Exploring New Horizons for Wine Grapes: Modulating Functional Effects by Varying Harvest Timing and Solar Exposure.

Grenache (GN) and Cabernet Sauvignon (CS) are two traditional red grape varieties widely cultivated in the Mediterranean area and both late-ripening cultivars, which makes them less sensitive to global warming conditions and more stable to harvest timing. Although different studies have evaluated the final antioxidant properties of grapes and pomaces, few studies have explored the effect of sun exposure and harvest on the nutritional and antioxidant properties of these products. This study investigates the control of sunlight and ripening as tools to tailor nutritional and antioxidant properties of grape juices (GJ) and their byproducts (pomace GP). The compositional analysis showed no significant (p ≥ 0.05) differences associated to either harvesting timing or exposure to sunlight for either of the two studied varieties. However, differences (p ≤ 0.05) were observed between varieties of protein and total dietary fibre (TDF). CS protein content ranged from 0.52 to 3.88 (g 100 g-1) in GJ and from 1.0 to 1.32 (g 100 g-1) in GP; meanwhile, GN had higher protein values in GJ (from 2.11 to 4.77 g 100 g-1) and GP (from 5.11 to 6.75 g 100 g-1). The opposite behaviour was observed in TDF; CS grape had higher values for juice (from 11.43 to 19.53 g 100 g-1) and pomace (from 42.20 to 65.80 g 100 g-1) than GN (from 11.43 to 17.22 g 100 g-1 in juice and from 25.90 to 54.0 g 100 g-1 in pomace). The total phenolic content (TP) in GP was 100 times higher than in the juices and showed a much less pronounced evolution compared to the GJ during the harvesting time. GN TP values ranged from 5835 to 8772 mg GAE 100 g-1; meanwhile, CS values ranged from 7637 to 9040 mg GAE 100 g-1. A significant (p ≤ 0.05) correlation between the TP total antioxidant capacity (TAC) results was observed, regardless of variety, harvesting time, and sunlight exposure. These findings show how the control of different factors can contribute to obtain modified grape-derived products from conventional varieties beyond the wine market.

Effect of Hopper Loading on the Formation of Alkyl Alcohols in Olive Fruits and Its Relationship with Sensory Quality Losses of Virgin Olive Oil.

The storage of olives in large hoppers is a widespread practice in oil mills, but these large volumes and their unloading can cause a physical deterioration of the olives that will affect the quality of the oil obtained. This research deals with the effect of hopper charge on the formation of alkyl alcohols in olive fruits and its relationship with the sensory quality losses of 'Arbequina' virgin olive oil. The contents of ethanol, methanol, and acetaldehyde were measured in olive samples loaded and stored for a short time in a large hopper and analyzed at three different hopper-discharging times, which are related to three different positions inside the hopper. The corresponding oil from each sampling was obtained by using ABENCOR and was evaluated by a trained tasting panel. Results showed that the ethanol content in olives increased during their storage in the hopper, while methanol and acetaldehyde contents did not show significant differences. Regarding their position in the hopper, fruits located at the bottom or on the lateral sides showed a greater deterioration. The sensory analyses showed an inverse relationship between the positive attributes of olive oils and their content of alcohols.

Monitoring the Evolution of the Aroma Profile of Lager Beer in Aluminium Cans and Glass Bottles during the Natural Ageing Process by Means of HS-SPME/GC-MS and Multivariate Analysis.

Headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry (HS-SPME/GC-MS), sensory evaluation, and multivariate analysis were applied to monitor and compare the evolution of the aromatic profile of a lager beer in different types of containers (aluminum cans and glass bottles) during the natural ageing process. Samples were aged naturally for a year in the absence of light with a controlled temperature of around 14 °C +/- 0.5 °C. The sensory evaluation applied was a blind olfactometric triangle test between canned and bottled samples at different periods of aging: fresh, 6 months, and 11 months. The sensory evaluation showed that the panelists were able to differentiate between samples, except for the fresh samples from the brewery. A total of 34 volatile compounds were identified using the HS-SPME/GC-MS technique for both packaging types in this experiment. The application of multivariate analysis to the GC-MS data showed that the samples could not be differentiated according to the type of packaging but could be differentiated by the ageing time. The results showed that the combination of sensory, HS-SPME-GC-MS, and multivariate analysis seemed to be a valuable tool for monitoring and identifying possible changes in the aroma profile of a beer during its shelf life. Furthermore, the results showed that storing beer under optimal conditions helped preserve its quality during its shelf life, regardless of the type of packaging (aluminum can and glass bottle).

