Orange spirit, a novel fruit distillate, was analysed by direct injection gas chromatography-mass spectrometry and headspace solid-phase microextraction (SPME) coupled to GC-MS. Different commercial SPME fibre types have been tested for the analysis of orange spirit. The divinylbenzene/carboxen on poly(dimethylsiloxane) fibre was chosen because it gave the best repeatability of the method. Headspace SPME-GC-MS selectivity was found to be comparable to GC direct injection for most orange spirit volatile compounds. The divinylbenzene/carboxen/poly(dimethylsiloxane) fibre had very high affinity for non-polar and less polar compounds, especially for some components of orange peel oil, which could be considered the impact compounds of orange spirit. In this way, good sensitiveness was ensured for these compounds. Conversely, the GC analysis was more sensitive for polar compounds, especially for molecules such as methanol, isobutanol, n-butanol and iso-amyl alcohols. SPME was a useful tool for quickly screening orange flavour compounds and can be considered as complementary to GC direct injection analysis, which should be used when an accurate quantitative determination of analytes is required. Copyright (C) 2002 John Wiley Sons, Ltd.