Impact of Fig Maceration under Various Conditions on Physicochemical and Sensory Attributes of Wine Vinegar: A comprehensive Characterization Study

Received: 23 December 2023 Revised: 8 July 2024 Accepted: 3 September 2024 DOI: 10.1111/1750-3841.17485 ORIGINAL ARTICLE Food Chemistry Impact of fig maceration under various conditions on physicochemical and sensory attributes of wine vinegar: A comprehensive characterization study Maria del Pilar Segura-Borrego1Pilar Ramírez2Rocío Ríos-Reina1 Maria Lourdes Morales1Raquel María Callejón1Juan Manuel León Gutiérrez2 1Área de Nutrición y Bromatología, Dpto. de Nutrición y Bromatología, Toxicología y Medicina Legal, Facultad de Farmacia, Universidad de Sevilla, Sevilla, España 2Departamento de Tecnología, Poscosecha e Industria Alimentaria, Centro IFAPA “Cabra”, Instituto de Investigación y Formación Agraria y Pesquera, Ctra, Córdoba, España Correspondence Callejón, R.M., Área de Nutrición y Bromatología, Dpto. de Nutrición y Bromatología, Toxicología y Medicina Legal, Facultad de Farmacia, Universidad de Sevilla, C/P. García González n◦2, Sevilla, España. Email: [email protected] Abstract: In this work, wine vinegars macerated with figs under different conditions have been characterized for the first time. Samples were analyzed by solid phase microextraction and gas chromatography coupled to mass spectrometry, sensory and physicochemical analysis. The results revealed that fig maceration of wine vinegars influenced the physicochemical, sensory, and volatile profiles of the final product, which were mainly affected by the fig amount (10, 20 or 30%), the fig type (fresh or dry) and the base wine vinegar (young or aged) used, and to a lesser extent the way the fig was added (crushed or chopped). The maceration, regardless the conditions used, increased the fruity notes, overall taste and visual impression, the tonality, total polyphenols and sugar content, and the presence of some volatile compounds, mainly terpenes and ketones, such as (Z)- p-mentha-2,8-dien-1-ol, or β-damascenone. Therefore, maceration increased the organoleptic complexity, which could enhance the acceptability of consumers towards these products. KEYWORDS GC/MS, macerated, SPME, volatile profile, wine vinegar Practical Application: This research studied how wine vinegars macerated with figs affect in different ways their taste, smell, and chemical properties. Thus, the results showed that these wine vinegars made with fig maceration by using different amounts and types of figs, as well as the type of vinegar used, changed their characteristics, making them smell and taste fruitier and more pleasant. This could be useful for making better-tasting and more appealing vinegars for consumers who enjoy unique and enhanced flavors in their food. This is an open access article under the terms of the Creative Commons Attribution-NonCommercial-NoDerivs License, which permits use and distribution in any medium, provided the original work is properly cited, the use is non-commercial and no modifications or adaptations are made. © 2024 The Author(s). Journal of Food Science published by Wiley Periodicals LLC on behalf of Institute of Food Technologists. J. Food Sci. 2024;89:8945–8968. wileyonlinelibrary.com/journal/jfds 8945 8946 A COMPREHENSIVE CHARACTERIZATION STUDY 1 INTRODUCTION Wine vinegar is a condiment derived from grapes and obtained exclusively through biotechnological processes by double fermentation: first, an alcoholic fermentation, in which natural sugars are converted to ethanol and, second, an acetic fermentation in which ethanol is transformed into acetic acid by the action of acetic acid bacteria (Callejón et al., 2008a;2008b; Ríos-Reina et al., 2019;Tesfaye et al., 2010). Wine vinegar is a traditional food product produced and consumed in many cultures since ancient times, but for many years it was regarded as a low-value secondary product. However, the consumer’s interest all over the world for wine vinegars is in continuous growth, as well as its consideration as a valued food product in gastronomy and a very versatile condiment (Ríos-Reina et al., 2019;2020). Undoubtedly, wine vinegar is the most common type and most highly-prized vinegar type, especially in the Mediterranean countries (Mas et al., 2014), of which Spain plays an important role as a producer (Ríos-Reina et al., 2019). The latest gastronomic trends and the high level of competitiveness of today’s market have led, in recent years, to a considerable expansion of the vinegar varieties available. The high demand for different and high-quality products has provided an opportunity for the development