Assessment of Variability Sources in Grape Ripening Parameters by Using FTIR and Multivariate Modelling.

The variability in grape ripening is associated with the fact that each grape berry undergoes its own biochemical processes. Traditional viticulture manages this by averaging the physicochemical values of hundreds of grapes to make decisions. However, to obtain accurate results it is necessary to evaluate the different sources of variability, so exhaustive sampling is essential. In this article, the factors "grape maturity over time" and "position of the grape" (both in the grapevine and in the bunch/cluster) were considered and studied by analyzing the grapes with a portable ATR-FTIR instrument and evaluating the spectra obtained with ANOVA-simultaneous component analysis (ASCA). Ripeness over time was the main factor affecting the characteristics of the grapes. Position in the vine and in the bunch (in that order) were also significantly important, and their effect on the grapes evolves over time. In addition, it was also possible to predict basic oenological parameters (TSS and pH with errors of 0.3 °Brix and 0.7, respectively). Finally, a quality control chart was built based on the spectra obtained in the optimal state of ripening, which could be used to decide which grapes are suitable for harvest.

Multivariate Analysis of the Influence of Microfiltration and Pasteurisation on the Quality of Beer during Its Shelf Life.

Gas chromatography-mass spectrometry (GC-MS), physicochemical and microbiological analyses, sensory descriptive evaluation, and multivariate analyses were applied to evaluate the efficiencies of microfiltration and pasteurization processes during the shelf life of beer. Samples of microfiltered and pasteurised beer were divided into fresh and aged groups. A forced ageing process, which consisted of storing fresh samples at 55° C for 6 days in an incubator and then keeping them under ambient conditions prior to analysis, was applied. Physicochemical analysis showed that both microfiltered and pasteurised samples had a slight variation in apparent extract, pH, and bitterness. The samples that underwent heat treatment had lower colour values compared with those that were microfiltered. Chromatographic peak areas of vicinal diketones increased in both fresh and aged samples. The results of the microbiological analysis revealed spoilage lactic acid bacteria (Lactobacillus) and yeasts (Saccharomyces and non-Saccharomyces) in fresh microfiltered samples. In the GC-MS analysis, furfural, considered by many authors as a heat indicator, was detected only in samples that underwent forced ageing and not in samples that were subjected to thermal pasteurisation. Finally, sensory analysis found differences in the organoleptic properties of fresh microfiltered samples compared with the rest of the samples.

An Overview of the Application of Multivariate Analysis to the Evaluation of Beer Sensory Quality and Shelf-Life Stability.

Achieving beer quality and stability remains the main challenge for the brewing industry. Despite all the technologies available, to obtain a high-quality product, it is important to know and control every step of the beer production process. Since the process has an impact on the quality and stability of the final product, it is important to create mechanisms that help manage and monitor the beer production and aging processes. Multivariate statistical techniques (chemometrics) can be a very useful tool for this purpose, as they facilitate the extraction and interpretation of information from brewing datasets by managing the connections between different types of data with multiple variables. In addition, chemometrics could help to better understand the process and the quality of the product during its shelf life. This review discusses the basis of beer quality and stability and focuses on how chemometrics can be used to monitor and manage the beer quality parameters during the beer production and aging processes.

Quantitation of endogenous amount of ethanol, methanol and acetaldehyde in ripe fruits of different Spanish olive varieties.

BACKGROUND: The use of healthy olives and their good management along the production process are necessary to obtain the best quality virgin olive oils. One parameter related to the health of the olives is the content of fatty acid alkyl esters. Because these come from the esterification of C16 and C18 free fatty acids with short chain alcohols, the control of methanol, ethanol and acetaldehyde (precursor of ethanol) and their origin (endogenous or from fermentation) is essential. The present study reports the endogenous amount of these compounds in some of the main Spanish olive varieties. For their analyses, headspace solid phase micro-extraction was applied and, to ensure quantitation reliability, the matrix-matched technique was used to build the calibration lines. RESULTS: For healthy and mature olives, the contents of ethanol and methanol are much higher and vary within a wider range than those corresponding to acetaldehyde. Because olives were not directly analyzed but previously homogenized, there was no correlation between the olive size parameters and the contents of the compounds investigated. However, these contents are characteristic of each variety. When comparing healthy and unhealthy olives, significant differences were only observed for ethanol contents. CONCLUSION: Higher contents of short alcohols are not only the result of an unhealthy or poor state of the fruits, but also the variety. Therefore, because these alcohols are precursors of fatty acid alkyl esters, the maximum permissible content of the latter should not be set at a single value for all olive varieties. © 2020 Society of Chemical Industry.

