Exploring the Effects of Cyclosporin A to Isocyclosporin A Rearrangement on Ion Mobility Separation.

Autor:	Mácha H; Institute of Microbiology of the Czech Academy of Sciences, Vídeňská 1083, Prague 142 00, Czech Republic.; Department of Analytical Chemistry, Faculty of Science, Palacký University, 17. listopadu 12, Olomouc 771 46, Czech Republic., Zápal J; Institute of Microbiology of the Czech Academy of Sciences, Vídeňská 1083, Prague 142 00, Czech Republic., Kuzma M; Institute of Microbiology of the Czech Academy of Sciences, Vídeňská 1083, Prague 142 00, Czech Republic.; Department of Analytical Chemistry, Faculty of Science, Palacký University, 17. listopadu 12, Olomouc 771 46, Czech Republic., Luptáková D; Institute of Microbiology of the Czech Academy of Sciences, Vídeňská 1083, Prague 142 00, Czech Republic., Lemr K; Institute of Microbiology of the Czech Academy of Sciences, Vídeňská 1083, Prague 142 00, Czech Republic.; Department of Analytical Chemistry, Faculty of Science, Palacký University, 17. listopadu 12, Olomouc 771 46, Czech Republic., Havlíček V; Institute of Microbiology of the Czech Academy of Sciences, Vídeňská 1083, Prague 142 00, Czech Republic.; Department of Analytical Chemistry, Faculty of Science, Palacký University, 17. listopadu 12, Olomouc 771 46, Czech Republic.
Jazyk:	angličtina
Zdroj:	Analytical chemistry [Anal Chem] 2024 Mar 12; Vol. 96 (10), pp. 4163-4170. Date of Electronic Publication: 2024 Mar 02.
DOI:	10.1021/acs.analchem.3c05165
Abstrakt:	Cyclosporin A (CycA) is a peptide secondary metabolite derived from fungi that plays a crucial role in transplantation surgery. Cyclic traveling wave ion mobility mass spectrometry (IM-MS) revealed an N → O peptidyl shift in singly protonated CycA to isocyclosporin A (isoA), whereas no such isomerization was observed for doubly protonated and sodiated molecules. CycA and isoA were able to be separated by considering doubly protonated precursors using a specific ion fragment. In parallel, sodium ion stabilization facilitated the simultaneous separation and quantitation of singly charged cyclosporin isomers with the limit of detection and coefficient of determination of 1.3% and 0.9908 for CycA in isoA and 1.0% and 0.9830 for isoA in CycA, respectively. Finally, 1 H- 13 C gHSQC NMR experiments permitted parallel recording of up to 11 cyclosporin conformers. The ratios were determined by integrating the volume of cross-peaks of the upfield resonating hydrogen in the diastereotopic methylene group of sarcosine-3.
Databáze:	MEDLINE
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