A method for the analysis of several volatiles compounds responsible for orange juice flavour (ethyl butanoate, limonene, linalool, alpha-pinene, geranial, neral and alpha-terpineol) has been developed. The isolation of this compounds was carried out by pervaporation (PV) followed by on-line gas chromatography-mass spectrometry (GC-MS). The coupling PV-GC-MS has been successfully applied to fresh hand-squeezed orange juices and frozen concentrated ones in order to establish differences in their flavour profile. Method has been validated with recovery spike experiments which showed its applicability for a wide range of concentrations.