| Sumario: | The characteristic volatile profile of the Spanish Vinagre de Jerez (VJ), Vinagre de Condado de Huelva (VC) and Vinagre de Montilla-Moriles (VMM) protected designation of origin (PDO) wine vinegars has been studied and compared for the first time by headspace stir bar sorptive extraction-gas chromatography–mass spectrometry (HSSE-GC–MS). The possible markers of each category and PDO were assessed. Acetates were the majority group in all vinegars, while ketones, C13-norisoprenoids and volatile phenols showed significant differences between the three PDOs. Analysis of variance (ANOVA), heatmap and partial least squares-discriminant analysis (PLS-DA) were performed. According to these results, 1-heptanol, methyl nonanoate, 2-methylbutanoic acid, 2,2,6-trimethyl-cyclohexanone, trans-2-decenal, eucalyptol and α-terpineol, were the most significant compounds for differentiating of VC, diacetyl and acetoin, ethyl 3-ethoxypropanoate, 2- and 3-heptanone, 2-methyl-1-hexadecanol, 1-octen-3-ol, p-Cresol and camphene for VMM; and β-damascenone, 5-hydroxymethylfurfural, 3-heptanol, trans-2-hexen-1-ol and trans-2-hexen-1-yl acetate for VJ. Classification results showed that 100% of PDO samples were correctly classified, reaffirming the utility of the volatile profiles for classifying and authenticating wine vinegar PDOs.
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