Aroma compounds static headspace methods

Some static headspace methods do not require an external calibration and are based on measurements performed at thermodynamic equilibrium between liquid and gas phase. In the phase ratio variation method (PRV) described by Ettre and Collaborators (1993), the partition coefficient calculation is based on the fact that the headspace concentration changes as a function of the phase volume ratio (gas and liquid phases), while the partition coefficient remains constant. This method has been recently applied to study the interactions between aroma compounds and macromolecules in different food systems (Savary et al. 2006, 2007) but so far not to the wine. 

The highly volatile odorants are not detected or are underestimated when the screening method is applied to an aroma extract. These compounds are lost when the extract is concentrated or they are masked in the gas chromatogram by the solvent peak. To overcome this limitation, the screening has to be completed by GC-O of static headspace samples (GCOH Fig. 16.3) [59-61]. 

For a compound to contribute to the aroma of a food, the compound must have odor activity and volatilize from the food into the head-space at a concentration above its detection threshold. Since aroma compounds are usually present in a headspace at levels too low to be detected by GC, headspace extraction also requires concentration. SPME headspace extraction lends itself to aroma analysis, since it selectively extracts and concentrates compounds in the headspace. Some other methods used for sample preparation for aroma analysis include purge-and-trap or porous polymer extraction, static headspace extraction, and solvent extraction. A comparison of these methods is summarized in Table Gl.6.2. 

Athes et al. (2004) compared the data from three static headspace methodologies (VPC, PRV and LC-SH) for determining gas/liquid partition coefficients of two aroma compounds in hydroalcoholic, multicomponent solutions at infinit dilution. They found that PRV was a simpler method compared to VPC and LC-SH and that VPC and PRV were more accurate than LC-SH since errors due to gas leaks and adsorption in gastight syringes are avoided. They suggested that these issues could be responsible for significant bias (50% lower values) obtained when using the LC-SH method. Nevertheless, all three methods were able to find an effect of ethanol (up to 20%) on the release of aroma compounds from their model system (Fig. 8F.1). 

A consideration of volatility as a means of aroma isolation requires an appreciation for the factors that influence the amount (or proportion) of an aroma compound in the gaseous phase vs. in the food at equilibrium (static headspace isolation methods) and nonequiUbrium conditions (dynamic headspace isolation methods). In both cases, our methodology requires that the aroma compound partitions into the gas phase for isolation. Considering equilibrium conditions first, the amount of an aroma compound in the gaseous phase is defined by the gas food partition coefficient (kg,). This can be most simply expressed as ... 

The aim of GC-0 techniques in food aroma research is to determine the relative odor potency of compounds present in the aroma extract. This method gives the order of priority for identification and thus indicates the chemical origin of olfactory differences (7). The value of the results obtained by GC-O depends directly on the effort invested in sample preparation and analytical conditions. Analysis of an aroma extract by dilution techniques (AEDA, Charm) combined with static headspace GC-O provides a complete characterization of the qualitative aroma composition of a food. However, this is only the first step in understanding the complex aroma of a food. 

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