Abstract

Static headspace is an easy to perform, convenient, and usually automated method for extraction of volatiles from various food matrices. Among other applications, it is used also for monitoring of volatile lipid oxidation products. However, the biggest disadvantage of this method is its low sensitivity especially when compared to such techniques as solid-phase microextraction or dynamic headspace. This paper focuses on the comparison of static headspace analysis of volatile lipid oxidation products with a modification of this technique, where volatiles extracted multiple times from oil matrix in a headspace vial are trapped on Tenax trap and subsequently desorbed into gas chromatograph. Twenty volatile compounds (mainly alkanals, 2-alkenals, ketones, and alcohols being volatile lipid oxidation products) in rapeseed oil were used for method comparison. For all compounds, a significant increase in method sensitivity and improvement of limits of detection (10 to 33 times) depending on the compound were noted; however, the repeatability was worse (for 16 out of 20 compounds) and carry-over values (also 16/20) were higher for combined headspace/trapping method.

Highlights

  • Aldehydes are volatile compounds which may indicate the deterioration of food, especially of fat rich foods as a result of processing, storage, or seed pre-treatment

  • Headspace techniques such as static or dynamic headspace (SHS or DHS, respectively), headspace sorptive extraction (HSSE), solid-phase microextraction (SPME), and direct thermal desorption (DTD) are robust methods which do not require the use of a solvent or circumstances which impede obtaining a pure volatile compound extract of the analyzed sample (Bylaite and Meyer 2006; Cavalli et al 2003)

  • The aim of the study was to compare the extraction of volatile lipid oxidation products (VLOP) from rapeseed oil using static headspace method, in which typical loop transfer for compound injection was used, with a combination of headspace method in which compounds can be extracted multiple times from a headspace vial into a Tenax trap before transferring them into gas chromatograph

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Summary

Introduction

Aldehydes are volatile compounds which may indicate the deterioration of food, especially of fat rich foods as a result of processing, storage, or seed pre-treatment. Employment of high temperature for the isolation of volatile compounds using distillation methods may result in their degradation, or in formation of artifacts Headspace techniques such as static or dynamic headspace (SHS or DHS, respectively), headspace sorptive extraction (HSSE), solid-phase microextraction (SPME), and direct thermal desorption (DTD) are robust methods which do not require the use of a solvent or circumstances which impede obtaining a pure volatile compound extract of the analyzed sample (Bylaite and Meyer 2006; Cavalli et al 2003). Each of these methods enables the isolation of volatile compounds usually without artifacts’ formation. HSSE and SPME are solvent-free methods based on various stationary

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