The resistance of edible oils to oxidative degradation, leading to rancidification, is an important parameter for assessing the quality of oil. This paper presents a new promising method to diagnose the volatile compounds which are products of oil oxidation reactions. Our experiment was carried out using a combined method of UV irradiation as an oxidation acceleration technique, headspace solid-phase microextraction (HS-SPME) as an extraction technique and capillary gas chromatography (GC) as an assay technique. Method precision and sensitivity expressed as RSD (<19%) and LOD (between 18 and173 ng/mL) are satisfactory. The induction period set on hexanal / t-2-nonenal ratio (IP=6.67 h) is comparable with those obtained with the Rancimat method (4.64–6.73 h).
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