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• A 1H Solid State NMR Application for Pharmaceutical Development by using Ultra Fast MAS: Drug-Polymer Intermolecular Interaction on Solid Dispersions_NM190003E

  The low oral bioavailability of a drug due to its poor aqueous solubility is a major challenge for pharmaceutical development. Solid dispersion (SD), where the amorphous drug is dispersed into the polymer matrix, is one of the useful approaches to improve the aqueous solubility. However, thermodynamically unstable nature of an amorphous drug increases its susceptibility to recrystallize upon storage, which, in turn, reduces its solubility and dissolution. Therefore, design of thermodynamically stable SD is required.
• Development of Coldspray Ionization Mass Spectrometry (CSI-MS) and Its Application to Labile Organometallic Compounds in Solution

  Coldspray ionization (CSI) mass spectrometry (MS) has been developed and applied to characterize labile organometallic compounds. While conventional ESI is not applicable to those compounds because of their instability to heat and/or air, CSI affords multiply charged molecular ions with many solvents molecules attached. Here we describe the CSI method and its application to several labile organometallic compounds.
• Development of JMS-S3000: MALDI-TOF/TOF Utilizing a Spiral Ion Trajectory

  We have developed the JMS-S3000, matrix assisted laser/desorption ionization time-of-flight mass spectrometer (MALDI-TOFMS). An innovative ion optical system, which achieved a spiral ion trajectory, surpassed basic specification of the reflectron ion optical system presently used in most commercially available TOFMSs. Furthermore, we have developed the TOF-TOF option for the JMS-S3000. In the case of attaching the TOF-TOF option, a spiral ion optical system is adopted for the first TOFMS, whereas a reflectron ion optical system with offset parabolic reflectron is adopted for the second one. Utilizing the spiral trajectory ion optical system, the JMS-S3000 provides unprecedentedly high mass resolution and high precursor ion selectivity. In this paper, we demonstrate not only the high mass resolution of more than 60,000 (FWHM) at m/z 2093 but also achievement of high mass resolution over a wide mass range. In addition, we present the high selectivity that enables selection of monoisotopic ions of precursor ions. By selecting only monoisotopic ions of precursor ions, one signal peak corresponding to each fragmentation channel is observed on a product ion spectrum. Consequently, the analysis of the product ion spectrum is made clearer.
• NMR Innovation: A Manufacturer’s Perspective on Analytical Advances and New Applications

  Looking back, NMR spectroscopy has been in use as a research tool and under constant development for almost 80 years. Some principles of magnetic resonance were initially described by Isidor Isaac Rabi of Columbia University in 1938. With further fundamental research being done in the late 1930s and early ’40s, the official birth of the technique is generally accepted to have been in 1946 and is attributed to Edward M. Purcell and Felix Bloch. Both were honored with the Nobel Prize for Physics in 1952 for the discovery of NMR spectroscopy. Dr. Ray Freeman, one of the pioneers of NMR applications technology, has created a resource for further reading on the history of both the science and development of NMR technology.
• X-ray, Electron and NMR Crystallography to Structural Determination of Small Organic Molecules

  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.
• Lithium Ion Battery Note

  The applications for lithium ion batteries (LIB) cover a wide range, from power sources for personal computers and mobile devices to automobiles, and there is always a demand for even better performance and safety. In order to ensure the performance and quality of LIB, analysis and evaluation using high-performance assessment systems is necessary. JEOL offers a full line-up of equipment to support the development of new LIB technologies and to improve product quality, including instruments for morphology observation and surface analysis, chemical analysis systems to perform structural analysis on a molecular level, as well as fabrication systems to create high-performance coatings and powders. This LIB note offers solutions for researchers and engineers who are looking for the best equipment for their application.