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Raquel M. Callejón - One of the best experts on this subject based on the ideXlab platform.
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Spectralprint techniques for Wine and vinegar characterization, authentication and quality control: Advances and projections
TrAC Trends in Analytical Chemistry, 2021Co-Authors: Rocío Ríos-reina, Raquel M. Callejón, José Manuel Camiña, Silvana Mariela AzcarateAbstract:Abstract The current review focuses on the use of the most popular spectroscopic techniques applied for Wine and Wine vinegar characterization, authentication, and quality control. The ever-increasing trend in the advance on untargeted analysis by spectroscopy analytical platforms, to obtain the so-called “fingerprint”, is showed. Moreover, the synergistic relationship with chemometric approaches as fast analytical methodologies able to solve these challenging analytical issues is put on stage. In this context, a critical change in the terminology fingerprint by spectralprint is discussed. In addition, a deep knowledge about advantages and weaknesses of each spectroscopy technique is presented. The advance of data handling and data modelling applications and updating about the latest chemometric tools and strategies to better exploit the acquired spectroscopy data from current instrumentation are also exposed. Finally, novelty prospects in Wines and Wine Vinegars analysis are revealed.
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Assessment of UV–visible spectroscopy as a useful tool for determining grape-must caramel in high-quality Wine and balsamic Vinegars
Food Chemistry, 2020Co-Authors: Rocío Ríos-reina, Silvana Mariela Azcarate, José Manuel Camiña, Raquel M. CallejónAbstract:Abstract The addition of E-150d caramel, known as grape-must caramel in Vinegars, is a legal but without limitation practice in Spanish Wine Vinegars, as those with a protected designation of origin (PDO), for unifying the final colour of different batches and barrels. It is also used in the production of ‘Balsamic vinegar of Modena’ Vinegars, with a maximum addition fixed at 2% v/v by law. Although its quantification in Vinegars was studied by other techniques, there is still not any official method for it. Therefore, UV–vis spectroscopy was assessed as a quick analytical method able to quantify grape-must caramel in Balsamic Vinegars of Modena and Spanish PDO Wine Vinegars. Univariate and multivariate calibrations were assessed for this quantification. Results demonstrated the ability of UV–vis spectroscopy coupled with multivariate calibration in the quantification of grape-must caramel, predicting caramel amounts under 2% v/v in both Balsamic and PDO Wine Vinegars.
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Sensory and spectroscopic characterization of Argentinean Wine and balsamic Vinegars: A comparative study with European Vinegars.
Food chemistry, 2020Co-Authors: Rocío Ríos-reina, Silvana Mariela Azcarate, José Manuel Camiña, Raquel M. CallejónAbstract:Abstract In Argentina, Vinegars are cheap agro-food products without exhaustive regulation and the production of high-quality Vinegars has not been exploited yet. In fact, Argentinean Vinegars have not been studied. In this context, a first study of Argentinean balsamic and Wine Vinegars was carried out by a sensory and spectroscopic characterization and by a comparison with well-recognized European Vinegars. For that, ultraviolet–visible and fluorescence spectroscopies were applied together with principal component analysis (PCA) and parallel factor analysis (PARAFAC) performed on each data set, respectively. Results showed differences between acetification processes, origin countries and a wide variability within Argentinean production. The sensory characterization on Argentinean Wine Vinegars was performed by triangular and ordering preference tests showing statistically significant preferences toward the traditional and the rapid Vinegars. This work highlights the effect of production on quality in order to provide added value to the Argentinean Vinegars.
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Characterization of the aroma profile and key odorants of the Spanish PDO Wine Vinegars
Food chemistry, 2019Co-Authors: Rocío Ríos-reina, M. Lourdes Morales, M. Pilar Segura-borrego, Raquel M. CallejónAbstract:Abstract The aroma profiles of Spanish Wine Vinegars with Protected Designation of Origin (PDO) were described and compared for the first time by gas chromatography–mass spectrometry–olfactometry (GC–MS–O), odor-active values (OAVs) and quantitative descriptive analysis (QDA). Vinagre de Jerez Reserva (JRE) showed higher percentage of ‘grassy-vegetal’ impact odorants, while ‘spicy’ compounds highlighted the Pedro Ximenez category (JPX). Vinagre de Montilla-Moriles Reserva (MRE) had ‘buttery-lactic’ impact odorants, while ‘empyreumatic’ and ‘sweet’ aromas stood out for Pedro Ximenez category (MPX). Vinagre de Condado de Huelva Reserva (CRE) showed a stronger percentage of ‘chemical’ impact odorants. The key odorants were ethyl propionate, ethyl octanoate, propanoic acid and 4-ethylphenol for JRE, diacetyl and methional/furfural for JPX, acetoin for MRE, ethyl phenylacetate and vanillin for MPX and acetaldehyde diethyl acetal, isobutyl acetate, ethyl isovalerate and guaiacol for CRE. A good relation among the impact odorants and the sensory descriptors was observed.
