Detection of low-level PTFE contamination: An application of solid-state NMR to structure elucidation in the pharmaceutical industry

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• 作者：Tran N. Pham ; Caroline J. Day ; Andrew J. Edwards ; Helen R. Wood ; Ian R. Lynch ; Simon A. Watson ; Anne-Sophie Z. Bretonnet ; Frederick G. Vogt
• 关键词：Solid-state NMR ; Polytetrafluoroethylene (PTFE) ; Quantitative analysis ; Crystallisation slurry ; Polymorphism
• 刊名：Journal of Pharmaceutical and Biomedical Analysis
• 出版年：2011
• 出版时间：25 January 2011
• 年：2011
• 卷：54
• 期：2
• 页码：401-405
• 全文大小：297 K

文摘

We report a novel use of solid-state ¹⁹F nuclear magnetic resonance to detect and quantify polytetrafluoroethylene contamination from laboratory equipment, which due to low quantity (up to 1 % w/w) and insolubility remained undetected by standard analytical techniques. Solid-state ¹⁹F NMR is shown to be highly sensitive to such fluoropolymers (detection limit 0.02 % w/w), and is demonstrated as a useful analytical tool for structure elucidation of unknown solid materials.