A method for the quantitative determination of 2 hydroxy 2 methylbutanoic (2OH2MB), 2 hydroxy 3 methylbutanoic (2OH3MB), 3 hydroxy 3 methylbutanoic (3OH3MB), 2 hydroxy 4 methylpentanoic (2OH4MP) and 3 hydroxybutanoic (3OHB) acids has been optimized, validated and applied to a set of wines and other alcoholic beverages. The analytes were preconcentrated in a solid phase extraction cartridge and derivatized with 2,3,4,5,6 pentafluorobenzyl bromide at room temperature for 30 min, followed by GC MS analysis. Detection limits were between 0.5 and 29 μg L , and linearity was maintained up to 3 or 12 mg L , depending on the analyte. Recovery values were between 85 and 106 %, and reproducibility was better than 12 % RSD in most cases. The first specific study of these analytes in wine and other alcoholic beverages is herein reported. Concentrations ranged from the method detection limits to 7820, 519, 8510, 3470 and 2500 μg L for 2OH2MB, 2OH3MB, 3OH3MB, 2OH4MP and 3OHB, respectively, which may have relevant sensory effects. These products were not found in distillates (except 3OHB) but were all present in beer. 2OH2MB, 3OH3MB and 3OHB were found in unfermented grape derivatives. Sherry wines had the highest levels of all except for 3OHB.