小样本异核二维 NMR 的实验极限研究。

Investigation of the experimental limits of small-sample heteronuclear 2D NMR.

机构信息

Discovery and Preclinical Sciences, Process Chemistry Rapid Structure Characterization Laboratory, Merck Research Laboratories, Summit, New Jersey 07901, USA.

出版信息

J Nat Prod. 2010 Sep 24;73(9):1465-9. doi: 10.1021/np100481m.

DOI:10.1021/np100481m

PMID:20812673

Abstract

Practical experimental performance limits for an ensemble of heteronuclear 2D NMR experiments using a state-of-the-art 600 MHz 1.7 mm Bruker TCI Micro CryoProbe are reported. In the specific case of multiplicity-edited GHSQC, it was possible to acquire data on a 540 ng sample of strychnine (1; ∼1.6 nmol), prepared by serial dilution, which was used as a model compound. The experiments discussed also included GCOSY, (13)C reference spectra, (1)H-(13)C GHMBC, IDR-GHSQC-TOCSY, 1,1-ADEQUATE, and (1)H-(15)N GHMBC.

摘要

本文报道了使用最先进的 600 MHz 1.7 mm Bruker TCI Micro CryoProbe 对异核二维 NMR 实验进行整体实验性能限制的实际评估。在多重编辑 GHSQC 的特殊情况下，有可能对士的宁（1；约 1.6 nmol）的 540 ng 样品进行数据采集，该样品通过连续稀释制备，用作模型化合物。讨论的实验还包括 GCOSY、（13）C 参考光谱、（1）H-（13）C GHMBC、IDR-GHSQC-TOCSY、1,1-ADEQUATE 和（1）H-（15）N GHMBC。