Headspace solid-phase microextraction combined with comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry for the determination of volatile compounds from marine salt.

摘要: Abstract In this work, a methodology to characterise the volatile and semi-volatile compounds from marine salt by headspace solid-phase microextraction (HS-SPME) comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC/TOFMS) was developed. Samples two saltpans of Aveiro, in Portugal, with diverse locations, obtained over three years (2004, 2005, 2007) were analysed. A 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane SPME fibre used. The volatiles present solid samples (crystals) equilibrated overnight at 60 °C extracted for 60 min prior injection GC × GC/TOFMS. 157 compounds, distributed chemical groups hydrocarbons, aldehydes, esters, furans, haloalkanes, ketones, ethers, alcohols, terpenoids, C13 norisoprenoids, lactones detected across samples. Furans, haloalkanes ethers identified first time salt. large number co-elutions on column that resolved GC × GC system revealed complexity composition. existence structured 2D chromatographic behaviour according volatility, dimension (1D), primarily polarity, second (2D), demonstrated, allowing more reliable identifications. resolution sensitivity GC × GC/TOFMS enabled separation identification higher compared GC–qMS, deeper characterisation natural product.