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A comparative study of the volatile profile of Wine Vinegars with protected designation of origin by headspace stir bar sorptive extraction.
Food research international (Ottawa Ont.), 2019Co-Authors: Rocío Ríos-reina, Diego L. García-gonzález, M. Lourdes Morales, M. Pilar Segura-borrego, Raquel M. CallejónAbstract:Abstract The characteristic volatile profile of the Spanish Vinagre de Jerez (VJ), Vinagre de Condado de Huelva (VC) and Vinagre de Montilla-Moriles (VMM) protected designation of origin (PDO) Wine Vinegars has been studied and compared for the first time by headspace stir bar sorptive extraction-gas chromatography–mass spectrometry (HSSE-GC–MS). The possible markers of each category and PDO were assessed. Acetates were the majority group in all Vinegars, while ketones, C13-norisoprenoids and volatile phenols showed significant differences between the three PDOs. Analysis of variance (ANOVA), heatmap and partial least squares-discriminant analysis (PLS-DA) were performed. According to these results, 1-heptanol, methyl nonanoate, 2-methylbutanoic acid, 2,2,6-trimethyl-cyclohexanone, trans-2-decenal, eucalyptol and α-terpineol, were the most significant compounds for differentiating of VC, diacetyl and acetoin, ethyl 3-ethoxypropanoate, 2- and 3-heptanone, 2-methyl-1-hexadecanol, 1-octen-3-ol, p-Cresol and camphene for VMM; and β-damascenone, 5-hydroxymethylfurfural, 3-heptanol, trans-2-hexen-1-ol and trans-2-hexen-1-yl acetate for VJ. Classification results showed that 100% of PDO samples were correctly classified, reaffirming the utility of the volatile profiles for classifying and authenticating Wine vinegar PDOs.
Rocío Ríos-reina - One of the best experts on this subject based on the ideXlab platform.
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Spectralprint techniques for Wine and vinegar characterization, authentication and quality control: Advances and projections
TrAC Trends in Analytical Chemistry, 2021Co-Authors: Rocío Ríos-reina, Raquel M. Callejón, José Manuel Camiña, Silvana Mariela AzcarateAbstract:Abstract The current review focuses on the use of the most popular spectroscopic techniques applied for Wine and Wine vinegar characterization, authentication, and quality control. The ever-increasing trend in the advance on untargeted analysis by spectroscopy analytical platforms, to obtain the so-called “fingerprint”, is showed. Moreover, the synergistic relationship with chemometric approaches as fast analytical methodologies able to solve these challenging analytical issues is put on stage. In this context, a critical change in the terminology fingerprint by spectralprint is discussed. In addition, a deep knowledge about advantages and weaknesses of each spectroscopy technique is presented. The advance of data handling and data modelling applications and updating about the latest chemometric tools and strategies to better exploit the acquired spectroscopy data from current instrumentation are also exposed. Finally, novelty prospects in Wines and Wine Vinegars analysis are revealed.
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Assessment of UV–visible spectroscopy as a useful tool for determining grape-must caramel in high-quality Wine and balsamic Vinegars
Food Chemistry, 2020Co-Authors: Rocío Ríos-reina, Silvana Mariela Azcarate, José Manuel Camiña, Raquel M. CallejónAbstract:Abstract The addition of E-150d caramel, known as grape-must caramel in Vinegars, is a legal but without limitation practice in Spanish Wine Vinegars, as those with a protected designation of origin (PDO), for unifying the final colour of different batches and barrels. It is also used in the production of ‘Balsamic vinegar of Modena’ Vinegars, with a maximum addition fixed at 2% v/v by law. Although its quantification in Vinegars was studied by other techniques, there is still not any official method for it. Therefore, UV–vis spectroscopy was assessed as a quick analytical method able to quantify grape-must caramel in Balsamic Vinegars of Modena and Spanish PDO Wine Vinegars. Univariate and multivariate calibrations were assessed for this quantification. Results demonstrated the ability of UV–vis spectroscopy coupled with multivariate calibration in the quantification of grape-must caramel, predicting caramel amounts under 2% v/v in both Balsamic and PDO Wine Vinegars.
