The measurement of heteronuclear transverse relaxation times in ax3 spin systems via polarization-transfer techniques

Lewis E Kay , T.E Bull , L.K Nicholson , C Griesinger , H Schwalbe , A Bax , D.A Torchia
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引用次数: 60

Abstract

Pulse schemes for the measurement of 13C transverse relaxation times in AX33 spin systems are described which make use of the sensitive 1H spin for detection. The experiments are based on reverse-DEPT and reverse-INEPT polarization-transfer sequences. It is shown that relaxation rates obtained from 13C-direct-observe and from polarization-transfer experiments are identical only if magnetization from each of the 13C transitions is transferred equally to the detected 1H spins. This requires judicious choices in pulse angles and delays in reverse-DEPT and reverse-INEPT experiments. For application to macromolecules, experimental and theoretical results suggest that polarization-transfer schemes based on reverse INEPT are superior to reverse-DEPT-based sequences and give results which are in good agreement with values measured via 13C-observe methods.

用极化转移技术测量轴3自旋系统中的异核横向弛豫时间
描述了AX33自旋系统中测量13C横向弛豫时间的脉冲方案,该方案利用敏感的1H自旋进行检测。实验基于反向dept和反向inept极化转移序列。结果表明,只有当每个13C跃迁的磁化强度相等地转移到探测到的1H自旋上时,直接观测得到的弛豫率和极化转移实验得到的弛豫率是相同的。这需要在反向dept和反向inept实验中明智地选择脉冲角度和延迟。对于大分子,实验和理论结果表明,基于反向INEPT的极化转移方案优于基于反向dept的序列,其结果与13c -观测方法的测量值吻合良好。
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