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Updated: Jun 10, 2026

Sample Preparation for Probe Electrospray Ionization Mass Spectrometry
Published on: February 19, 2020
(15)N-Labeled ionic probes for bioanalytical mass spectrometry
Fumihiro Ito1, Shin Ando, Masato Iuchi
1Faculty of Pharmaceutical Sciences at Kagawa Campus, Tokushima Bunri University, 1314-1 Shido, Sanuki, Kagawa 769-2193, Japan. h-itoh@kph.bunri-u.ac.jp
Stable isotopically labeled probes using a lanthanum (La) complex and the 2,6-bis(oxazolin-2-yl)pyridine (pybox) ligand were synthesized. These novel probes effectively ionize large complex molecules and bioactive peptides using cold-spray ionization mass spectrometry.
Area of Science:
- Analytical Chemistry
- Mass Spectrometry
- Chemical Synthesis
Background:
- Developing efficient ionization methods is crucial for analyzing complex molecules in mass spectrometry.
- Stable isotopically labeled probes can enhance sensitivity and accuracy in analytical measurements.
- Lanthanum (La) complexes offer unique properties for potential applications in ionization techniques.
Purpose of the Study:
- To synthesize novel stable isotopically labeled probes based on a La-complex and a 2,6-bis(oxazolin-2-yl)pyridine (pybox) ligand.
- To evaluate the effectiveness of these probes in the ionization of large complex molecules.
- To demonstrate the utility of the (15)N-labeled pybox-La complex for analyzing bioactive peptides via cold-spray ionization mass spectrometry.
Main Methods:
- Synthesis of novel stable isotopically labeled probes: succinimide-tetramethylpybox (NHS-TMpybox), maleimide-tetramethylpybox (Mal-TMpybox), and 4-(tetramethylpybox)-butyl bromoacetate (BrAc-TMpybox).
- Utilizing a (15)N-labeled pybox-La complex as the core ionization agent.
- Employing cold-spray ionization mass spectrometry (CSI-MS) for the analysis of various compounds.
Main Results:
- Successful synthesis of novel stable isotopically labeled pybox-based probes.
- Demonstration of the La-complex-based probe's effectiveness in ionizing large complex molecules.
- Effective ionization of bioactive peptides was achieved using the (15)N-labeled pybox-La complex with CSI-MS.
Conclusions:
- The developed La-complex-based probe ionization method is effective for analyzing complex samples.
- The synthesized stable isotopically labeled probes, particularly the (15)N-labeled pybox-La complex, show significant value in mass spectrometry.
- This approach offers a promising tool for the analysis of challenging biomolecules like peptides.
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