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Sensory and spectroscopic characterization of Argentinean Wine and balsamic Vinegars: A comparative study with European Vinegars.
Food chemistry, 2020Co-Authors: Rocío Ríos-reina, Silvana Mariela Azcarate, José Manuel Camiña, Raquel M. CallejónAbstract:Abstract In Argentina, Vinegars are cheap agro-food products without exhaustive regulation and the production of high-quality Vinegars has not been exploited yet. In fact, Argentinean Vinegars have not been studied. In this context, a first study of Argentinean balsamic and Wine Vinegars was carried out by a sensory and spectroscopic characterization and by a comparison with well-recognized European Vinegars. For that, ultraviolet–visible and fluorescence spectroscopies were applied together with principal component analysis (PCA) and parallel factor analysis (PARAFAC) performed on each data set, respectively. Results showed differences between acetification processes, origin countries and a wide variability within Argentinean production. The sensory characterization on Argentinean Wine Vinegars was performed by triangular and ordering preference tests showing statistically significant preferences toward the traditional and the rapid Vinegars. This work highlights the effect of production on quality in order to provide added value to the Argentinean Vinegars.
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Characterization of the aroma profile and key odorants of the Spanish PDO Wine Vinegars
Food chemistry, 2019Co-Authors: Rocío Ríos-reina, M. Lourdes Morales, M. Pilar Segura-borrego, Raquel M. CallejónAbstract:Abstract The aroma profiles of Spanish Wine Vinegars with Protected Designation of Origin (PDO) were described and compared for the first time by gas chromatography–mass spectrometry–olfactometry (GC–MS–O), odor-active values (OAVs) and quantitative descriptive analysis (QDA). Vinagre de Jerez Reserva (JRE) showed higher percentage of ‘grassy-vegetal’ impact odorants, while ‘spicy’ compounds highlighted the Pedro Ximenez category (JPX). Vinagre de Montilla-Moriles Reserva (MRE) had ‘buttery-lactic’ impact odorants, while ‘empyreumatic’ and ‘sweet’ aromas stood out for Pedro Ximenez category (MPX). Vinagre de Condado de Huelva Reserva (CRE) showed a stronger percentage of ‘chemical’ impact odorants. The key odorants were ethyl propionate, ethyl octanoate, propanoic acid and 4-ethylphenol for JRE, diacetyl and methional/furfural for JPX, acetoin for MRE, ethyl phenylacetate and vanillin for MPX and acetaldehyde diethyl acetal, isobutyl acetate, ethyl isovalerate and guaiacol for CRE. A good relation among the impact odorants and the sensory descriptors was observed.
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A comparative study of the volatile profile of Wine Vinegars with protected designation of origin by headspace stir bar sorptive extraction.
Food research international (Ottawa Ont.), 2019Co-Authors: Rocío Ríos-reina, Diego L. García-gonzález, M. Lourdes Morales, M. Pilar Segura-borrego, Raquel M. CallejónAbstract:Abstract The characteristic volatile profile of the Spanish Vinagre de Jerez (VJ), Vinagre de Condado de Huelva (VC) and Vinagre de Montilla-Moriles (VMM) protected designation of origin (PDO) Wine Vinegars has been studied and compared for the first time by headspace stir bar sorptive extraction-gas chromatography–mass spectrometry (HSSE-GC–MS). The possible markers of each category and PDO were assessed. Acetates were the majority group in all Vinegars, while ketones, C13-norisoprenoids and volatile phenols showed significant differences between the three PDOs. Analysis of variance (ANOVA), heatmap and partial least squares-discriminant analysis (PLS-DA) were performed. According to these results, 1-heptanol, methyl nonanoate, 2-methylbutanoic acid, 2,2,6-trimethyl-cyclohexanone, trans-2-decenal, eucalyptol and α-terpineol, were the most significant compounds for differentiating of VC, diacetyl and acetoin, ethyl 3-ethoxypropanoate, 2- and 3-heptanone, 2-methyl-1-hexadecanol, 1-octen-3-ol, p-Cresol and camphene for VMM; and β-damascenone, 5-hydroxymethylfurfural, 3-heptanol, trans-2-hexen-1-ol and trans-2-hexen-1-yl acetate for VJ. Classification results showed that 100% of PDO samples were correctly classified, reaffirming the utility of the volatile profiles for classifying and authenticating Wine vinegar PDOs.
