氧化石墨烯-环戊胺(GO-d-CP)液晶作为分析物回收的各向异性核磁共振新取向介质

IF 6.1 Q1 CHEMISTRY, MULTIDISCIPLINARY
Sandesh Chickmagalur Jatheendranath, Akhi Das, Sudhindra H Deshpande, Nilamoni Nath, Walter Maier, Verena Streitferdt, Udaya Kiran Marelli
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引用次数: 0

摘要

在这项研究中,我们提出了氧化石墨烯与环戊胺衍生(GO-d-CP)作为dmso兼容的液晶取向介质,不受任何背景核磁共振信号的影响,用于各向异性核磁共振。这种新型对准介质在单样品制备过程中实现了最佳的各向同性和各向异性条件,通过超声控制,从而实现了各向异性核磁共振参数的测量-残余偶极耦合(RDC)和残余化学位移各向异性(RCSA)。GO-d-CP具有几个优点,包括易于合成,固体GO-d-CP作为稳定的非吸湿性材料的分离,以及保持各向异性状态稳定性(30天),允许长时间和重复实验。值得注意的是,在分析后,它可以很容易地回收有价值的分析物以及GO-d-CP进行再利用,使各向异性核磁共振在小分子结构分析中的常规应用成为可能。我们利用各向异性核磁共振数据分析了四种化合物——雌酮、桑托宁、灰黄霉素和辛甲基林的相对立体化学,证明了它的有效性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Graphene Oxide-Cyclopentylamine (GO-d-CP) Liquid Crystals as a Novel Alignment Medium for Anisotropic NMR with Analyte Recovery

Graphene Oxide-Cyclopentylamine (GO-d-CP) Liquid Crystals as a Novel Alignment Medium for Anisotropic NMR with Analyte Recovery

In this study, we present graphene oxide derivatized with cyclopentylamine (GO-d-CP) as a DMSO-compatible liquid crystal alignment medium that is free from any background NMR signal for application in anisotropic NMR. This novel alignment medium facilitates optimal isotropic and anisotropic conditions within a single sample preparation, controlled by sonication, thereby enabling the measurement of anisotropic NMR parameters- residual dipolar couplings (RDC) and residual chemical shift anisotropy (RCSA). GO-d-CP offers several advantages, including ease of synthesis, isolation of solid GO-d-CP as a stable non-hygroscopic material, and maintenance of the anisotropic state stability >30 days, allowing for prolonged and repetitive experiments. Notably, post the analysis it allows for easy recovery of valuable analytes as well as GO-d-CP for reuse, enabling the routine application of anisotropic NMR in structural analysis of small molecules. We demonstrate its efficacy by analyzing the relative stereochemistry of four compounds - estrone, santonin, griseofulvin, and cinmethylin - using anisotropic NMR data.

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