A proton and carbon 13 nuclear magnetic resonance study of neomycin B and its interactions with phosphatidylinositol 4,5-bisphosphate.
A proton and carbon 13 nuclear magnetic resonance study of neomycin B and its interactions with phosphatidylinositol 4,5-bisphosphate.
复制标题
新霉素 B 及其与磷脂酰肌醇 4,5-二磷酸相互作用的质子和碳 13 核磁共振研究。
DOI：
10.1016/s0021-9258(18)47512-6
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发表时间：
1987
期刊：
影响因子：
--
通讯作者：
K. Gajjar
中科院分区：
文献类型：
--
作者：
D. Reid;K. Gajjar
氨基糖苷类抗生素新霉素B的整个质子核磁共振谱已被指定在生理pH值的组合的二维J-分辨和J-相关和核欧沃豪泽增强差谱。通过观察环之间和环内的核奥弗豪泽增强，可以在不求助于模型或衍生化合物的情况下，对所有四个环系统进行无敌意的分配。随后的碳13光谱的分配是简单地实现使用二维异质结J相关技术。首次报道了细胞内第二信使前体磷脂酰肌醇4，5-二磷酸的超声水分散液的质子NMR谱。该光谱与高度侧链不饱和度和肌醇头部基团的构象一致，该头部基团表现出高度移动的，其中所有大体积取代基均为平伏的（2-羟基除外）。向新霉素B的缓冲水溶液中加入等份的磷脂酰肌醇4，5-二磷酸盐，会引起后者整个光谱的复杂变化，包括几个分辨良好的信号（即端基异构体）和取代环己烷的亚甲基质子对的微分幅度的低场位移。络合动力学在25 ° C下在NMR时间标度上是快速的。结合的结果进行了讨论，在一个试探性的络合几何。
The entire proton NMR spectrum of the aminoglycoside antibiotic neomycin B has been assigned at physiological pH by a combination of two-dimensional J-resolved and J-correlated and nuclear Overhauser enhancement difference spectroscopy. Unambiguous assignment of all four ring systems is possible without recourse to model or derivative compounds by observing nuclear Overhauser enhancements between as well as within rings. The subsequent assignment of the carbon 13 spectrum is simply achieved using two-dimensional heteronuclear J-correlated techniques. The proton NMR spectrum of a sonicated aqueous dispersion of the intracellular second messenger precursor phosphatidylinositol 4,5-bisphosphate is reported for the first time. The spectrum is consistent with a high degree of side chain unsaturation and a conformation for the myo-inositol head group, which appears highly mobile, in which all bulky substituents are equatorial (except the 2-hydroxyl). Addition of aliquots of phosphatidylinositol 4,5-bisphosphate to an aqueous buffered solution of neomycin B induces complex changes in the whole spectrum of the latter, including downfield shifts of differential magnitude for several well-resolved signals, viz. the anomerics, and the pair of methylene protons of the substituted cyclohexane. The complexation kinetics are fast on the NMR time scale at 25 degrees C. The binding results are discussed in terms of a tentative complexation geometry.