A GC-FID method for major volatile analysis in cider and wine was validated under the requirements of the ISO/ IEC 17025 regulation using a split mode injection. This method presented a good linearity (R 2 >0.999, C m >99%), a wide range of calibration, the maximum random errors for repeatability and intermediate precision were 5% and 8%, respectively, and the maximum limit of quantifi cation and limit of detection were 14.1 mg l -1 and 4.6 mg l -1 , respectively. Trueness, expressed as

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... (%), was successfully validated by means of two different methods, standard addition (92-110%) and comparison against reference materials (93-115%). Expanded uncertainty estimated at 95% confi dence level ranged between 11% for methanol and 7% for allyl alcohol. The validated method was successfully applied for the analysis of major volatiles in ciders and wines, and to detect yeast and lactic acid bacteria spoilage.