of new value-added options. Nowadays, all gastronomy products tend to diversify for various purposes. Aspects such as sustainability and consumer´s health are taking on an important role among the 21st century population, as they are being used as competitive market strategies. In this regard, it is worth noting that, in recent years, the growing knowledge about the nutritional impact on human health has led to an increased interest in fruits and vegetables due to their beneficial nutrient content. This could explain the constant emergence of new gourmet and healthier products. On the other hand, the use of fruits in vinegar production could be a good solution to take advantage of fruit surpluses, providing an additional income to the agricultural sector (Ubeda et al., 2016a). Considering the above mentioned facts, the use of waste by-products from agrifood production might be a good solution to save resources and provide sustainable foods, activating a circular economy. In recent years, different authors have focused on the study of fruit vinegars such as persimmon (Ubeda et al., 2011), strawberry (Ubeda et al., 2012), orange, mango, cherry (Cejudo-Bastante et al., 2016; Coelho et al., 2017)or blueberry (Da Silva Fonseca et al., 2018), as well as on commercial fruit aromatized vinegars (Cejudo-Bastante et al., 2013b), but wine vinegars macerated with fruit have been little studied. Fig is commonly considered a fruit, but technically it is an inverted flower into itself (Grison-Pigé et al., 2002; Slavin, 2001). It is one of the most important fruit species in the Mediterranean diet, as well as one of the first cultivated ones (Caliskan, 2015; Slavin, 2001). Figs produce large crops and show low interannual variation in its production. It is characterized by significant amounts of minerals, such as calcium and iron and a wide range of phytochemicals (Caliskan, 2015; Slavin, 2001). Moreover, as fresh figs are a perishable product, the use of dried figs, that can be stored for 6–8 months, characterized by a higher amount of fiber and sugars, could be also a good alternative (Slatnar et al., 2011). These characteristics, together with the possibility of using fruit surpluses, could become a good option for the agricultural sector. The use of figs, commonly consumed fresh or dried, as a raw material for gourmet wine vinegars production might be a good business strategy, given that these vinegars provide different organoleptic characteristics such as taste, odor, color, and even nutritional composition than the original ones. Aroma is one of the main quality indicators of vinegars (Callejón et al., 2008b), and, hence, one of the most important determinants of new food products acceptance (Ríos-Reina et al., 2020; Ubeda et al., 2012). Sometimes, a single volatile compound is sufficient to give a product its characteristic aroma, but, usually, it is influenced by different ones (Mestres et al., 2000). As it is well known, the characteristic volatile profile of wine vinegar is determined by different factors, as the wine substrate, the production process, and aging (Callejón et al., 2008b; Ríos-Reina et al., 2019). In general, the characteristic volatile compounds of vinegar are acetic acid, acetoin and ethyl acetate which are found in greater quantities than others. However, vinegars contain a wide variety of chemical compounds that belong to different families such as carboxylic acids, alcohols, ethyl and acetic acid esters, and, depending on the type of vinegar, different proportions of aldehydes, acetals, ketones, lactones, terpenes, volatile phenols or pyrazines (Ubeda et al., 2020). In the case of wine vinegar macerated with figs, some volatile compounds may come from the fruit. A widely used technique in the study of volatile composition of vinegars is gas chromatography coupled to a mass spectrometry detector (GC/MS) (Callejón et al., 2008a; Mas et al., 2014; Ríos-Reina et al., 2019,2020; Truta et al., 2010). Always, a prior extraction step is necessary for this kind of analyses. Different extraction techniques have been used for the determination of volatile composition of wine vinegar such as classical liquid–liquid extraction (LLE) (Castro et al., 2004; Ortega et al., 2001) and solid 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License A COMPREHENSIVE CHARACTERIZATION STUDY 8947 phase extraction (SPE) (López et al., 2002), as well as dynamic headspace (DHS) (Ríos-Reina et al., 2018; Ubeda et al., 2016a), headspace sorptive extraction (HSSE) (Callejón et al., 2008a; Weldegergis et al., 2007), and solid phase microextraction (SPME) (Mestres et al., 2000; Roda et al., 