Sensitivity enhancement in solid state 15N NMR by indirect detection with high-speed magic angle spinning
Sensitivity enhancement in solid state 15N NMR by indirect detection with high-speed magic angle spinning
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DOI：
10.1006/jmre.1999.1976
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发表时间：
2000-01-01
影响因子：
2.2
通讯作者：
Tycko, R
中科院分区：
文献类型：
--
作者：
Ishii, Y;Tycko, R
在高速魔角旋转和高场条件下，通过氢 - 1核磁共振信号间接检测来提高固态氮 - 15核磁共振的灵敏度，这在两种氮 - 15标记的肽上进行了实验验证，即多晶丙氨酰甘氨酰甘氨酸以及冻干形式的形成螺旋的17个残基的肽MB(i + 4)EK。根据氮 - 15和氢 - 1的线宽以及极化转移效率，实验观察到的灵敏度增强因子在2.0到3.2之间。丙氨酰甘氨酰甘氨酸的氢 - 1检测的二维氢 - 1/氮 - 15相关谱表明，除了灵敏度提高之外，在间接检测实验中还可能提高光谱分辨率和进行共振归属。
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.