Design, construction, and validation of a 1-mm triple-resonance high-temperature-superconducting probe for NMR
Design, construction, and validation of a 1-mm triple-resonance high-temperature-superconducting probe for NMR
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DOI：
10.1016/j.jmr.2005.12.008
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发表时间：
2006-04-01
影响因子：
2.2
通讯作者：
Withers, RS
中科院分区：
文献类型：
--
作者：
Brey, WW;Edison, AS;Withers, RS
我们报告了一种用于核磁共振波谱的 600 MHz 1 mm 三重共振高温超导 (HTS) 探头。该探针的实际样品体积约为 7.5 μl，有效体积为 6.3 μl，并且在任何场强下似乎都具有最高的质量灵敏度。该探头由四组 HTS 线圈构成，调谐为 H-1、H-2、C-13 和 N-15，并且存在 z 轴梯度。使用传统的 Bruker CryoPlatform 将线圈冷却至约 20 K，并且可以使用 Bruker 可变温度装置在适度范围内将样品室调节到高于或低于室温。 0.1% 乙苯的绝对信噪比约为传统 5 mm 探头的 1/3，而样品体积仅为 1/70。我们通过仅 1.7 μg 布洛芬和 400 μM N-15 标记的泛素的 2D 光谱证明了该探针对小分子和蛋白质的实用性。 (c) 2006 Elsevier Inc. 保留所有权利。
We report a 600-MHz 1-mm triple-resonance high-temperature-superconducting (HTS) probe for nuclear magnetic resonance spectroscopy. The probe has a real sample volume of about 7.5 mu l, an active volume of 6.3 mu l, and appears to have the highest mass sensitivity at any field strength. The probe is constructed with four sets of HTS coils that are tuned to H-1 H-2, C-13, and N-15, and there is a z-axis gradient. The coils are cooled with a conventional Bruker CryoPlatform to about 20 K, and the sample chamber can be regulated above or below room temperature over a moderate range using a Bruker variable temperature unit. The absolute S/N for 0.1% ethylbenzene is approximately 1/3 that of a conventional 5 mm probe With just 1/70 of the sample volume. We demonstrate the utility of this probe for small molecules and proteins with 2D spectra of just 1.7 mu g of ibuprofen and 400 mu M N-15-labeled ubiquitin. (c) 2006 Elsevier Inc. All rights reserved.