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Structure-Correlation NMR Spectroscopy for Macromolecules Using Repeated Bidirectional Photoisomerization of Azobenzene
Analytical Chemistry ( IF 6.7 ) Pub Date : 2015-10-27 00:00:00 , DOI: 10.1021/acs.analchem.5b03427 Toshio Nagashima 1 , Keisuke Ueda 1 , Chiaki Nishimura 2 , Toshio Yamazaki 1
Analytical Chemistry ( IF 6.7 ) Pub Date : 2015-10-27 00:00:00 , DOI: 10.1021/acs.analchem.5b03427 Toshio Nagashima 1 , Keisuke Ueda 1 , Chiaki Nishimura 2 , Toshio Yamazaki 1
Affiliation
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Control over macromolecular structure offers bright potentials for manipulation of macromolecular functions. We here present structure-correlation NMR spectroscopy to analyze the correlation between polymorphic macromolecular structures driven by photoisomerization of azobenzene. The structural conversion of azobenzene was induced within the mixing time of a NOESY experiment using a colored light source, and the reverse structural conversion was induced during the relaxation delay using a light source of another color. The correlation spectrum between trans- and cis-azobenzene was then obtained. To maximize the efficiency of the bidirectional photoisomerization of azobenzene-containing macromolecules, we developed a novel light-irradiation NMR sample tube and method for irradiating target molecules in an NMR radio frequency (rf) coil. When this sample tube was used for photoisomerization of an azobenzene derivative at a concentration of 0.2 mM, data collection with reasonable sensitivity applicable to macromolecules was achieved. We performed isomerization of an azobenzene-cross-linked peptide within the mixing time of a NOESY experiment that produced cross-peaks between helix and random-coil forms of the peptide. Thus, these results indicate that macromolecular structure manipulation can be incorporated into an NMR pulse sequence using an azobenzene derivative and irradiation with light of two types of wavelengths, providing a new method for structural analysis of metastable states of macromolecules.
中文翻译：
大分子的结构相关核磁共振波谱使用偶氮苯的双向双向光异构化
对大分子结构的控制为操纵大分子功能提供了广阔的前景。我们在这里提出结构相关的核磁共振波谱，以分析由偶氮苯的光异构化驱动的多晶型大分子结构之间的相关性。在有色光源的NOESY实验的混合时间内，引发了偶氮苯的结构转化，在弛豫延迟期间，使用了另一种颜色的光源，诱导了反向结构转化。反式与顺式的相关谱。然后获得-偶氮苯。为了最大程度地提高含偶氮苯的大分子的双向光异构化效率，我们开发了一种新型的光辐射NMR样品管和在NMR射频（rf）线圈中辐照目标分子的方法。当将该样品管用于浓度为0.2 mM的偶氮苯衍生物的光异构化时，可获得适用于大分子的具有合理灵敏度的数据收集。我们在NOESY实验的混合时间内进行了偶氮苯交联肽的异构化，该实验在肽的螺旋和无规螺旋形式之间产生了交叉峰。因此，
更新日期：2015-10-27
中文翻译：
大分子的结构相关核磁共振波谱使用偶氮苯的双向双向光异构化
对大分子结构的控制为操纵大分子功能提供了广阔的前景。我们在这里提出结构相关的核磁共振波谱，以分析由偶氮苯的光异构化驱动的多晶型大分子结构之间的相关性。在有色光源的NOESY实验的混合时间内，引发了偶氮苯的结构转化，在弛豫延迟期间，使用了另一种颜色的光源，诱导了反向结构转化。反式与顺式的相关谱。然后获得-偶氮苯。为了最大程度地提高含偶氮苯的大分子的双向光异构化效率，我们开发了一种新型的光辐射NMR样品管和在NMR射频（rf）线圈中辐照目标分子的方法。当将该样品管用于浓度为0.2 mM的偶氮苯衍生物的光异构化时，可获得适用于大分子的具有合理灵敏度的数据收集。我们在NOESY实验的混合时间内进行了偶氮苯交联肽的异构化，该实验在肽的螺旋和无规螺旋形式之间产生了交叉峰。因此，
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