Analytical Instrument Documents

In 2013, JEOL RESONANCE launched the cryogenic NMR probe systems,”UltraCOOL” and “SuperCOOL”. Delivering sensitivity far exceeding conventional room temperature probes together with ease of use beyond that previously associated with cooled probes, such as probe change whilst cooled, and variable temperature measurement capability, the products received a lot of positive response. However, many dramatic stories lay behind the birth of these products.

Here we present the recent development at RIKEN CLST-JEOL collaboration laboratory to explore the molecular structures of low-molecular weight pharmaceutical compounds in natural abundance (without any isotopic labeling); the recent progress in fast magic angle spinning (MAS) technology in solid-state nuclear magnetic resonance (ssNMR) and in ultra high sensitivity camera in transmission electron microscopy (TEM) paves a new way to answer problems in the pharmaceutical industry and sciences. 1) Crystalline polymorphs and 2) salt/cocrystal are two major concerns in terms of quality control, stability, and intellectual property. To identify the crystalline form, powder X-ray diffraction and 13C cross-polarization MAS ssNMR are widely used methods, however, the former is sometimes not suitable for mixture analysis and latter fails to distinguish crystalline forms with similar molecular conformations. To solve these issues, we use electron diffraction (ED) and 1H fast MAS NMR. The crystalline form can be determined from nano- to micro-meter sized single crystals using ED, since electron interactions are 4 to 5 order stronger than X-ray interactions. 1H NMR also gives suitable information to molecular packing since 1H is located at the surface of the crystals. The salt/cocrystal issue, where hydrogen plays a key role, is a serious problem, since single crystal X-ray diffraction (SCXRD) cannot determine the hydrogen atom position precisely. Here we determine the internuclear distances between 1H and 15N using ssNMR at fast MAS conditions, while the global structure is obtained through SCXRD, answering the salt/cocrystal questions.

Download all eight Delta QuickTime movie tutorials.

How to acquire and process proton spectra: process lists in 1D Processor, using the Pointer Tools to interact with data, peak picking, J-coupling tool, integration, plotting.

How to acquire and process 1D, 2D, nOe spectra: comparing multiple data sets in Data Slate, loading high-resolution projections, Level Tool, plotting, understanding through-bond correlations, common nOe experiments, data interpretation.

A comprehensive description and demonstration of contouring data with Level Tool.

How to acquire and process HMBC spectra: loading high-resolution projections, Level Tool, plotting, understanding HMBC, data interpretation.

How to acquire and process multiplicity-edited HSQC spectra: phasing 2D data, loading high-resolution projections, setting contrast colors in Level Tool, plotting, HMQC versus HSQC, data interpretation.

How to acquire and process COSY spectra: process lists in nD Processor, loading high-resolution projections into 2D Viewer, Level Tool, using Cursor mode to highlight coupling partners, plotting, 1D proton versus 2D COSY, data interpretation, common COSY sequence variants.

How to acquire and process HETCOR and HMQC spectra: loading high- resolution projections into 2D Viewer, Level Tool, plotting, understanding inverse experiments, HETCOR versus HMQC, data interpretation, normal versus inverse probe geometries.

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