Ana M Troncoso - One of the best experts on this subject based on the ideXlab platform.
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Anthocyanin composition in Cabernet Sauvignon red Wine vinegar obtained by submerged acetification
Food Research International, 2010Co-Authors: Ana B. Cerezo, M. Carmen Garcia-parrilla, Elyana Cuevas, Peter Winterhalter, Ana M TroncosoAbstract:Abstract Vinegars elaborated from white Wine can be characterized by their phenolic composition. Indeed, for authenticity purpose, phenolic composition can be used to identify Sherry and Balsamic Vinegars. However, the phenolic composition of red Wine Vinegars has scarcely been studied. Anthocyanin compounds in particular remain largely unknown. This study focuses on the analysis of anthocyanin compounds in red Wine vinegar and the effect of acetification with submerged culture on such Vinegars. The vinegar used in this study was produced from a young Cabernet Sauvignon Wine in a laboratory-scale fermenter. Subsequent analyses of both Wine and vinegar included their anthocyanin profile (by LC/MS), and their non-anthocyanin phenolic profile (by LC/DAD). In addition, Wine and vinegar anthocyanin extracts were fractionated by CCC to determine the contribution of the fractions to overall antioxidant activity (AA), using ORAC, FRAP and DPPH assays. A total of 20 anthocyanin compounds were identified in the vinegar. As far as we know, this is the first time that anthocyanin-derived pigments (pyranoanthocyanins and ethyl-linked compounds) have been identified in red vinegar in such detail. Moreover, an original contribution of this study is the identification for the first time of catechyl-pyranocyanidin-3-glucoside in vinegar and Wine, as well as two anthocyanin compounds not previously reported in vinegar or Cabernet Sauvignon Wine: acetyl vitisin B and coumaroyl vitisin B. After the acetification process, vitisin-type and ethyl-linked compounds increased and monomeric anthocyanins, phenolic acids (ferulic acid, caffeic acid and caftaric acid) and flavan-3-ol ((+)-catechin) decreased. Although the proportion by weight of the polymeric compound fraction is similar in Wine and vinegar, the AA of these polymers in vinegar is significantly greater (p
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DESCRIPTIVE SENSORY ANALYSIS OF Wine VINEGAR: TASTING PROCEDURE AND RELIABILITY OF NEW ATTRIBUTES
Journal of Sensory Studies, 2010Co-Authors: Wendu Tesfaye, Raquel M. Callejón, Maria Carmen García-parrilla, M L Morales, Antonio G. González, Ana B. Cerezo, Ana M TroncosoAbstract:ABSTRACT A procedure for the sensory analysis of vinegar, which provides reproducible results and minimizes the standard deviation of attributes, was developed. A new tasting protocol was proposed that leads to low dispersions of panelists' answers. The list of attributes that describe Vinegars was extended to a total of 13, the importance (or discriminant utility) of which was analyzed by using Partial Least Squares Regression related techniques. The attributes selected showed a good between-run reproducibility as was shown by the Discriminant Partial Least Squares Regression analysis on replications. The proposed methodology proved to be useful for tasting very different types of Wine Vinegars (i.e., sherry and red and white Wine Vinegars). PRACTICAL APPLICATIONS As the vinegar market is now making products from different raw materials, we believed that it would be interesting to improve sensory analysis. The European Union (EU) regulates the sensory analysis of oil but not of vinegar. Our manuscript describes a tasting protocol that aims to provide more reproducible results, proposes a broader vocabulary for describing Vinegars and uses statistical tools to verify the reliability of new attributes.
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Changes of volatile compounds in Wine Vinegars during their elaboration in barrels made from different woods
Food Chemistry, 2010Co-Authors: Raquel M. Callejón, M L Morales, María Jesús Torija, Albert Mas, Ana M TroncosoAbstract:Abstract Changes in the volatile components of red Wine Vinegars and balsamic Vinegars were investigated during 1 year of aging in wood barrels and bottles. Barrels of four different woods (oak, chestnut, acacia and cherry) were used. A total of 57 volatile compounds were analysed by Gas Chromatography–Flame Ionization Detection (GC–FID) and Headspace Sorptive Extraction GC–Mass Spectrometry (HSSE-TD–GC–MS). We observed significant increases in the total content of volatile compounds only for balsamic Vinegars. The concentrations of ethyl furoate, ethyl benzoate, benzaldehyde and acetophenone were highest in cherry barrels. These compounds, then, seem to be characteristic of this wood. Oak lactones presented the highest increases for Vinegars aged in oak. Eugenol was only present in Vinegars aged in chestnut and oak barrels. Oak and cherry seem to be the best type of wood for aging of vinegar due to their distinctive aromatic characteristics.
