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Exploring the Effects of Cyclosporin A to Isocyclosporin A Rearrangement on Ion Mobility Separation.
Mácha, Hynek; Zápal, Jakub; Kuzma, Marek; Luptáková, Dominika; Lemr, Karel; Havlícek, Vladimír.
Afiliación
  • Mácha H; Institute of Microbiology of the Czech Academy of Sciences, Vídenská 1083, Prague 142 00, Czech Republic.
  • Zápal J; Department of Analytical Chemistry, Faculty of Science, Palacký University, 17. listopadu 12, Olomouc 771 46, Czech Republic.
  • Kuzma M; Institute of Microbiology of the Czech Academy of Sciences, Vídenská 1083, Prague 142 00, Czech Republic.
  • Luptáková D; Institute of Microbiology of the Czech Academy of Sciences, Vídenská 1083, Prague 142 00, Czech Republic.
  • Lemr K; Department of Analytical Chemistry, Faculty of Science, Palacký University, 17. listopadu 12, Olomouc 771 46, Czech Republic.
  • Havlícek V; Institute of Microbiology of the Czech Academy of Sciences, Vídenská 1083, Prague 142 00, Czech Republic.
Anal Chem ; 96(10): 4163-4170, 2024 03 12.
Article en En | MEDLINE | ID: mdl-38430121
ABSTRACT
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, 1H-13C 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.
Asunto(s)

Texto completo: 1 Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Péptidos / Ciclosporina / Ciclosporinas Idioma: En Revista: Anal Chem Año: 2024 Tipo del documento: Article País de afiliación: República Checa Pais de publicación: Estados Unidos

Texto completo: 1 Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Péptidos / Ciclosporina / Ciclosporinas Idioma: En Revista: Anal Chem Año: 2024 Tipo del documento: Article País de afiliación: República Checa Pais de publicación: Estados Unidos