• Headspace analysis;
  • fish oil;
  • lipid oxidation;
  • solid-phase microextraction


Long-chain polyunsaturated fatty acids (LC-PUFA) have various positive biological effects. Fish oil represents a major source of LC-PUFA; therefore it is extensively used to enrich food products as, for example, infant formulae, dairy products and fruit juices. However, in the presence of oxygen and metals, LC-PUFA readily degrade, producing off-flavors and decreasing the nutritional value of the product. The deterioration of sensory properties (taste and odor) can be easily perceived by the consumer, due to the formation of volatile compounds that are formed by decomposition of lipid hydroperoxides, also known as primary oxidation products. In this study, we used the headspace solid-phase microextraction-gas chromatography/mass spectrometry technique (HS-SPME-GC/MS) to characterize and quantify volatile compounds in a food matrix supplemented with fish oil. We demonstrated that the HS-SPME-GC/MS method is a valuable tool to monitor lipid oxidation at early stages. We identified t-2-hexenal and c-4-heptenal as possible oxidation markers during the storage of milk enriched with 5% of cod oil.