Large volume headspace GC/MS analysis for the identification of volatile compounds relating to seafood decomposition.

Decomposition in seafood products in the United States is monitored by the Food and Drug Administration (FDA) laboratories using sensory testing, which requires highly trained analysts. A large-volume headspace (LVHS) gas chromatography/mass spectrometry (GC/MS) method was developed to generate analytical results that can be directly compared to sensory evaluation. Headspace vapor was withdrawn from a 1-L vial containing 50 g seafood sample using a large volume headspace autosampler. Various volatile compounds were collected simultaneously. Analytes were preconcentrated by a capillary column trapping system and then sent through a cryo-focuser mounted onto the GC injector. A selected ion monitoring (SIM) MS acquisition method was used to selectively monitor 38 compounds of interest. Samples of red snapper, croaker, weakfish, mahi-mahi, black tiger shrimp, yellowfin tuna, and sockeye salmon that have been assessed and scored by an FDA National Seafood Sensory Expert (NSSE) were used for method performance evaluation. Characteristic compounds potentially associated with seafood quality deterioration for each seafood species were identified by quantitative analysis using pooled matrix-matched calibrations and two-sample