Freitas, JorgeSilva, PedroVaz-Pires, PauloCâmara, José S.2022-10-062022-10-062020Freitas, J., Silva, P., Vaz-Pires, P., & Câmara, J. S. (2020). A systematic AQbD approach for optimization of the most influential experimental parameters on analysis of fish spoilage-related volatile amines. Foods, 9(9), 1321.http://hdl.handle.net/10400.13/4689The volatile amines trimethylamine (TMA) and dimethylamine (DMA) could be used as important spoilage indices for seafood products, assisting in the determination of the rejection period. In the present study, a systematic analytical duality-by-design (AQbD) approach was used as a powerful strategy to optimize the most important experimental parameters of headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) conditions for the quantification of TMA and DMA in Sparus aurata. This optimization enabled the selection of the best points in the method operable design region for HS-SPME extraction (30 min; 35 ◦C; NaOH 15 M and NaCl 35%, w/v) and GC-MS analysis (80 ◦C; gradient 50 ◦C/min; flow rate 1 mL/min and splitless mode). The rejection day, estimated through the TMA concentration (>12 mg/100 g, at days 9–10), was compared with sensory (quality index method: day 7–8), physical (Torrymeter: day 8–9), and microbial (day 9–10) analysis, corroborating the suitability of the proposed approach for estimating the period for which they will retain an acceptable level of eating quality from a safety and sensory perspective.engSparus aurataTrimethylamineDimethylamineFreshnessHS-SPMEGC-MSMicrobiologyDielectric propertiesSensory analysis.Faculdade de Ciências Exatas e da EngenhariaCentro de Química da Madeirajournal article10.3390/foods9091321