Open AccessDevelopment of Identification Test Methods for Triptorelin Acetate and Goserelin Acetate Substances using NMR spectroscopy
Author(s) -
Sergey Moiseev,
Н. Е. Кузьмина,
А. И. Лутцева
Publication year - 2019
Publication title -
vedomosti naučnogo centra èkspertizy sredstv medicinskogo primeneniâ
Language(s) - English
Resource type - Journals
eISSN - 2619-1172
pISSN - 1991-2919
DOI - 10.30895/1991-2919-2019-9-1-54-63
Subject(s) - chemistry , triptorelin , nuclear magnetic resonance spectroscopy , proton nmr , chromatography , stereochemistry , biochemistry , hormone , gonadotropin releasing hormone , luteinizing hormone
The work is a continuation of the research on the use of NMR spectroscopy in the quality control of natural peptide hormone-based active substances and their synthetic analogues. The aim of the paper was to develop identification test methods for triptorelin acetate and goserelin acetate substances using NMR spectroscopy that does not require reference standards ‒ with the aim of using the newly developed test methods in pharmacopoeial analysis. Materials and methods: the procedure was developed using two-dimensional NMR spectroscopy ( 1 H- 1 H gCOSY, 1 H- 13 C gHSQC, 1 H- 13 C gHMBC). Results: thestudy made it possible to assign 1 H and 13 C NMR signals to a specific molecular fragment, and to determine the amino acid composition of each oligopeptide. Conclusions: the authors drew up a table showing structural assignment of NMR signals, which makes it possible to use the NMR method for identification testing of triptorelin acetate and goserelin acetate substances without the use of pharmacopoeial reference standards. The study helped to determine the optimal temperature conditions for recording 13 C NMR spectra (27 °С and 50 °С for triptorelin acetate and goserelin acetate, respectively). It was demonstrated that 13 C NMR spectroscopy could be used for identification testing in pharmacopoeial analysis.