2017). The last one, although have several disadvantages such as lower sensitivity than other extraction techniques, it seems to provide a complete knowledge of the vinegar’s volatile profile and it also presents the advantage of being cost-effective and rapid. In this context, the aim of this work was to study and characterize, for the first time, the different wine vinegar products obtained after maceration with figs at different conditions (i.e. dried figs, fresh figs, different amounts, and different wine vinegars as base material). To achieve such goal, physicochemical, sensory and SPME-GC/MS analyses were carried out. 2 MATERIALS AND METHODS 2.1 Materials for sample preparation Wine vinegars were produced by submerged culture in FRINGS acetifier by UNICO Vinagres y Salsas S. L. L., Doña Mencía (Córdoba). Two types were used: young wine vinegar without aging and wine vinegar aged for an average time of 10 years in American oak barrels. The base wine used to make both vinegars (young and aged) was a young wine from the Montilla-Moriles Protected Designation of Origin (PDO), which was obtained from Pedro Ximénez grape variety. The figs used in maceration belonged to the species Ficus carica L. Fresh ones were dark-skinned figs of the Albacor variety from the Valencian Community, purchased in the local market, while dried ones came from figs grown naturally in the Alpujarra region of Granada and processed by Industria Higuera Alpujarreña S. L., located in Motril (Granada). 2.2 Samples considered for the study Different samples were obtained for this study according to the type of fig (fresh or dry), the base wine vinegar used (young or aged in wood barrels), the fig addition type (crushed and chopped) and the percentage of fig macerated (10%, 20% and 30%). However, according to the preliminary sensory results, not all the samples were characterized in deep. Hence, the preliminary test started with vinegars macerated with fresh figs. For that, all possible different conditions were tested: two different base vinegars (one young and one aged) and addition types (crushed by mixer and chopped by knife), as well as three different percentages of addition (10%, 20% and 30%). According to the sensory results, vinegars made by maceration of fresh fig in aged wine vinegar were discarded due to the characteristics of the aged vinegar fully masked the addition of fig, and no sensory differences were detected in the final product. Then, preliminary sensory tests were carried out on macerated vinegars with dried figs. In this case, young and aged wine vinegars showed differences in the preliminary sensory tests, and, for this reason, both types were considered. However, dried figs were only crushed by a mixer, due to the manual difficulty. Moreover, although a 30% of addition was considered in the macerated vinegars with fresh figs, that were produced in first place, this amount was discarded in macerated vinegars with dried figs due to the highest sensory difference observed between 10% and 20% and the fact that none of the panelists were able to differentiate in any case from 20% to 30%. Macerations of the vinegars were carried out in polyethylene (PE) tanks of 7 L of capacity, in duplicate, at room temperature (between 20◦Cand25 ◦C), placed at in the “Instituto de Investigación y Formación Agraria y Pesquera” (IFAPA) in Cabra (Cordoba, Spain). Before the maceration process, both the young and the aged wine vinegars were diluted with mineral water in order to adjust the total acidity to 7 g/100 mL of acetic acid. Hence, for dried fig vinegars the maceration time was 7 days, and, for fresh figs, 20 days. After the process, macerated wine vinegars were separated from fruits by filtrations and centrifugations. The resulting vinegars were stored at room temperature after bottling. All maceration assays were performed in duplicated. After this preliminary study, a total of 22 wine vinegars were finally analyzed: one young wine vinegar and one aged wine vinegar without maceration; eight wine vinegars macerated with dried figs at different doses of fruit, using the two different base wine vinegars, and 12 young wine vinegars macerated with fresh figs (chopped or crushed) at different fruit doses. More information about samples and codes are shown in Table 1. 