Abstract

The 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.

Highlights

  • Fish constitute a complex system in which enzymatic, microbial, and physicochemical interactions occur simultaneously, which has an impact on flavor, texture, and shelf life

  • The scouting of the analytical method, which implies the study of the relevant parameters for the chosen methodology and the target analyte characteristics, was based on previously developed studies for headspace solid-phase microextraction (HS-SPME)/gas chromatography-mass spectrometry (GC-MS) [4,8,12,23,27,35,36,37,38]

  • For GC-MS analysis, the best instrumental conditions achieved with a BP-20 column were an oven temperature of 80 °C, ramp speed of 50 °C/min to a maximum of 220 °C, and gas flow rate of 1.0 mL/min

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Summary

Introduction

Fish constitute a complex system in which enzymatic, microbial, and physicochemical interactions occur simultaneously, which has an impact on flavor, texture, and shelf life (the time a product remains acceptable for consumption). After fish death and rigor mortis resolution, a succession of reactions takes place, which are of great importance for fish freshness and shelf life. These reactions are influenced by fish species, their physiological and environmental conditions, (e.g., water temperature), and will impact fish freshness and spoilage progress. Catching and harvesting methods will have a major influence on fish deterioration. Such alterations can arise from: (i) Chemical deterioration that can be non-enzymatic, enzymatic, or rancidity (oxidative or hydrolytic); (ii) physical changes that can have several forms, such as moisture loss; and (iii) microbiological changes by bacteria, fungi, viruses, and

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