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Title: A multi-technique analytical approach for impurity profiling during synthesis : the case of difluprednate
Authors: Sammut Bartolo, Nicolette
Zoidis, Grigoris
Gikas, Evagelos
Benaki, Dimitra
Ferrito, Victor
Serracino-Inglott, Anthony
Keywords: Secondary ion mass spectrometry
Nuclear isomers
Mass spectrometry
Nuclear magnetic resonance
Chemistry, Physical and theoretical
Issue Date: 2020
Publisher: Elsevier BV
Citation: Sammut Bartolo, N., Zoidis, G., Gikas, E., Benaki, D., Ferrito, V., & Serracino-Inglott, A. (2020). A multi-technique analytical approach for impurity profiling during synthesis: The case of difluprednate. Journal of Pharmaceutical and Biomedical Analysis, 113483.
Abstract: A methodology for the qualitative analysis of a mixture of compounds obtained during the synthesis of difluprednate is described herein for the first time. For this scope a multi-technique analytical approach was developed, combining Liquid Chromatography/Mass Spectrometry (LC/MS), Nuclear Magnetic Resonance (NMR) and computational chemistry. Separation of isomers is frequently required for the identification of impurities in active pharmaceutical ingredients (APIs) to assess the impact they may exhibit on public health. During the final step of the difluprednate synthesis apart from the desired product, various by-products may be obtained. Structural analysis of the products using LC/MS and NMR indicated that the steroid difluprednate was obtained along with its acetyl/butyryl regional isomers, whereas the results were further supported by semi-empirical calculations of the MS-derived data. Following the proposed approach, we managed to elucidate the structures of the challenging 11-acetate, 17-butyrate from the 17-acetate, 21-butyrate, 6α,9α-difluoro prednisolone isomers. The approach utilized may be of general applicability for the analysis of impurities in active pharmaceutical ingredients obtained during chemical synthesis.
Appears in Collections:Scholarly Works - FacM&SPha

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