Impurity profiling in bulk pharmaceutical batches using 19F NMR spectroscopy and distinction between monomeric and dimeric impurities by NMR-based diffusion measurements
| Autor: | Ismail M. Ismail, R. D. Farrant, Maili Liu, John C. Lindon, Nisha Mistry, Jeremy K. Nicholson |
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| Rok vydání: | 1999 |
| Předmět: |
Magnetic Resonance Spectroscopy
Diffusion Dimer Clinical Biochemistry Analytical chemistry Pharmaceutical Science Mass spectrometry Sensitivity and Specificity Mass Spectrometry Analytical Chemistry chemistry.chemical_compound Impurity Drug Discovery Chromatography High Pressure Liquid Spectroscopy Detection limit Molecular diffusion Reproducibility of Results Fluorine Nuclear magnetic resonance spectroscopy Androstadienes Monomer chemistry Fluticasone Drug Contamination Dimerization |
| Zdroj: | Journal of Pharmaceutical and Biomedical Analysis. 19:511-517 |
| ISSN: | 0731-7085 |
| DOI: | 10.1016/s0731-7085(98)00247-7 |
| Popis: | The impurity profile of production batches of fluorine-containing drugs can be characterised efficiently using F-19 NMR spectroscopy. This yields the number and proportions of impurities in the bulk drug to a level of approximate to 0.1 mole% in a few minutes of NMR experiment time. The approach has been exemplified using a partially purified batch of the steroidal product fluticasone propionate, the impurities in which include a number of dimeric species. Further distinction between the monomer and dimer impurities has been achieved through high resolution chemical shift-resolved NMR measurement of molecular diffusion coefficients on the intact mixture using F-19 NMR spectroscopy. The ability of NMR-based diffusion coefficient determination to distinguish between monomeric and dimeric substances was validated using a standard mixture of authentic materials containing both monomers and dimers. (C) 1999 Elsevier Science B.V. All rights reserved. |
| Databáze: | OpenAIRE |
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