Multinuclear 1H/13C/15N chemical shift assignment of therapeutic octreotide acetate performed at natural abundance.
Magn Reson Chem
; 62(7): 486-496, 2024 07.
Article
in En
| MEDLINE
| ID: mdl-38351244
ABSTRACT
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.
Key words
Full text:
1
Collection:
01-internacional
Database:
MEDLINE
Main subject:
Octreotide
Language:
En
Journal:
Magn Reson Chem
Journal subject:
QUIMICA
Year:
2024
Type:
Article
Affiliation country:
United States