2.3 Chemicals and materials Alkane standard mixture C10–C40, used for calculating the linear retention index (LRI) for GC/MS analysis was purchased from Fluka (Madrid, Spain), while Milli-Q water was obtained from a Milli-Q purification system (Millipore, Burlington, MA, USA). In addition, 4-methyl-2-pentanol (99%), employed as internal standard (IS), and ethanol (≥99.9%) were bought from Merck (Darmstadt, Germany), while 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License 8948 A COMPREHENSIVE CHARACTERIZATION STUDY TABLE 1 Samples used in the present study. Fruit type Base vinegar Fig addition type Fig (%) Code Fresh fig (FF) Young (YV) Chopped (CH) 10% FF10CH1 FF10CH2 20% FF20CH1 FF20CH2 30% FF30CH1 FF30CH2 Crushed (CR) 10% FF10CR1 FF10CR2 20% FF20CR1 FF20CR2 30% FF30CR1 FF30CR2 Dried fig (DF) Young (YV) Crushed (CR) 10% DF10Y1 DF10Y2 20% DF20Y1 DF20Y2 Aged (AV) 10% DF10A1 DF10A2 20% DF20A1 DF20A2 Note: All maceration assays were performed in duplicated. analytical-quality sodium chloride was obtained from Sigma-Aldrich (Madrid, Spain). The SPME fibre (1 cm length and 50/30 µmfilm thickness) was purchased from Supelco (Bellefonte, PA, USA), and it was endowed with the Stable Flex stationary phase of divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS). It was previously conditioned following the instructions of the supplier. 2.4 Analytical determinations 2.4.1 Physicochemical parameters Residual alcohol content, dry extract, ash, pH, total acidity, total sugars content, methanol and acetoin content were determined according to OIV (2020), while total polyphenols were determined according to the method previously reported in the literature (Waterhouse, 2001). The total polyphenol index (TPI), color parameters (optical density, color intensity, tonality, L*, a*, b*, hue angle (hab)and chroma (C*)) were studied by spectrophotometry using as reference the Compendium of International Methods of Analysis of Wines and Musts (C.I.E., 2004; OIV, 2019). All parameters were determined in triplicate for each sample. 2.4.2 Sensory analysis Assessors Eight expert panelists from the Sensory Laboratory (IFAPA) have taken part in this study. The experts were members of the Fundación para el “Control de la Calidad Agroalimentaria de Andalucía” (FCCAA), an entity accredited by the “Entidad Nacional de Acreditación” (ENAC) with number 151/C-PR318. This study was reviewed and approved by the “Fundación Control de la Calidad Agroalimentaria de Andalucía” (Project APPROVAL IRB #TRA.TRA.2019.007) and among other fulfilled requirements from the aforementioned institution, the participants were requested to provide informed consent prior to their participation in the study. The expert panelists from the Sensory Laboratory (IFAPA) underwent comprehensive sensory analysis training for over 65 h, including moreover a specific training in vinegar for more than 50 h. The training consisted of exercises of varying intensity levels and stimulus detection. Real reference samples from the PDO Montilla-Moriles and Condado de Huelva were utilized for this purpose. During tastings, the panel evaluated sets of four samples with 30 min of rest between each set, with a maximum 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License A COMPREHENSIVE CHARACTERIZATION STUDY 8949 of three sets per session. Each sample was sensorially evaluated twice, and the volume of each tasted sample was 40 mL. Descriptive profile The panellists evaluated olfactory sensations such as fruity, caramel, nutty, wood, vanilla, ethyl acetate, acetic and wine character odors by orthonasal pathway, and other attributes such as taste balance, general and visual impressions of macerated wine vinegar. They also were asked to rate the intensity of the different descriptors on a continuous scale from 1 to 10. The sensory profile of each macerated wine vinegar sample was expressed as the intensity average value of each descriptor. 2.4.3 Determination of the volatile profile Headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry analysis (GC/MS) Volatile compounds were analyzed by an Agilent 8890 GC system coupled up to an Agilent 5977B simple quadrupole mass spectrometer (Agilent Technologies, Santa Clara, CA, USA) equipped with a multipurpose sampler MPS Robotic Pro LS (Gerstel, Müllheim an der Ruhr, Germany). All extraction procedures were performed by SPME in sample headspace. In all cases, 5 mL of macerated wine vinegar were placed into a 20 mL vial, together with 1.65 g of NaCl and 10 µL of 4-methyl-2-pentanol as internal standard (IS) at 1045 mg/L. The vials with the samples were kept at 20◦C in a thermostatized autosampler tray until analysis. Then, the sample was incubated at 62◦C during 20 min with stirring at 250 rpm and the extraction of the volatile compounds was performed from headspace with SPME fiber during 40 min at 62◦C. Afterwards, for the desorption of compounds, the fiber was desorbed during 4 min at 250◦C, in splitless mode. For this procedure, a 50 m × 250 µm CP-Wax 57 CB column with a 0.20 µm film thickness (Agilent Technologies, Santa Clara, CA, USA) was used. The carrier gas was He at a 1 mL/min flow rate. The initial oven temperature was 35◦Cfor5minanditwasrisen up to 220◦C at a rate of 2.5◦C/min, then held for 7 min. The MS quadrupole, source and transfer line temperatures were maintained at 150◦C, 230◦Cand250 ◦C, respectively. The electron ionization mass spectra in the full-scan mode were recorded at 70 eV with an electron energy range from 29 to 350 m/z. In all cases, all samples were analyzed in duplicate. 