Prediction of olive oil sensory descriptors using instrumental data fusion and partial least squares (PLS) regression.

Headspace-Mass Spectrometry (HS-MS), Fourier Transform Mid-Infrared spectroscopy (FT-MIR) and UV-Visible spectrophotometry (UV-vis) instrumental responses have been combined to predict virgin olive oil sensory descriptors. 343 olive oil samples analyzed during four consecutive harvests (2010-2014) were used to build multivariate calibration models using partial least squares (PLS) regression. The reference values of the sensory attributes were provided by expert assessors from an official taste panel. The instrumental data were modeled individually and also using data fusion approaches. The use of fused data with both low- and mid-level of abstraction improved PLS predictions for all the olive oil descriptors. The best PLS models were obtained for two positive attributes (fruity and bitter) and two defective descriptors (fusty and musty), all of them using data fusion of MS and MIR spectral fingerprints. Although good predictions were not obtained for some sensory descriptors, the results are encouraging, specially considering that the legal categorization of virgin olive oils only requires the determination of fruity and defective descriptors.

Olive oil sensory defects classification with data fusion of instrumental techniques and multivariate analysis (PLS-DA).

Three instrumental techniques, headspace-mass spectrometry (HS-MS), mid-infrared spectroscopy (MIR) and UV-visible spectrophotometry (UV-vis), have been combined to classify virgin olive oil samples based on the presence or absence of sensory defects. The reference sensory values were provided by an official taste panel. Different data fusion strategies were studied to improve the discrimination capability compared to using each instrumental technique individually. A general model was applied to discriminate high-quality non-defective olive oils (extra-virgin) and the lowest-quality olive oils considered non-edible (lampante). A specific identification of key off-flavours, such as musty, winey, fusty and rancid, was also studied. The data fusion of the three techniques improved the classification results in most of the cases. Low-level data fusion was the best strategy to discriminate musty, winey and fusty defects, using HS-MS, MIR and UV-vis, and the rancid defect using only HS-MS and MIR. The mid-level data fusion approach using partial least squares-discriminant analysis (PLS-DA) scores was found to be the best strategy for defective vs non-defective and edible vs non-edible oil discrimination. However, the data fusion did not sufficiently improve the results obtained by a single technique (HS-MS) to classify non-defective classes. These results indicate that instrumental data fusion can be useful for the identification of sensory defects in virgin olive oils.

Data fusion methodologies for food and beverage authentication and quality assessment - a review.

The ever increasing interest of consumers for safety, authenticity and quality of food commodities has driven the attention towards the analytical techniques used for analyzing these commodities. In recent years, rapid and reliable sensor, spectroscopic and chromatographic techniques have emerged that, together with multivariate and multiway chemometrics, have improved the whole control process by reducing the time of analysis and providing more informative results. In this progression of more and better information, the combination (fusion) of outputs of different instrumental techniques has emerged as a means for increasing the reliability of classification or prediction of foodstuff specifications as compared to using a single analytical technique. Although promising results have been obtained in food and beverage authentication and quality assessment, the combination of data from several techniques is not straightforward and represents an important challenge for chemometricians. This review provides a general overview of data fusion strategies that have been used in the field of food and beverage authentication and quality assessment.

Identification of olive oil sensory defects by multivariate analysis of mid infrared spectra.

Mid-infrared (MIR) spectra (4000-600 cm(-1)) of olive oils were analyzed using chemometric methods to identify the four main sensorial defects, musty, winey, fusty and rancid, previously evaluated by an expert sensory panel. Classification models were developed using partial least squares discriminant analysis (PLS-DA) to distinguish between extra-virgin olive oils (defect absent) and lower quality olive oils (defect present). The most important spectral ranges responsible for the discrimination were identified. PLS-DA models were able to discriminate between defective and high quality oils with predictive abilities around 87% for the musty defect and around 77% for winey, fusty and rancid defects. This methodology advances instrumental determination of results previously only achievable with a human test panel.

Quantification of phenolic compounds during red winemaking using FT-MIR spectroscopy and PLS-regression.

