Journal of chromatography. A
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In this work, a methodology to characterise the volatile and semi-volatile compounds from marine salt by headspace solid-phase microextraction (HS-SPME) and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GCxGC/TOFMS) was developed. Samples from two saltpans of Aveiro, in Portugal, with diverse locations, obtained over three years (2004, 2005, and 2007) were analysed. A 50/30microm divinylbenzene/carboxen/polydimethylsiloxane SPME fibre was used. ⋯ The large number of co-elutions on the first column that were resolved by the GCxGC system revealed the complexity of marine salt volatile composition. The existence of a structured 2D chromatographic behaviour according to volatility, in the first dimension ((1)D), and primarily polarity, in the second dimension ((2)D), was demonstrated, allowing more reliable identifications. The resolution and sensitivity of GCxGC/TOFMS enabled the separation and identification of a higher number of volatile compounds compared to GC-qMS, allowing a deeper characterisation of this natural product.