María Ángeles Pozo-Bayón

Polydimethylsiloxane solid-phase microextraction-gas chromatography method for the analysis of volatile compounds in wines. Its application to the characterization of varietal wines.

A study was made of the validity of the solid-phase microextraction method, using a polydimethylsiloxane coated fused-silica fiber, for the extraction-desorption of the minor volatile compounds from wine before their gas chromatographic analysis. The aspects considered were the influence of ethanol on extraction, repeatability, limits of detection, linearity and recovery of compounds. This method, together with the direct injection of the major volatile compounds, was applied to 16 varietal wines. The findings indicate that the method is a highly suitable technique for the analysis of wines and that the volatile composition of wines depends, at least partly, on the grapes with which they have been made.

Flavor Control in Baked Cereal Products

Baked cereal products represent one of the most consumed foodstuffs in the world. Extensive scientific research has been focused on the volatile composition of these types of products. It has been shown that in spite of the great number of compounds identified, only a small number of them are responsible for the aroma. Many factors can affect the aroma composition of baked cereal products and different strategies have been proposed to improve the endogenous aroma. Furthermore, the addition of exogenous aroma compounds is extensively employed when baked cereal products with special traits are required. This article reviews the different ways in which the aroma is generated in baked cereal products and the methods that can be used to control or modify their flavor, as well as the problems related to the flavoring and the different approaches that flavor technologists have proposed to solve these problems. Some important issues and directions for future research in the flavor of baked cereal products are listed.

Analytical performance of three commonly used extraction methods for the gas chromatography-mass spectrometry analysis of wine volatile compounds.

The analytical performance of three extraction procedures based on cold liquid-liquid extraction using dicloromethane (LLE), solid phase extraction (SPE) using a styrene-divinylbenzene copolymer and headspace solid phase microextraction (SPME) using a carboxen-polydimethylsiloxane coated fibre has been evaluated based on the analysis of 30 representative wine volatile compounds. From the comparison of the three procedures, LLE and SPE showed very good linearity covering a wide range of concentrations of wine volatile compounds, low detection limits, high recovery for most of the volatile compounds under study and higher sensitivity compared to the headspace-SPME procedure. The latter showed in general, poor recovery for polar volatile compounds. Despite some drawbacks associated with the LLE and SPE procedures such as the more tedious sampling treatment and the use of organic solvents, the analytical performance of both procedures showed that they are more adequate for the analysis of wine volatiles.

Interactions Between Wine Matrix Macro-Components and Aroma Compounds

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Impact of the nonvolatile wine matrix composition on the in vivo aroma release from wines.

The impact of the nonvolatile wine matrix composition on the retronasal aroma release of four volatile compounds added to different types of wines has been evaluated. For this purpose, a tailor-made retronasal aroma trapping device (RATD) was used to entrap the exhaled breath of six panelists previously trained in a specific consumption procedure. Five wines of different composition (white wine, sparkling white wine, young red wine, aged red wine, and a sweet wine) were evaluated. Prior to the evaluation, with the exception of the sweet wine, the wines were adjusted to the same ethanol content and aromatized with a mixture of four target volatile compounds. Aroma release data were submitted to multivariate statistical analysis in order to relate wine chemical composition and aroma release during wine drinking. Results showed interindividual differences and a clustering of panelists among lower and higher aroma releasers, which was in agreement to the differences in their breathing capacity. A significant influence of the matrix composition in the low aroma releasers group during wine consumption was observed. The consumption of red wines provoked a significantly higher aroma release than the consumption of white and sweet wines. From the chemical composition determined in the wine samples (pH, total acidity, total polyphenols, neutral polysaccharides, residual sugar, and nitrogenous compounds), the amount of total polyphenols was better correlated with the observed effect.

Influence of complexation between amylose and a flavored model sponge cake on the degree of aroma compound release.

Flavoring is used in the food industry to reinforce the aroma profile of baked cereal goods. During the processing of such products, interactions between starch and aroma compounds can occur, and this may have an impact on aroma release and perception. In the present study, 20 aroma compounds were tested to establish whether they formed complexes with amylose. The structure of the complexes was determined by wide-angle X-ray scattering (WAXS). A cocomplexation study proved that several complexing compounds could be present in the same crystalline aggregate. WAXS and differential scanning calorimetry (DSC) experiments were performed in a flavored model sponge cake at different steps of processing and showed that aroma compounds might form complexes with amylose in a sponge cake as they can do in simple system containing only amylose. Some of the aroma compounds trapped in the sponge cake were quantified, and their release behavior was followed by headspace analysis. The V-type structure could partly explain aroma retention in the product and the rate of aroma release.

Determining specific food volatiles contributing to PTR-MS ion profiles using GC-EI-MS.

