIS G A . A simple method for suppressing dispersion-mode contributions in NMR spectra: The "pseudo echo"[J]. J Magn Reson, 1981, 43 (2): 333- 338. |
| 26 | ARMSTRONG G S , CHEN J H , CANO K E , et al. Regularized resolvent transform for direct calculation of 45° projections of 2D J spectra[J]. J Magn Reson, 2003, 164 (1): 136- 144. |
| 27 | CHEN J H , SHAKA A J , MANDELSHTAM V A . RRT: The regularized resolvent transform for high-resolution spectral estimation[J]. J Magn Reson, 2000, 147 (1): 129- 137. |
| 28 | MANDELSHTAM V A , TAYLOR H S , SHAKA A J . Application of the filter diagonalization method to one- and two-dimensional NMR spectra[J]. J Magn Reson, 1998, 133 (2): 304- 312. |
| 29 | HU H T , DE ANGELIS A A , MANDELSHTAM V A , et al. The multidimensional filter diagonalization method - Ⅱ. Application to 2D projections of 2D, 3D, and 4D NMR experiments[J]. J Magn Reson, 2000, 144 (2): 357- 366. |
| 30 | KEELER J , NEUHAUS D . Comparison and evaluation of methods for two-dimensional NMR spectra with absorption-mode lineshapes[J]. J Magn Reson, 1985, 63 (3): 454- 472. |
| 31 | ZANGGER K , STERK H . Homonuclear broadband-decoupled NMR spectra[J]. J Magn Reson, 1997, 124 (2): 486- 489. |
| 32 | PELL A J , KEELER J . Two-dimensional J-spectra with absorption-mode lineshapes[J]. J Magn Reson, 2007, 189 (2): 293- 299. |
| 33 | MISHRA S K , LOKESH N , SURYAPRAKASH N . Clean G-SERF an NMR experiment for the complete eradication of axial peaks and undesired couplings from the complex spectrum[J]. RSC Adv, 2017, 7 (2): 735- 741. |
| 34 | LOKESH N , CHAUDHARI S R , SURYAPRAKASH N . Quick re-introduction of selective scalar interactions in a pure-shift NMR spectrum[J]. Chem Commun, 2014, 50 (98): 15597- 15600. |
| 35 | FOROOZANDEH M , ADAMS R W , MEHARRY N J , et al. Ultrahigh-resolution NMR spectroscopy[J]. Angew Chem Int Ed, 2014, 53 (27): 6990- 6992. |
| 36 | FOROOZANDEH M , ADAMS R W , KIRALY P , et al. Measuring couplings in crowded NMR spectra: pure shift NMR with multiplet analysis[J]. Chem Commun, 2015, 51 (84): 15410- 15413. |
| 37 | SINNAEVE D , FOROOZANDEH M , NILSSON M , et al. A general method for extracting individual coupling constants from crowded 1H NMR spectra[J]. Angew Chem Int Ed, 2016, 55 (3): 1090- 1093. |
| 38 | SINNAEVE D . Clean pure shift 2D J-resolved spectroscopy[J]. Magn Reson Chem, 2018, 56 (10): 947- 953. |
| 39 | NAGAYAMA K . Spin decoupling in two-dimensional J-resolved NMR spectroscopy[J]. J Chem Phys, 1979, 71, 4404- 4415. |
| 40 | THRIPPLETON M J , EDDEN R A E , KEELER J . Suppression of strong coupling artefacts in J-spectra[J]. J Magn Reson, 2005, 174 (1): 97- 109. |
| 41 | GAL M , MISHKOVSKY M , FRYDMAN L . Real-time monitoring of chemical transformations by ultrafast 2D NMR spectroscopy[J]. J Amer Chem Soc, 2006, 128 (3): 951- 956. |
| 42 | VIANT M R . Improved methods for the acquisition and interpretation of NMR metabolomic data[J]. Biochem Biophys Res Commun, 2003, 310 (3): 943- 948. |
| 43 | TAL A , FRYDMAN L . Single-scan multidimensional magnetic resonance[J]. Prog Nucl Magn Reson Spectrosc, 2010, 57 (3): 241- 292. |
| 44 | HUANG Y Q , YANG Y , CAI S H . General two-dimensional absorption-mode J?resolved NMR spectroscopy[J]. Anal Chem, 2017, 89 (23): 12646- 12651. |
| 45 | PELUPESSY P , RENNELLA E , BODENHAUSEN G . High-resolution NMR in magnetic fields with unknown spatiotemporal variations[J]. Science, 2009, 324 (5935): 1693- 1697. |
| 46 | FUGARIU I , BERMEL W , LANE D , et al. In-phase ultra high-resolution in vivo NMR[J]. Angew Chem Int Ed, 2017, 56 (22): 6324- 6328. |
| 47 | ZHAN H L , HUANG Y Q , CHEN Z . An orthogonal-pattern absorption-mode 2D J-resolved NMR spectroscopy for analyses on complex samples[J]. IEEE Trans Instrum Meas, 2021, 70, 6004509. |
| 48 | FACKE T , BERGER S . SERF, a new method for H, H spin-coupling measurement in organic chemistry[J]. J Magn Reson Ser A, 1995, 113 (1): 114- 116. |
| 49 | GIRAUD N , BEGUIN L , COURTIEU J , et al. Nuclear magnetic resonance using a spatial frequency encoding: application to J-edited spectroscopy along the sample[J]. Angew Chem Int Ed, 2010, 49 (20): 3481- 3484. |
| 50 | MISHRA S K , LOKESH N , SURYAPRAKASH N . Clean G-SERF an NMR experiment for the complete eradication of axial peaks and undesired couplings from the complex spectrum[J]. RSC Adv, 2017, 7 (2): 735- 741. |
| 51 | LIN L J , WEI Z L , LIN Y Q , et al. Measuring JHH values with a selective constant-time 2D NMR protocol[J]. J Magn Reson, 2016, 272, 20- 24. |
| 52 | CHEN J Y , ZENG Q , LIN Y Q , et al. Simultaneous multi-slice selective constant-time J-resolved spectroscopy for measuring J values[J]. Chinese J Magn Reson, 2019, 36 (4): 456- 462. |
| 52 | 陈金永, 曾庆, 林雁勤, 等. 用于测量J偶合常数的同时多层选择性恒时J分解谱的方法[J]. 波谱学杂志, 2019, 36 (4): 456- 462. |
| 53 | ZHAN H L , HUANG Y Q , WANG X C , et al. Highly efficient determination of complex NMR multiplet structures in inhomogeneous magnetic fields[J]. Anal Chem, 2021, 93, 2419- 2423. |
| 54 | PELUPESSY P , RENNELLA E , BODENHAUSEN G . High-resolution NMR in magnetic fields with unknown spatiotemporal variations[J]. Science, 2009, 324 (5935): 1693- 1697. |
| 55 | GAN Z H , HUNG I , WANG X L , et al. NMR spectroscopy up to 35.2 T using a series-connected hybrid magnet[J]. J Magn Reson, 2017, 284, 125- 136. |
| 56 | LAMBERT J , HERGENRODER R , SUTER D , et al. Probing liquid-liquid interfaces with spatially resolved NMR spectroscopy[J]. Angew Chem Int Ed, 2009, 48 (34): 6343- 6345. |
/
| 〈 |
|
〉 |