The 10th Asia-Oceania Mass Spectrometry Conference (AOMSC2025) - organized by the Mass Spectrometry Society of Japan

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Day 2, June 23(Mon.) 

Room P (Maesato East, Foyer, Ocean Wing)

Development of New Crystalline Sponges with Solvent and Vacuum Resistance

(1The Univ. of Tokyo, 2IMS, 3Daicel Corp.)
oSota Sato1,2, Keisuke Gondo3, Tomoko Adachi3

In molecular structure analysis, determination of three-dimensional structure including absolute configuration is important, and single crystal X-ray diffraction is the most powerful technique. Since the information obtained from MS is limited to the determination of molecular weight, compositional formula, and the estimation of planar structure, it is useful to combine MS with diffraction techniques. Crystal sponge (CS) method does not require crystallization process and can be applied to gaseous and liquid molecules, that do not crystallize by their nature. In this study, new CS bearing highly polar amide groups were prepared and applied to modified preparative GC-MS system. These CS are resistant to highly polar solvents and can retain their crystallinity, and it was found that they can be applied to highly polar guest molecules whose crystals would collapse using conventional CS. In addition, the amide groups inside the nanopore of CS were found to interact effectively with the guest molecules and contribute to their precise alignment. Furthermore, the CS can maintain its crystallinity even after the solvent molecules are removed from inside nanopore. A new analytical strategy, "preparative GC-MS x direct CS method", was developed, and the structures of the separated volatile components were determined by X-ray structural analysis.