Optimization of pulsed DEER measurements for Gd-based labels: choice of operational frequencies, pulse durations and positions, and temperature.

Optimization of pulsed DEER measurements for Gd-based labels: choice of operational frequencies, pulse durations and positions, and temperature.
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DOI:
10.1007/s00723-012-0434-6
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发表时间:
2013-06
影响因子:
1
通讯作者:
Meade, T. J.
Meade, T. J.
中科院分区:
物理与天体物理4区
文献类型:
--
作者:
Raitsimring, A.;Astashkin, A. V.;Enemark, J. H.;Kaminker, I.;Goldfarb, D.;Walter, E. D.;Song, Y.;Meade, T. J.

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本文分析了Gd(III)标记生物大分子远距离(≥ 60 nm)双电子-电子共振(DEER)测量所需的实验条件和参数。讨论的具体参数是温度,微波波段,泵浦和观察频率之间的分离,脉冲串重复率,脉冲持续时间和脉冲定位在电子顺磁共振谱。结果发现:(i)在优化的DEER测量中,观测脉冲必须在EPR谱的最大值处施加;(ii)Ka波段测量的最佳温度范围为14-17 K,而在W波段中,最佳温度在6-9 K之间;(iii)对于DEER测量,W波段优于Ka波段。本文还简要地讨论了最近的成就和短距离测量(<15 μ m)所需的条件。
In this work, the experimental conditions and parameters necessary to optimize the long-distance (≥ 60 Å) Double Electron-Electron Resonance (DEER) measurements of biomacromolecules labeled with Gd(III) tags are analyzed. The specific parameters discussed are the temperature, microwave band, the separation between the pumping and observation frequencies, pulse train repetition rate, pulse durations and pulse positioning in the electron paramagnetic resonance spectrum. It was found that: (i) in optimized DEER measurements, the observation pulses have to be applied at the maximum of the EPR spectrum; (ii) the optimal temperature range for Ka-band measurements is 14–17 K, while in W-band the optimal temperatures are between 6–9 K; (iii) W-band is preferable to Ka-band for DEER measurements. Recent achievements and the conditions necessary for short-distance measurements (<15 Å) are also briefly discussed.
DOI: 10.1006/jmre.1999.1988
发表时间: 2000-04-01
影响因子: 2.2
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