Multinuclear 1H/13C/15N chemical shift assignment of therapeutic octreotide acetate performed at natural abundance

Bibliographische Detailangaben
Veröffentlicht in:	Magnetic resonance in chemistry : MRC. - 1985. - 62(2024), 7 vom: 01. Juli, Seite 486-496
1. Verfasser:	Menke, Alexander J (VerfasserIn)
Weitere Verfasser:	Chen, Fu, Chen, Kang
Format:	Online-Aufsatz
Sprache:	English
Veröffentlicht:	2024
Zugriff auf das übergeordnete Werk:	Magnetic resonance in chemistry : MRC
Schlagworte:	Letter Research Support, U.S. Gov't, Non-P.H.S. 13C/15N CP‐MAS HMBC HSQC‐TOCSY NMR solid state Octreotide RWM8CCW8GP mehr... Carbon Isotopes Nitrogen Isotopes Protons Nitrogen-15

Beschreibung
Zusammenfassung:	© 2024 John Wiley & Sons Ltd. This article has been contributed to by U.S. Government employees and their work is in the public domain in the USA. Octreotide acetate, the active pharmaceutical ingredient in the long-acting release (LAR) drug product Sandostatin®, is a cyclic octapeptide that mimics the naturally occurring somatostatin peptide hormone. Modern NMR can be a robust analytical method to identify and quantify octreotide molecules. Previous 1H chemical shift assignments were mostly performed in organic solvents, and no assignments for heteronuclear 13C, 15N, and aromatic 1H nuclei are available. Here, using state-of-the-art 1D and 2D homo- and heteronuclear NMR experiments, octreotide was fully assigned, including water exchangeable amide protons, in aqueous buffer except for 13CO and 15NH of F1, 15NH of C2, and 15NζHζ of K5 that were not observed because of water exchange or conformational exchange. The solution NMR spectra were then directly compared with 1D 1H/13C/15N solid-state NMR (SSNMR) spectra showing the potential applicability of 13C/15N SSNMR for octreotide drug product characterization
Beschreibung:	Date Completed 29.05.2024 Date Revised 17.09.2024 published: Print-Electronic Citation Status MEDLINE
ISSN:	1097-458X
DOI:	10.1002/mrc.5436