This work focused on developing a method to determine the volatile compounds that contribute to individual masses observed by PTR-MS in the headspace of a food product (e.g., cheese crackers). The process of interfacing a PTR-MS with a GC-MS (electron impact) through an existing sniffing port is outlined, and the problems faced in doing so are discussed. For the interface developed, linearity for both detectors working online for a wide range of concentrations of a selected compound (hexanal) was good (R(2) = 0.88). There was also a good correlation between the responses for both instruments (confidence interval for the slope between 0.56 and 1.18) over a range in concentrations despite the different ionization processes taking place. The application of our system (PTR-MS/GC-MS interface) to a real food system (cheese crackers) in which volatiles were isolated via purge and trap allowed the assignments of most of the PTR-MS masses to major volatile compounds in the samples. However, in this interface it is important to consider some limitations related to GC resolution, compound identification by EI-MS, PTR-MS sensitivity (and overloading), PTR-MS inlet requirements (ca. 20 mL/min), ion chemistry in the PTR-MS, and potentially changing sample composition over time, altering the contribution of a given compound to a specific ion. These issues are discussed.

Feasibility and application of liquid-liquid extraction combined with gas chromatography-mass spectrometry for the analysis of phenolic acids from grape polyphenols degraded by human faecal microbiota.

In this study the feasibility of a LLE-GC-EI-MS method for the analysis of 43 phenolic acids belonging to different chemical structure families which have been described in the literature as microbial-derived metabolites after consumption of dietary polyphenols was proved. In addition, the method was applied for the characterisation of phenolic metabolites resulting from the incubation, in anaerobic conditions, of a commercial grape seed extract (GSE) and their corresponding flavan-3-ol monomeric (GSE-M) and oligomeric (GSE-O) fractions with human faeces from healthy volunteers (n=3). The method showed average values of repeatability and reproducibility of 5.0% and 6.3%, respectively, adequate and low detection (1.8-30.8 μg L(-1)) and quantification limits (6.0-102.8 μg L(-1)) and good recovery values (95%, as average value). A total of 27 phenolic acids were identified in the faecal solutions after incubation with the grape seed extracts. In general, faecal samples incubated with GSE and GSE-M (monomeric fraction) yield a higher formation of phenolic acids compared to the samples incubated with the oligomer fraction (GSE-O).

Impact of Using New Commercial Glutathione Enriched Inactive Dry Yeast Oenological Preparations on the Aroma and Sensory Properties of Wines

The effect of the addition of a commercial enriched glutathione inactive dry yeast oenological preparation in the volatile and sensory properties of industrially manufactured rosé Grenache wines was evaluated during their shelf-life. In addition, triangle tests were performed at different times during wine aging (among 1 and 9 months) to determine the sensory differences between wines with and without glutathione inactive dry yeast preparations. Descriptive sensory analysis with a trained panel was carried out when sensory differences in the triangle test were noticed. In addition, consumer tests were performed in order to investigate consumers’ acceptability of wines. Results revealed significant sensory differences between control and glutathione inactive dry yeast wines after 9 months of aging. At that time, glutathione inactive dry yeast wines were more intense in fruity aromas (strawberry, banana) and less intense in yeast notes than control wine. The impact of the glutathione inactive dry yeast in the aroma might be the consequence of different effects that these preparations could induce in wine composition: modification of yeast byproducts during fermentation, release of volatile compounds from inactive dry yeast, interaction of wine volatile compounds with yeast macromolecules from inactive dry yeast and a possible antioxidant effect of the glutathione released by the inactive dry yeast preparation on some specific volatile compounds.

Targeted Metabolomic Analysis of Polyphenols with Antioxidant Activity in Sour Guava (Psidium friedrichsthalianum Nied.) Fruit

Psidium is a genus of tropical bushes belonging to the Myrtaceae family distributed in Central and South America. The polar extract of Psidium friedrichsthalianum Nied. was partitioned with ethyl ether, ethyl acetate, and n-butanol, and the total phenolic content and antioxidant activity were measured by Folin-Ciocalteu and ABTS assays, respectively. The ethyl acetate fraction exhibited both the highest phenolic content and antioxidant activity. Due to the complexity of this fraction, an analytical method for the comprehensive profiling of phenolic compounds was done by UPLC-ESI/QqQ in MRM (multiple reaction monitoring) mode. In this targeted analysis, 22 phenolic compounds were identified, among which several hydroxybenzoic, phenylacetic, and hydroxycinnamic acid derivatives were found. This is the first time that (+)-catechin, procyanidin B1, procyanidin B2, and (−)-epicatechin have been reported as constituents of sour guava. A fractionation by exclusion size, C18-column chromatography, and preparative RRLC (rapid resolution liquid chromatography) allowed us to confirm the presence of ellagic acid and isomeric procyanidins B, well-known bioactive compounds. The content of phenolic compounds in this fruit shows its potential for the development of functional foods.