A headspace solid-phase microextraction coupled to gas-chromatography and mass spectrometry (HS-SPME-GC-MS) was developed and validated for the determination of 26 terpenes in sparkling wines. The use of a Box-Behnken experimental design, together with the desirability function D, allowed the extraction conditions of the method to be optimized. The optimal extraction conditions were found at a dilution ratio of 2:3, the addition of 3.5 g of NaCl, an extraction temperature of 46 °C and an extraction time of 52 min, using the DVB/CAR/PDMS fibre. Afterwards, the analytical method was successfully validated in terms of linearity, matrix effect, limit of detection and quantification, precision and accuracy. To test the developed method, 35 commercial sparkling wines from different grape varieties, geographical regions and ageing times were analysed and their terpenoid profile was monitored. The use of multivariate statistical tools made it possible to highlight differences in the samples related to the terpene profile. Finally, the most important compounds involved in the discrimination of the samples were identified by means of iterative variable selection procedures.
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