Proton micro-magic-angle-spinning NMR spectroscopy of nanoliter samples

被引：17

作者：

Brinkmann, Andreas ^{[1
,2
]}

Vasa, Suresh Kumar ^{[2
]}

Janssen, Hans ^{[2
]}

Kentgens, Arno P. M. ^{[2
]}

机构：

[1] CNR, Steacie Inst Mol Sci, Ottawa, ON K1A 0R6, Canada

[2] Radboud Univ Nijmegen, Inst Mol & Mat, Phys Chem Solid State NMR, NL-6500 GL Nijmegen, Netherlands

来源：

CHEMICAL PHYSICS LETTERS | 2010年 / 485卷 / 4-6期

关键词：

SOLID-STATE NMR; NUCLEAR-MAGNETIC-RESONANCE; MULTIPLE-PULSE SEQUENCES; HIGH-RESOLUTION; MAS NMR; CROSS-POLARIZATION; NATURAL-ABUNDANCE; INVERSE DETECTION; ROTATING SOLIDS; BOND;

D O I：

10.1016/j.cplett.2009.12.054

中图分类号：

O64 [物理化学（理论化学）、化学物理学];

学科分类号：

070304 ; 081704 ;

摘要：

We present our recent progress in the development of micro-magic-angle-spinning solenoid-based probeheads for the application in high-resolution (1)H solid-state NMR of nanoliter sample volumes. The use of fused-silica capillaries as sample holders results in spectra without any 1H background signal. It is possible to obtain (1)H spectra of 40-80 nl samples in a few scans. We obtained high-resolution (1)H spectra employing different homonuclear decoupling sequences on powdered samples of L-alanine, the tripeptide AGG, and a single crystal of L-tyrosine center dot HCl. In addition, we recorded high-resolution two-dimensional proton-detected (1)H-(13)C heteronuclear correlation spectra of [U-(13)C(3), (15)N]-L-alanine and AGG with natural abundant isotope distribution. Crown Copyright (C) 2009 Published by Elsevier B.V. All rights reserved.

引用

页码：275 / 280

页数：6

共 48 条

[1]

ASHIDA J, 1996, MAGN MOMENTS, V8, P19

[2] FREQUENCY-SWITCHED PULSE SEQUENCES - HOMONUCLEAR DECOUPLING AND DILUTE SPIN NMR IN SOLIDS [J].

BIELECKI, A ;

KOLBERT, AC ;

LEVITT, MH .

CHEMICAL PHYSICS LETTERS, 1989, 155 (4-5) :341-346

[3] Probing proton-proton proximities in the solid state [J].

Brown, Steven P. .

PROGRESS IN NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY, 2007, 50 (04) :199-251

[4] Recent Advances in Solid-State MAS NMR Methodology for Probing Structure and Dynamics in Polymeric and Supramolecular Systems [J].

Brown, Steven P. .

MACROMOLECULAR RAPID COMMUNICATIONS, 2009, 30 (9-10) :688-716

[5] Indirect detection of nitrogen-14 in solids via protons by nuclear magnetic resonance spectroscopy [J].

Cavadini, Simone ;

Antonijevic, Sasa ;

Lupulescu, Adonis ;

Bodenhausen, Geoffrey .

JOURNAL OF MAGNETIC RESONANCE, 2006, 182 (01) :168-172

[6] Simple and efficient decoupling in magic-angle spinning solid-state NMR: the XiX scheme [J].

Detken, A ;

Hardy, EH ;

Ernst, M ;

Meier, BH .

CHEMICAL PHYSICS LETTERS, 2002, 356 (3-4) :298-304

[7] Direct spectral optimisation of proton-proton homonuclear dipolar decoupling in solid-state NMR [J].

Elena, B ;

de Paëpe, G ;

Emsley, L .

CHEMICAL PHYSICS LETTERS, 2004, 398 (4-6) :532-538

[8] Electromagnetic wave compression and radio frequency homogeneity in NMR solenoidal coils: Computational approach [J].

Engelke, F .

CONCEPTS IN MAGNETIC RESONANCE, 2002, 15 (02) :129-155

[9] 13C NMR of liquid crystals with different proton homonuclear dipolar decoupling methods [J].

Fung, BM ;

Ermolaev, K ;

Yu, YL .

JOURNAL OF MAGNETIC RESONANCE, 1999, 138 (01) :28-35

[10] Proton-detected 14N MAS NMR using homonuclear decoupled rotary resonance [J].

Gan, Zhehong ;

Amoureux, Jean Paul ;

Trebosc, Julien .

CHEMICAL PHYSICS LETTERS, 2007, 435 (1-3) :163-169

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