We present a rapid method to quantify phenolic compounds all during the red winemaking process using Fourier transform mid-infrared (FT-MIR) spectroscopy and chemometrics. To get the reference values, we used the usual UV­vis spectroscopy methods, and the compounds studied were evaluated as total phenolic compounds (TPC), total anthocyanins (TA), and condensed tannins (CT). Sampling from five different grape varieties (Merlot, Tempranillo, Syrah, Cariñena, and Cabernet sauvignon), harvested at different ripening states, and monitored over 10 days of vinification produced a total of 600 spectra. These were used to build and validate four different predictive models by partial least-squares (PLS) regression. The spectral regions selected for each model were between 979 and 2989 cm(­1), and when selecting the most suitable one in each case, good values of performance parameters were obtained (R2(val) > 0.95 and RPD > 4.0 for TPC; R2(val) > 0.90 and RPD > 3.0 for TA; R2(val) < 0.8 and RPD < 3.0 for CT). Furthermore, also more specific PLS regression models for each phenolic parameter and each grape variety were developed using different regions with results similar to those obtained when dealing with all of the grape varieties. It is concluded that FT-MIR spectroscopy together with multivariate calibration could be a rapid and valuable tool for wineries to carry out the monitoring of phenolic compound extraction during winemaking.

Chemical characterization of commercial Sherry vinegar aroma by headspace solid-phase microextraction and gas chromatography-olfactometry.

The sensorial representativeness of the headspace solid-phase microextraction (HS-SPME) aroma extract from commercial Sherry vinegars has been determined by direct gas chromatography-olfactometry (D-GCO). Extracts obtained under optimal conditions were used to characterize the aroma of these vinegars by means of GCO and aroma extract dilution analysis (AEDA). Among the 37 different odorants determined, 13 of them were identified for the first time in Sherry vinegars: 2 pyrazines (3-isopropyl-2-methoxypyrazine, 3-isobutyl-2-methoxypyrazine), 2 sulfur compounds (methanethiol, dimethyl trisulfide), 1 unsaturated ketone (1-octen-3-one), 1 norisoprenoid (ß-damascenone), 1 ester (ethyl trans-cinnamate) and 6 aldehydes (2- and 3-methylbutanal, octanal, nonanal, (E)-2-nonenal and (E,E)-2,4-decadienal). The determination of the odor thresholds in a hydroacetic solution together with the quantitative analysis-which was also performed using the simple and fast SPME technique-allowed obtaining the odor activity values (OAV) of the aromatic compounds found. Thus, a first pattern of their sensory importance on commercial Sherry vinegar aroma was provided.

Determination of roasted pistachio (Pistacia vera L.) key odorants by headspace solid-phase microextraction and gas chromatography-olfactometry.

Key odorants in roasted pistachio nuts have been determined for the first time. Two different pistachio varieties (Fandooghi and Kerman) have been analyzed by means of headspace solid-phase microextraction (HS-SPME) and gas chromatography-olfactometry (GCO). The aroma extract dilution analyses (AEDA) applied have revealed 46 and 41 odor-active regions with a flavor dilution (FD) factor≥64 for the Fandooghi and the Kerman varieties, respectively, and 39 of them were related to precisely identified compounds. These included esters, pyrazines, aldehydes, acids, furans, and phenols. The results show that the Fandooghi variety presents, not only more odor-active regions but also higher FD factors than the Kerman variety that can lead to the conclusion that the first variety has a richer aromatic profile than the second one. The descriptive sensory analysis (DSA) showed that the roasted, chocolate/coffee, and nutty attributes were rated significantly higher in the Fandooghi variety, whereas the green attribute was significantly higher in the Kerman one.

Application of FT-MIR spectroscopy for fast control of red grape phenolic ripening.

The content of phenolic compounds determines the state of phenolic ripening of red grapes and is a key criterion in setting the harvest date to produce quality red wines. In this study, the feasibility of Fourier transform mid-infrared (FT-MIR) spectroscopy combined with partial least-squares (PLS) regression to quantify phenolic compounds is reported. The reference methods used for quantifying these compounds (which were evaluated as total phenolic compounds, total anthocyanins, and condensed tannins) were the usual ones used in cellars that employed UV-vis spectroscopy. To take into account the high natural variability of grapes when building the calibration models, fresh grapes from six varieties, at different phenolic ripening states were harvested during three vintages. Destemmed and crushed grapes were subjected to an accelerated extraction process and used as calibration standards. A total of 192 extracts (objects) were obtained, and these were divided into a training set (106 objects) and a test set (86 objects) to evaluate the predictive ability of the models. Among the different MIR regions of the extract raw spectra, those that provided the highest variability on the absorption were selected. The results showed that the best PLS regression model was the one obtained when working in the region of 1168-1457 cm(-1) because it gave the most accurate and robust prediction for total phenolic compounds (RMSEP%=4.3 and RPD=4.5), total anthocyanins (RMSEP%=5.9 and RPD=3.5), and condensed tannins (RMSEP%=5.8 and RPD=3.8). Therefore, it can be concluded that FT-MIR spectroscopy can be a fast and reliable technique for monitoring the phenolic ripening in red grapes during the harvest period.

