On-line coupled liquid chromatography-gas chromatography-flame ionisation detection (LC-GC-FID) enables efficient and unambiguous determination of irradiation for some fat-containing foods (e.g. meat). Other products, however, contain interfering components or are contaminated, e.g., with mineral oil. Since more selective detection by mass spectrometry has limited success, the determination was improved by a more selective isolation of some key components among the fat degradation products, e.g. the dienes or trienes, by LC-LC-GC-FID. Applications are shown for soup mixes, some spices, fish, and shrimps.