Abstract

A novel sample preparation method based on the use of the Arrow solid-phase microextraction device was used to extract and preconcentrate volatile organic compounds (VOCs) from milk samples prior to their determination by gas chromatography–mass spectrometry (GC-MS). The experimental parameters of the solid-phase microextraction (SPME) Arrow method were evaluated in terms of fiber type, sample volume, extraction temperature, extraction time, stirring rate and salt addition. Under the optimum extraction conditions, the SPME Arrow was compared with conventional SPME fibers to evaluate the effectiveness of the SPME Arrow method. Evaluation of the conventional SPME procedure was also performed under optimized conditions, for appropriate method comparison. Due to the larger sorption phase volume of SPME Arrow, a higher sensitivity and reproducibility were observed for the determined chromatographic peaks in comparison with conventional SPME fibers. The use of Carbon wide range (WR) SPME Arrow/polydimethylsiloxane (CAR/PDMS) SPME Arrow fibers leads to a compound-dependent improvement of a factor of 4–5x over the classical SPME setup. Moreover, the relative standard deviation (RSD) of the total volatiles for a conventional SPME procedure was 12.5%, while for SPME Arrow it was 6.2%. Finally, the novel method was successfully employed for the analysis of commercially available milk samples. The findings of this study indicate that SPME Arrow can be effectively used for the determination of volatile organic compounds in complex food matrixes.

Highlights

  • Volatile organic compounds (VOCs) count among the most important compounds in foods, since they determine the sensory characteristics of the food, which are closely related to the acceptance or preference of particular food varieties [1]

  • The findings of this study indicate that solid-phase microextraction (SPME) Arrow can be effectively used for the determination of volatile organic compounds in complex food matrixes

  • We developed a sensitive and reproducible method for determining VOCs in milk samples based on the use of the headspace SPME Arrow technique

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Summary

Introduction

Volatile organic compounds (VOCs) count among the most important compounds in foods, since they determine the sensory characteristics of the food, which are closely related to the acceptance or preference of particular food varieties [1]. The determination of VOCs in foods is of high importance in order to understand their origins, to evaluate the aroma profile differences among similar foods and to ensure food safety and quality. Due to the presence of a plethora of VOCs in largely varying concentrations, the determination of the volatile profile in complex food matrices is considered difficult. Individual VOCs may have very high odor activities and may contribute to the characteristic flavor of a given food even at very low concentrations [2]. Typical examples of solvent extraction techniques include conventional solvent extraction, vacuum distillation, simultaneous distillation extraction (SDE/Likens–Nickerson extraction) and solvent-assisted flavor evaporation (SAFE), while

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