Sensitivity enhancement in solid state 15N NMR by indirect detection with high-speed magic angle spinning

被引:225
作者
Ishii, Y [1 ]
Tycko, R [1 ]
机构
[1] NIDDKD, Chem Phys Lab, NIH, Bethesda, MD 20892 USA
关键词
solid state NMR; magic angle spinning; indirect detection; nitrogen-15; NMR; peptides;
D O I
10.1006/jmre.1999.1976
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Enhancement of sensitivity in solid state N-15 NMR by indirect detection through H-1 NMR signals under high-speed magic angle spinning and high-field conditions is demonstrated experimentally on two N-15-labeled peptides, polycrystalline AlaGlyGly and the helix-forming, 17-residue peptide MB(i + 4)EK in lyophilized form. Sensitivity enhancement factors ranging from 2.0 to 3.2 are observed experimentally, depending on the (1)5N and H-1 linewidths and polarization transfer efficiencies. The H-1-detected two-dimensional H-1/N-15 correlation spectrum of AlaGlyGly illustrates the possibility of increased spectral resolution and resonance assignments in indirectly detected experiments, in addition to the sensitivity enhancement.
引用
收藏
页码:199 / 204
页数:6
相关论文
共 41 条
[1]  
Abragam A., 1961, PRINCIPLES NUCL MAGN
[2]   BROAD-BAND POLARIZATION-TRANSFER EXPERIMENTS FOR ROTATING SOLIDS [J].
BALDUS, M ;
TOMASELLI, M ;
MEIER, BH ;
ERNST, RR .
CHEMICAL PHYSICS LETTERS, 1994, 230 (4-5) :329-336
[3]   CORRELATION OF PROTON AND N-15 CHEMICAL-SHIFTS BY MULTIPLE QUANTUM NMR [J].
BAX, A ;
GRIFFEY, RH ;
HAWKINS, BL .
JOURNAL OF MAGNETIC RESONANCE, 1983, 55 (02) :301-315
[4]   Quantitative conformational measurements in solid state NMR by constant-time homonuclear dipolar recoupling [J].
Bennett, AE ;
Weliky, DP ;
Tycko, R .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1998, 120 (19) :4897-4898
[5]   Homonuclear radio frequency-driven recoupling in rotating solids [J].
Bennett, AE ;
Rienstra, CM ;
Griffiths, JM ;
Zhen, WG ;
Lansbury, PT ;
Griffin, RG .
JOURNAL OF CHEMICAL PHYSICS, 1998, 108 (22) :9463-9479
[6]   CHEMICAL-SHIFT CORRELATION SPECTROSCOPY IN ROTATING SOLIDS - RADIO FREQUENCY-DRIVEN DIPOLAR RECOUPLING AND LONGITUDINAL EXCHANGE [J].
BENNETT, AE ;
OK, JH ;
GRIFFIN, RG ;
VEGA, S .
JOURNAL OF CHEMICAL PHYSICS, 1992, 96 (11) :8624-8627
[7]   NUCLEAR MAGNETIC RESONANCE IN THE CESIUM HALIDES [J].
BLOEMBERGEN, N ;
SOROKIN, PP .
PHYSICAL REVIEW, 1958, 110 (04) :865-875
[8]   NATURAL ABUNDANCE N-15 NMR BY ENHANCED HETERONUCLEAR SPECTROSCOPY [J].
BODENHAUSEN, G ;
RUBEN, DJ .
CHEMICAL PHYSICS LETTERS, 1980, 69 (01) :185-189
[9]  
Ernst R. R., 1987, PRINCIPLES NUCL MAGN, P148
[10]   Solid-state nuclear magnetic resonance spectra of dipolar-coupled multi-spin systems under fast magic angle spinning [J].
Filip, C ;
Hafner, S ;
Schnell, I ;
Demco, DE ;
Spiess, HW .
JOURNAL OF CHEMICAL PHYSICS, 1999, 110 (01) :423-440