scholarly journals A Systematic AQbD Approach for Optimization of the Most Influential Experimental Parameters on Analysis of Fish Spoilage-Related Volatile Amines

Foods ◽  
2020 ◽  
Vol 9 (9) ◽  
pp. 1321
Author(s):  
Jorge Freitas ◽  
Pedro Silva ◽  
Paulo Vaz-Pires ◽  
José S. Câmara

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.

2008 ◽  
Vol 91 (6) ◽  
pp. 1409-1415 ◽  
Author(s):  
Rosa Ana Pérez ◽  
Maria Dolores Rojo ◽  
Gema Gonzlez ◽  
Cristina De Lorenzo

Abstract A method using solid-phase microextraction (SPME) and gas chromatography/mass spectrometry was developed and applied to the determination of volatile compounds generated in meat, at different times, from ground beef stored under refrigeration. Selection of the extractive fiber, extraction time, and headspace (HS) or direct extraction was optimized for the determination of volatile compounds from ground meat. Various fibers were investigated, and carboxen/polydimethylsiloxane was selected for these analyses. The HS analysis of the solid sample by HS-SPME produced a higher volatile signal than did direct-SPME. The meat samples were stored under refrigeration and analyzed after 0, 3, and 6 days of storage. These analyses at different times showed important changes in the volatile profile of the evaluated samples. The ketones 3-hydroxy-2-butanone and 2,3-butanedione, and the alcohol 3-methyl-1-butanol were the most representative compounds generated during the meat storage. In general, compounds associated with a butter off-flavor were detected during the storage of raw ground beef.


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