Comparative study of two extraction techniques to obtain representative aroma extracts for being analysed by gas chromatography-olfactometry: application to roasted pistachio aroma.

This research paper presents a comparative study of two different extraction and concentration techniques to obtain representative pistachio aroma extracts: the traditional direct solvent extraction (DSE) followed by high-vacuum transfer (HVT) and the headspace solid-phase microextraction (HS-SPME). The results showed that, although both techniques provide accurate information about the aromatic composition that will be perceived by the consumer, the precision in terms of within-day repeatability and between-days repeatability (intermediate precision) of the chromatographic areas presented better values for HS-SPME than for DSE-HVT. Moreover the solvent-free HS-SPME allows the extraction of more odour-active regions, requires very little sample handling and shorter time for sampling.

Comparison of three extraction methods used to evaluate phenolic ripening in red grapes.

Because there is not a single method for carrying out phenolic ripening analysis, it is very difficult to compare the results obtained by different researchers. In this study, the three most widely used extraction methods of polyphenols (Glories, AWRI, and ITV) have been analytically compared by evaluating two of the most important parameters for the wine industry: total polyphenols and total anthocyanins. Samples from different grape varieties (Tempranillo, Garnacha, Carinena, Syrah, Merlot, and Cabernet Sauvignon), from three different vintages (2006, 2007, and 2008), and at different ripening states (from the beginning of ripeness until harvest) were analyzed to obtain a wide range of representative phenolic contents. To avoid external interferences on the comparisons, the same grape puree was used to make the maceration assays using the different solvents according to each extraction method. Although every extraction method exhibits a different extraction efficiency, the correlation between the results obtained with each one was very good both for total anthocyanins and for total polyphenols. Thus, after having determined a parameter value of the phenolic ripeness using a specific method, the relationship found can be used to predict the parameter value of the phenolic ripeness provided by the other two methods.

Release and perception of ethyl butanoate during and after consumption of whey protein gels: relation between textural and physiological parameters.

The influence of gel texture on parameters such as positioning of food material in the oral cavity during mastication, and salivation, and their influence on aroma release in vivo was studied. Retronasal perception was followed by means of time-resolved sensory evaluation, while volatile release patterns were observed by means of PTR-MS. A clear correlation was found between individual-specific consumption patterns and the respective sensory perception. Also, gel texture could be clearly correlated with respective physicochemical release patterns in vivo and to the corresponding retronasal aroma perception.

Investigation of the retronasal perception of strawberry aroma aftersmell depending on matrix composition.

The development of strawberry aroma aftersmell after consumption in aqueous and milk model systems was followed. A recently developed sensory approach was used to seize the qualitative, quantitative, and temporal aspects of aroma profile development. The results obtained from sensory evaluation were then correlated to analytical data, obtained by means of intraoral aroma detection using the buccal odor screening system (BOSS). A clear correlation was found between the sensory persistence of single odor impressions and the intraoral detectability of odorants by BOSS. For the strawberry aroma mixture it could be shown that BOSS is capable of selecting those odorants of a complex aroma mixture that elicit a certain aftersmell impression developing after a certain period of time in the oral cavity. Also, the changes in in vivo odorant persistence depending on changes in food matrix composition could be directly followed by means of BOSS.

Aroma release and retronasal perception during and after consumption of flavored whey protein gels with different textures. 1. in vivo release analysis.

The influence of gel texture on retronasal aroma release during mastication was followed by means of real-time proton-transfer reaction mass spectrometry and compared to sensory perception of overall aroma intensity. A clear correlation was found between individual-specific consumption patterns and the respective physicochemical release patterns in vivo. A modified data analysis approach was used to monitor the aroma changes during the mastication process. It was found that the temporal resolution of the release profile played an important role in adequate description of the release processes. On the basis of this observation, a hypothesis is presented for the observed differences in intensity rating.