Department of Chemistry, University of Southern California, Los Angeles, CA, USA.
Biophys J. 2010 Oct 6;99(7):2180-9. doi: 10.1016/j.bpj.2010.08.005.
In this report, stereospecific structural and dynamic features in DNA are studied using the site-directed spin labeling technique. A stable nitroxide radical, 1-oxyl-4-bromo-2,2,5,5-tetramethylpyrroline (R5a), was attached postsynthetically to phosphorothioates that were chemically introduced, one at a time, at five sites of a DNA duplex. The two phosphorothioate diastereomers (R(p) or S(p)) were separated, and nitroxide rotational motions were monitored using electron paramagnetic resonance spectroscopy. The resulting spectra vary according to diastereomer identity and location of the labeling site, with R(p)-R5a spectra effectively reporting on local DNA structural features and S(p)-R5a spectra sensing variations in local DNA motions. This establishes R(p)- and S(p)-R5a as unique probes for investigating nucleic acids in a site- and stereospecific manner, which may aid studies of stereospecific DNA/protein interactions. In addition, weighted averages of individual R(p) and S(p) spectra match those of R5a attached to mixed diastereomers. This suggests that R5a linked to mixed diastereomers reports on the composite behaviors of R(p)- and S(p)-R5a and is useful in initial probing of the DNA local environment. This work advances understanding of R5a/DNA coupling, and is a key step forward in developing a nucleotide-independent spectroscopic probe for studying nucleic acids.
在本报告中,使用定点自旋标记技术研究了 DNA 中的立体特异性结构和动态特征。一种稳定的氮氧自由基,1-氧代-4-溴-2,2,5,5-四甲基吡咯烷(R5a),在化学上逐个引入 DNA 双链体的五个位置的硫代磷酸酯后被附着。两种硫代磷酸酯非对映异构体(R(p)或 S(p))被分离,并用电子顺磁共振波谱法监测氮氧化物的旋转运动。所得光谱根据非对映异构体的身份和标记位置的不同而变化,其中 R(p)-R5a 光谱有效地报告局部 DNA 结构特征,而 S(p)-R5a 光谱则检测局部 DNA 运动的变化。这确立了 R(p)-和 S(p)-R5a 作为以位点和立体特异性方式研究核酸的独特探针,这可能有助于研究立体特异性 DNA/蛋白质相互作用。此外,单个 R(p)和 S(p)光谱的加权平均值与连接到混合非对映异构体的 R5a 的光谱相匹配。这表明连接到混合非对映异构体的 R5a 报告 R(p)-和 S(p)-R5a 的复合行为,并且在初始探测 DNA 局部环境时很有用。这项工作推进了对 R5a/DNA 偶联的理解,并且是开发用于研究核酸的核苷酸独立光谱探针的关键一步。