Sub-ambient temperature sampling of fish volatiles using vacuum-assisted headspace solid phase microextraction: Theoretical considerations and proof of concept.
[en] The extraction of volatiles from perishable food at a sub-ambient temperature using headspace solid-phase microextraction (HS-SPME) has not been considered in the past due to the corresponding loss in sensitivity. We propose HS-SPME sampling under vacuum (Vac-HS-SPME) to compensate problems of sensitivity loss and achieve substantial improvement in extraction efficiencies whilst sampling at temperatures as low as 5 °C. The approach was applied to fish samples, representing a highly vulnerable perishable food sample. The theoretical considerations explaining the performance of Vac-HS-SPME at sub-ambient temperatures are discussed and related to the increase in gas diffusivities when sampling under vacuum. A comparative study between Vac- and regular HS-SPME for the extraction of 18 compounds from salmon was carried out at different temperatures (5, 30 and 40 °C) and sampling times (10-60 min). For the majority of the compounds, Vac-HS-SPME at 5 °C yielded similar or superior extraction efficiencies than regular HS-SPME even when sampling at 40 °C. However, four compounds were better extracted at 1 atm presumably due to the intensification of competitive adsorption of analytes on the SPME fiber under vacuum or the partial losses of more volatile analytes during air-evacuation in the presence of the frozen samples. Sub-ambient temperature sampling (5 °C) combined with Vac-HS-SPME was also applied to monitor the changes in the 18 compounds present in salmon, redfish, and cod refrigerated for up to five days. The results were compared to those obtained with regular HS-SPME at 40 °C. Overall, Vac-HS-SPME sampling at 5 °C represents a new and powerful approach for the analysis of volatiles in refrigerated foods, and has a great potential for future studies in quality control and freshness assessment.
Disciplines :
Chemistry Food science
Author, co-author :
Delbecque, Nathalie; Gembloux Agro-Bio Tech, University of Liège, Gembloux, 5030, Belgium
Mascrez, Steven ; Université de Liège - ULiège > Département GxABT > Chimie des agro-biosystèmes
Psillakis, Elefteria ; Laboratory of Aquatic Chemistry, School of Chemical and Environmental Engineering, Technical University of Crete, GR-73100, Chania, Greece. Electronic address: elia@enveng.tuc.gr
Purcaro, Giorgia ; Université de Liège - ULiège > TERRA Research Centre > Chimie des agro-biosystèmes
Language :
English
Title :
Sub-ambient temperature sampling of fish volatiles using vacuum-assisted headspace solid phase microextraction: Theoretical considerations and proof of concept.
The authors are grateful to Millipore Sigma, The life science business of Merck KGaA for providing the SPME fibers. The authors wish to thank the fish shop “Pitsikakis Nikos” (Chania, Crete, Greece) for providing fish samples during initial screening tests. This article is based upon work from the Sample Preparation Study Group and Network, supported by the Division of Analytical Chemistry of the European Chemical Society. This article is based upon work from COST Action CA 16215, supported by COST (European Cooperation in Science and Technology, http://www.cost.eu).The authors are grateful to Millipore Sigma, The life science business of Merck KGaA for providing the SPME fibers. The authors wish to thank the fish shop “Pitsikakis Nikos” (Chania, Crete, Greece) for providing fish samples during initial screening tests. This article is based upon work from the Sample Preparation Study Group and Network, supported by the Division of Analytical Chemistry of the European Chemical Society . This article is based upon work from COST Action CA 16215 , supported by COST ( European Cooperation in Science and Technology , http://www.cost.eu ).
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