Analysis of low-molar-mass materials in commercial rubber samples by Soxhlet and headspace extractions followed by GC-MS analysis

Very tight regulations apply to materials used for pharmaceutical packaging and for administering drugs. In this paper, we describe a simple and reliable procedure involving both gas- and liquid-phase extraction steps followed by an analysis step to identify the low-molar-mass materials in commercial-rubber samples. Representative commercial rubbers, that could be used for pharmaceutical packaging, have been selected and cryogenically powdered. Headspace and Soxhlet extractions have been carried out and the key parameters are discussed. The obtained extracts have been analyzed by gas chromatography (GC)-mass spectrometry (MS). More than 100 compounds have been detected and identified. Headspace allowed to extract the more-volatile compounds, whereas Soxhlet extraction recovered less-volatile compounds, but induced a loss of the volatile ones. Thus, both extraction techniques are required to fully characterize the low-molar-mass compounds present in rubber. (C) 2004 Elsevier B.V. All rights reserved.