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Effect of wood on the phenolic profile and sensory properties of Wine Vinegars during ageing
Journal of Food Composition and Analysis, 2010Co-Authors: Ana B. Cerezo, Wendu Tesfaye, Maria Carmen García-parrilla, M.e. Soria-díaz, M. Jesús Torija, Estibaliz Mateo, Ana M TroncosoAbstract:Abstract A crucial step in the production of high-quality Wine Vinegars is ageing in wood. This study aims to determine how wood barrels affect vinegar quality. For this purpose, Vinegars were aged in barrels made from acacia, cherry, chestnut and oak wood. Two kinds of Vinegars were studied: balsamic and red-Wine Vinegars. Analysis of samples included total phenol index (TPI), total monomeric anthocyanins (TA), dry extract, and phenolic and furanic compounds by liquid chromatography with photodiode array detection (LC–DAD) in a total of 98 samples. The concentration of HMF, 2-furfuraldehyde, protocatechualdehyde and vanillin significantly increased during ageing. Taxifolin is present in Vinegars aged in cherry wood, confirmed by liquid chromatography–mass spectrometry/mass (LC–MS/MS). Hence, it can be a marker of Vinegars aged in cherry wood. This is the first time that this compound has been identified in Wine Vinegars. On the other hand, ellagic acid is a characteristic compound for samples aged in chestnut and oak barrels. An unknown peak was found in all vinegar samples (groups F, T and M) which were aged in acacia wood. Linear discriminant analysis was used to classify samples as a function of the type of wood and ageing time, with phenolic compounds as variables. The linear functions obtained correctly classified – at 100% – red Vinegars according to the type of wood. If ageing time (0–365 days) is considered, 62.5% and 100% of the red and balsamic vinegar samples, respectively, were well classified. The effect of wood on vinegar quality is obvious enough to be perceived by the senses in triangle tests. Woody, sweet and vanilla descriptors presented the highest scores for Vinegars aged in oak wood. On the other hand, ageing in cherry wood increased markers for red-fruit attributes. These results prove that wood used in vinegar ageing determines both the chemical composition and sensorial properties.
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Volatile compounds in red Wine Vinegars obtained by submerged and surface acetification in different woods
Food Chemistry, 2009Co-Authors: Raquel M. Callejón, Wendu Tesfaye, Ana M Troncoso, María Jesús Torija, Albert Mas, M L MoralesAbstract:Abstract Changes in volatile components were investigated during controlled acetifications. The substrates used to perform traditional surface acetifications were two red Wines. Barrels of four different woods (oak, chestnut, acacia and cherry) were used. Submerged acetifications were performed at the laboratory scale. Volatile compounds were analysed by Headspace Sorptive Extraction and Gas Chromatography–Mass Spectrometry (HSSE-TD–GC–MS). Out of 57 compounds identified in the samples, 38 were quantified. Of these, ethyl furoate, ethyl benzoate and limonene had never been described in Wine Vinegars. Acetifications led to an increase in the total quantity of volatile components, which were higher in the surface processes. Acetic esters were predominant in surface culture Vinegars, whereas acids were predominant in submerged culture Vinegars. Oak-lactones were quantified only in Vinegars produced in oak barrels. Ethyl furoate and ethyl benzoate increased in cherry wood barrels. Multivariate statistical analysis supported the influence of the process on the volatile composition of the final Vinegars.
José Manuel Amigo - One of the best experts on this subject based on the ideXlab platform.
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Data fusion approaches in spectroscopic characterization and classification of PDO Wine Vinegars.
