Identification of a pharmaceutical packaging off-odor using solid phase microextraction gas chromatography/mass spectrometry
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Updated: Oct 7, 2026

Gas Chromatography-Mass Spectrometry Paired with Total Vaporization Solid-Phase Microextraction as a Forensic Tool
Published on: May 25, 2021
S L Sides1, K B Polowy, A D Thornquest
1Pharmaceutical Development Division, Glaxo Wellcome Inc., Five Moore Drive, Research Triangle Park, NC 27709, USA.
Abstract:
The use of a solid phase microextraction (SPME) sampling technique, in conjunction with gas chromatography/mass spectrometry (GC/MS) analysis, to identify an off-odor in a heat-stressed pharmaceutical packaging material is described. The ability of the commercially available polydimethylsiloxane (PDMS) coated microfiber to concentrate a trace volatile compound of interest enabled identification of the odor compound of interest. Despite being present at levels that defied detection using conventional headspace sampling techniques, ethyl-2-mercaptoacetate was determined to be the compound responsible for the offending odor. Formation of the thioester resulted from an unanticipated reaction (either esterification or transesterification) between a common residual solvent (ethanol), present in a commonly used pharmaceutical tablet dispersant, and low-level amounts of reactants or synthetic intermediates of an FDA-approved polyvinyl chloride (PVC)-resin thermal stabilizing agent.
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