The aim of this work was to develop, evaluate and apply an analytical workflow for investigation of volatile metabolites to leaves of grapevine. The experimental approach included sampling, quenching, cooled homogenisation with a ball mill, extraction of metabolites by solid phase microextraction, analysis by gas-chromatography - mass spectrometry, annotation/identification (AMDIS, identification criteria: match factor 90, retention time deviation 2% from reference), and statistical data treatment data (t-test, principal component analysis PCA). Application of the workflow to grapevine leaves resulted in the detection of 63 metabolites and the separation of leaves from two sampling days with PCA. In phylloxera-attacked roots 38 metabolites were detected, of which 14 showed significant different concentrations compared to non-attacked roots. Moreover, a database containing 1619 entries from 39 studies using GC concerning grapevine was compiled.