Talanta, 2019Co-Authors: Rocío Ríos-reina, Raquel M. Callejón, José Manuel Amigo, Francesco Savorani, Marina CocchiAbstract:Abstract Spain is one of the major producers of high-quality Wine Vinegars having three protected designations of origin (a.k.a. PDOs): “Vinagre de Jerez”, “Vinagre de Condado de Huelva” and “Vinagre de Montilla-Moriles”. Their high prices due to their high quality and their high production costs explain the need for developing an adequate quality control technique and the interest in extensive characterization in order to capture the identity of each denomination. In this framework, methodologies based on non-targeted techniques, such as spectroscopies, are becoming popular in food authentication. Thus, for improving vinegar quality assessment, fusion of data blocks obtained from the same samples but different analytical techniques could be a good strategy, since the quantity and quality of sample knowledge could be enhanced providing new insights into the differentiation of Vinegars. Therefore, the aim of this manuscript is the development of a multi-platform methodology and a model able to classify the Spanish Wine vinegar PDOs. Sixty-five PDO Wine Vinegars were analyzed by four spectroscopic techniques: Fourier-transform mid-infrared spectroscopy (MIR), near infrared spectroscopy (NIR), multidimensional fluorescence spectroscopy (EEM) and proton nuclear magnetic resonance (1H-NMR). Two different data fusion strategies were evaluated: Mid-level data fusion with different preprocessing, and Common Component and Specific Weights analysis multiblock method. Exploratory and classification analysis on the data from individual techniques were also performed and compared with data fusion models. The data fusion models improved the classification, providing a more efficient differentiation, than the models based on single methods, and supporting the approach to combine these methods to achieve synergies for an optimized PDO differentiation.
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Application of hierarchical classification models and reliability estimation by bootstrapping, for authentication and discrimination of Wine Vinegars by UV–vis spectroscopy
Chemometrics and Intelligent Laboratory Systems, 2019Co-Authors: Rocío Ríos-reina, Raquel M. Callejón, Silvana Mariela Azcarate, José Manuel Camiña, José Manuel AmigoAbstract:Abstract In recent years, three Spanish Wine Vinegars have obtained the indication of Protected Denomination of Origin (PDOs) due to their unique characteristics and traditional method of production: “Vinagre de Jerez”, “Vinagre de Condado de Huelva” and “Vinagre de Montilla-Moriles”. These Vinegars are expensive due to their high quality, the long aging time and the high cost of production, reason why the adulteration and unfair competition in the vinegar industry are frequent practices. To avoid these frauds, several analytical techniques have been already studied for the characterization and authentication of these high quality Vinegars. Nevertheless, ultraviolet–visible (UV–vis) spectroscopy, especially attractive for its simplicity and low cost, has not been previously used to assess PDO or other qualities as type of production or aging, in Wine Vinegars. For this reason, the potential of UV–vis spectroscopy was investigated for the first time as a rapid and inexpensive methodology for developing classification models to discriminate Wine Vinegars according to the production method, the PDO and the aging category. Spectra from 70 Wine Vinegars -including different categories within the 3 PDOs and also Vinegars without PDO as known as rapid Vinegars-have been analyzed and compared in the selected region of 280–600 nm. Principal components analysis (PCA) was used as exploratory method, while soft independent modelling-class (SIMCA) and partial least squares-discriminant analysis (PLS-DA) were employed for the development of a hierarchical classification model. Differences between categories and PDOs, as well as between PDO and Non-PDO Wine Vinegars, were observed according to the spectral regions around 300 nm and the visible regions around 500 nm. Furthermore, bootstrap resampling method was employed to generate distributions of classification results and to obtain confidence intervals in the classification. The hierarchical classification results open up the possibility of developing a tool that provides an easy and fast differentiation for the authentication of Wine Vinegars from different categories and denomination of origins.
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NIR spectroscopy and chemometrics for the typification of Spanish Wine Vinegars with a protected designation of origin
Food Control, 2018Co-Authors: Rocío Ríos-reina, Raquel M. Callejón, Diego L. García-gonzález, José Manuel AmigoAbstract:Abstract High-quality Wine Vinegars protected by the indication “Protected Designation of Origin” (PDO) need efficient tools to protect their brands and prevent adulteration and unfair competition. In this sense, Near-Infrared spectroscopy (NIRs) combined with chemometrics has demonstrated its usefulness in food authentication. This work assessed NIRs and Chemometrics as a rapid and non-destructive methodology for this purpose. In this study, 83 high-quality Wine Vinegars of the Spanish PDOs “Vinagre de Jerez”, “Vinagre de Condado de Huelva” and “Vinagre de Montilla-Moriles” of different categories, and 11 Wine Vinegars without PDO, were analyzed in the range 12000-4000 cm−1. Principal component analysis (PCA) was performed to explore the spectra and Partial Least Squares-Discriminant Analysis (PLS-DA) was used to build classification models. The high ability of prediction obtained (>90% correct classification) demonstrated the usefulness of this methodology for authentication of PDO Wine Vinegars and their categories.
