Affiliation:
1. Scientific Centre for Expert Evaluation of Medicinal Products
Abstract
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 aimof 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 (1H-1H gCOSY,1H-13C gHSQC,1H-13C gHMBC).Results:thestudy made it possible to assign1H and13C 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 recording13C NMR spectra (27 °С and 50 °С for triptorelin acetate and goserelin acetate, respectively). It was demonstrated that13C NMR spectroscopy could be used for identification testing in pharmacopoeial analysis.
Reference12 articles.
1. Kuz’mina NE, Moiseev SV, Krylov VI, Yashkir VA, Merkulov VA. Development of a procedure for the identification of pharmaceutical substance buserelin acetate by NMR spectroscopy without using pharmacopoeia reference standard. Antibiotiki i Khimioterapiya 2017; 62(9-10): 40-46 (in Russ.).
2. Kuz’mina NE, Moiseev SV, Krylov VI, Deryabin AS, Yashkir VA, Merkulov VA. Validation of an NMR-Spectroscopic Method for Authenticity Confirmation of Buserelin Acetate Pharmaceutical Substance. Pharmaceutical Chemistry Journal. 2018; 52(2): 48-53; (in Russ.). https://doi.org/10.30906/0023-1134-2018-52-2-48-53.
3. Kovaleva SV, Isaeva IV, Lutseva AI, Aladysheva GI, Pikhtar AV. Problems for standardization of hormonal preparations of protein-peptide nature. Russian Journal of General Chemistry. 2005; XLIX(1):135-145 (in Russ.).
4. Matveyev BP. The Role of Triptorelin (Diphereline) in the Treatment of Prostate Cancer. Oncourology. 2008; (4): 53-56 (in Russ.).
5. Frampton JE. Triptorelin: A Review of its Use as an Adjuvant Anticancer Therapy in Early Breast Cancer. Drugs. 2017; 77(18):2037-2048.
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1. NMR as Used in the Russian and Foreign Pharmacopoeias for Quality Control of Medicinal Products;The Bulletin of the Scientific Centre for Expert Evaluation of Medicinal Products. Regulatory Research and Medicine Evaluation;2022-02-18
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