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Abstract
An isocratic reversed phase high performance liquid chromatographic method with charged aerosol detection (CoronaTM CADTM) was developed and validated for the quantitative determination (assay) of 4-methanesulfonyl-piperidine (MSP). This compound has no ultraviolet (UV) chromophore and showed no retention on a reversed phase column. Heptafluorobutyric acid (HFBA) was used as a basic ion pairing agent for increased retention. An Atlantis C18 (150 × 4.6 mm, 3.5 µm) column was eluted with a mobile phase consisting of 0.1% heptaflurobutyric acid in water-acetonitrile (90:10, v/v). The analyses were performed at 40°C with a flow rate of 1 mL/min and CAD detection with Nitrogen operating gas pressure maintained at 35 psi. The method was validated for precision, linearity, and specificity. The procedure described here is simple, selective, and is suitable for routine quality control analysis.
ACKNOWLEDGMENTS
Our thanks go to our colleagues Dr. Magnus Eriksson (Chemical Development) for providing us with relevant intermediates; Sherry Shen, Dr. Nelu Grinberg, Amy Birch, and Johanna Ubben for initial GC method development. We thank our management for their support of this work.