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Sampling methods for the study of volatile profile of PDO Wine Vinegars. A comparison using multivariate data analysis.
Food research international (Ottawa Ont.), 2017Co-Authors: Rocío Ríos-reina, Diego L. García-gonzález, José Manuel Amigo, M. Lourdes Morales, Raquel M. CallejónAbstract:High-quality Wine Vinegars have been registered in Spain under protected designation of origin (PDO): "Vinagre de Jerez", "Vinagre de Condado de Huelva" and "Vinagre de Montilla-Moriles". The raw material, production and aging processes determine their quality and their aromatic composition. Vinegar volatile profile is usually analyzed by gas chromatography-mass spectrometry (GC-MS), being necessary a previous extraction step. Thus, three different sampling methods (Headspace solid phase microextraction "HS-SPME", Headspace stir bar sorptive extraction "HSSE" and Dynamic headspace extraction "DHS") were studied for the analysis of the volatile composition of Spanish PDO Wine Vinegars. Multivariate curve resolution (MCR) was used to solve chromatographic problems, improving the results obtained. Principal component analysis (PCA) showed that not all the sampling methods were equally suitable for the characterization and differentiation between PDOs and categories, being HSSE the technique that made able the best vinegar characterization.
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Characterization and authentication of Spanish PDO Wine Vinegars using multidimensional fluorescence and chemometrics
Food chemistry, 2017Co-Authors: Rocío Ríos-reina, Diego L. García-gonzález, José Manuel Amigo, Saioa Elcoroaristizabal, Juan Antonio Ocaña-gonzález, Raquel M. CallejónAbstract:Abstract This work assesses the potential of multidimensional fluorescence spectroscopy combined with chemometrics for characterization and authentication of Spanish Protected Designation of Origin (PDO) Wine Vinegars. Seventy-nine Vinegars of different categories (aged and sweet) belonging to the Spanish PDOs “ Vinagre de Jerez ” , “ Vinagre de Montilla-Moriles ” and “ Vinagre de Condado de Huelva ”, were analyzed by excitation-emission fluorescence spectroscopy. A visual assessment of fluorescence landscapes pointed out different trends with vinegar categories. PARAllel FACtor analysis (PARAFAC) extracted the potential fluorophores and their values in the PDO Vinegars. This information, coupled with different classification methods (Partial Least Square Discrimination Analysis “PLS-DA” and Support Vectors Machines “SVM”), was able to discriminate the Wine vinegar category within each PDO, for which SVM models obtained better results (>92% of classification). In each category, SVM also allows the differentiation between PDOs. The proposed methodology could be used as an analysis method for the authentication of Spanish PDO Wine Vinegars.
M L Morales - One of the best experts on this subject based on the ideXlab platform.
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Elemental characterisation of Andalusian Wine Vinegars with protected designation of origin by ICP-OES and chemometric approach
Food Control, 2017Co-Authors: Patricia Paneque, M L Morales, Pilar Burgos, L. Ponce, Raquel M. CallejónAbstract:Abstract Wine Vinegars from three Protected Designations of Origin (PDO), Vinagre de Jerez (J), Vinagre de Montilla-Moriles (MM) and Vinagre del Condado de Huelva (CH) from Andalusia, Southern Spain, were investigated for their mineral elements content. Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, Pb, S, Sr, V and Zn were determined by inductively coupled plasma optical-emission (ICP-OES). Jerez Vinegars had a statistically significant higher Sr content than the others, while with respect to B the same was true for Montilla-Moriles Vinegars. Moreover, the ageing time of the Vinegars clearly played a role in vinegar mineral content, with higher mineral levels found in aged Vinegars than in young ones, especially in samples from Condado de Huelva. Multivariate analysis was performed in order to assess if the Vinegars' geographical classification was possible through their elemental profile. Classification models were obtained by LDA and SVM, achieving good prediction abilities, 73 and 80%, respectively.
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A survey of biogenic amines in Vinegars.
