Solid-phase microextraction method for the determination of volatile compounds associated to oxidation of fish muscle

A procedure for the determination of volatile compounds derived from lipid oxidation of fish muscle samples is presented. Analytes are concentrated on a solid-phase microextraction fiber employed in the headspace mode (HS-SPME), and selectively determined using gas chromatography in combination with mass spectrometry (GC–MS). The influence of several parameters on the efficiency of microextraction such as type of fiber, volume of sample, time, temperature, salting-out effect and stirring was systematically investigated. A saline extraction of fish muscle followed by incubation on a Carboxen-polydimethylsiloxane fiber during 30 min at 60 °C gave the most effective and accurate extraction of the analytes. Quantification of them was performed by MS in the selected ion monitoring mode and by the internal standard method. Satisfactory linearity, repeatability and quantification limits were achieved under these conditions. The method was applied to the determination of the volatile compounds associated to oxidation of Atlantic horse mackerel (Trachurus trachurus) minced muscle and excellent correlations were obtained with chemical indexes for monitoring lipid oxidation as peroxide value and thiobarbituric acid reactive substances. This combined technique is fast, simple, sensitive, inexpensive and useful to monitor target compounds associated to fish rancidity as 1-penten-3-ol, 2,3-pentanedione or 1-octen-3-ol.