Food Chemistry, 2013Co-Authors: J.l. Ordóñez, Raquel M. Callejón, M L Morales, Maria Carmen García-parrillaAbstract:Abstract This paper reports the determination of biogenic amines by high-performance liquid chromatography (HPLC) and fluorescence detection after derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) in balsamic, apple, and red, white, and Sherry Wine Vinegars. A solid-phase extraction (SPE) with mixed-mode resins method was used before analysis. The method was successfully validated obtaining adequate values of selectivity, response linearity, precision, accuracy, and low detection and quantification limits. The total content of biogenic amines in Vinegars ranged from 23.35 to 1445.2 μg/L, being lower than those reported in Wines. Putrescine was the amine that showed the highest concentrations in most samples. Methylamine and phenylethylamine were not determined in any vinegar. Balsamic and “Pedro Ximenez” Sherry Vinegars reached the highest amounts of biogenic amines, while apple, white and Sherry Wine Vinegars had the lowest concentrations. Principal component analysis using the biogenic amines as variables, allowed to separate the different kind of Vinegars, excepting red Vinegars.
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Changes of volatile compounds in Wine Vinegars during their elaboration in barrels made from different woods
Food Chemistry, 2010Co-Authors: Raquel M. Callejón, M L Morales, María Jesús Torija, Albert Mas, Ana M TroncosoAbstract:Abstract Changes in the volatile components of red Wine Vinegars and balsamic Vinegars were investigated during 1 year of aging in wood barrels and bottles. Barrels of four different woods (oak, chestnut, acacia and cherry) were used. A total of 57 volatile compounds were analysed by Gas Chromatography–Flame Ionization Detection (GC–FID) and Headspace Sorptive Extraction GC–Mass Spectrometry (HSSE-TD–GC–MS). We observed significant increases in the total content of volatile compounds only for balsamic Vinegars. The concentrations of ethyl furoate, ethyl benzoate, benzaldehyde and acetophenone were highest in cherry barrels. These compounds, then, seem to be characteristic of this wood. Oak lactones presented the highest increases for Vinegars aged in oak. Eugenol was only present in Vinegars aged in chestnut and oak barrels. Oak and cherry seem to be the best type of wood for aging of vinegar due to their distinctive aromatic characteristics.
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DESCRIPTIVE SENSORY ANALYSIS OF Wine VINEGAR: TASTING PROCEDURE AND RELIABILITY OF NEW ATTRIBUTES
Journal of Sensory Studies, 2010Co-Authors: Wendu Tesfaye, Raquel M. Callejón, Maria Carmen García-parrilla, M L Morales, Antonio G. González, Ana B. Cerezo, Ana M TroncosoAbstract:ABSTRACT A procedure for the sensory analysis of vinegar, which provides reproducible results and minimizes the standard deviation of attributes, was developed. A new tasting protocol was proposed that leads to low dispersions of panelists' answers. The list of attributes that describe Vinegars was extended to a total of 13, the importance (or discriminant utility) of which was analyzed by using Partial Least Squares Regression related techniques. The attributes selected showed a good between-run reproducibility as was shown by the Discriminant Partial Least Squares Regression analysis on replications. The proposed methodology proved to be useful for tasting very different types of Wine Vinegars (i.e., sherry and red and white Wine Vinegars). PRACTICAL APPLICATIONS As the vinegar market is now making products from different raw materials, we believed that it would be interesting to improve sensory analysis. The European Union (EU) regulates the sensory analysis of oil but not of vinegar. Our manuscript describes a tasting protocol that aims to provide more reproducible results, proposes a broader vocabulary for describing Vinegars and uses statistical tools to verify the reliability of new attributes.
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Volatile compounds in red Wine Vinegars obtained by submerged and surface acetification in different woods
Food Chemistry, 2009Co-Authors: Raquel M. Callejón, Wendu Tesfaye, Ana M Troncoso, María Jesús Torija, Albert Mas, M L MoralesAbstract:Abstract Changes in volatile components were investigated during controlled acetifications. The substrates used to perform traditional surface acetifications were two red Wines. Barrels of four different woods (oak, chestnut, acacia and cherry) were used. Submerged acetifications were performed at the laboratory scale. Volatile compounds were analysed by Headspace Sorptive Extraction and Gas Chromatography–Mass Spectrometry (HSSE-TD–GC–MS). Out of 57 compounds identified in the samples, 38 were quantified. Of these, ethyl furoate, ethyl benzoate and limonene had never been described in Wine Vinegars. Acetifications led to an increase in the total quantity of volatile components, which were higher in the surface processes. Acetic esters were predominant in surface culture Vinegars, whereas acids were predominant in submerged culture Vinegars. Oak-lactones were quantified only in Vinegars produced in oak barrels. Ethyl furoate and ethyl benzoate increased in cherry wood barrels. Multivariate statistical analysis supported the influence of the process on the volatile composition of the final Vinegars.