2.4.4 Data processing and identification of volatile compounds HS-SPME-GC/MS data was extracted by Agilent MSD Chemstation software and total ion current (TIC) peak areas were obtained with Deconvolution and Identification System 3.0 (PARADISe) software. It enables to process chromatographic data automatically and directly from the raw data based on the deconvoluted mass spectra (Johnsen et al., 2017). Furthermore, it allows to handle overlapping signals, lower signal-to-noise peaks, the simultaneous deconvolution of the pure mass spectra of peaks, and the integration of areas of deconvoluted peaks for all samples. Obtained data were normalized dividing the values of peak area of each compound by the value of peak area of the IS. The Identification of compounds was performed by using the NIST/EPA/NIH Mass Spectral Library (version 2.3, 2017) (Gaithersburg, MD, USA) and confirmed with the LRI value of standards when it was available. LRI values were calculated using the retention times of a series of n-alkanes analyzed under identical conditions to the samples. A tentative identification (TI) was considered when the LRI value agreed only with the literature LRI value without confirmation by standard. 2.4.5 Statistical analysis Significant differences among the data (physicochemical parameters, volatile compounds and all panelists’ sensory attributes scores) were evaluated by the analysis of variance (ANOVA), using Tukey´s test as a post hoc comparison test by INFOSTAT software (FCA, Universidad Nacional de Córdoba, Argentina). Furthermore, as an unsupervised exploratory method, a principal component analysis (PCA) was performed in order to ascertain the degree of differentiation among samples according to the type of fig used (dry or fresh), its addition type (crushed or chopped), the amount of fruit, and the kind of the base wine vinegar used. PCA was undertaken using PLS_Toolbox 7.9.5 (Eigenvector Research Inc., Wenatchee, WA, USA) software working under a MATLAB environment (R2016a, The MathWorks, Inc., Natick, MA, USA). Data was autoscaled to normalize it before the development of the PCA models. Finally, the correlation coefficients between volatile compounds and sensory attributes, and their statistical significance determined using the t-test were calculated using Microsoft Excel’s Data Analysis Package to clearly identify the associations between 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License 8950 A COMPREHENSIVE CHARACTERIZATION STUDY volatile compounds and sensory attributes. Statistical analysis was performed in the replicates performed in each determination (triplicate for physicochemical parameters and in duplicate for sensory and volatile determinations). 3RESULTS AND DISCUSSION 3.1 Influence of macerated fruit on physicochemical parameters of wine vinegar The physicochemical parameters determined as quality parameters to study the fig maceration process in wine vinegar were alcohol content, dry extract, ash, pH, total acidity, total sugars, total polyphenol index (TPI), optical density, color intensity, hue, total polyphenols, methanol, acetoin, and CIELAB parameters of color (L*, a*, b*, hab and C*) (Table 2). To study of the differences in the physicochemical parameters between the different samples, data were submitted to an analysis of variance (ANOVA) followed by a Tukey’s test considering four factors (the amount of fig added, the fig type, the addition type, and the base wine vinegar used). As can be seen in Table 2, in general terms, all fig-macerated vinegars showed significant differences in most of the physicochemical parameters studied in the different comparisons. First, the values were assessed according to the standards of wine vinegars (RD 661/2012). Regarding acidity, vinegars are those products which have a minimum of 5 g/100 mL acidity, except for wine vinegar, which is exclusively obtained from wine and whose acidity is, at least, 6g/100mL.AscanbeseeninTable2, all the acidity values of the macerated samples were over 5 g/100 mL, ranging from 5.2 g/100 mL (FF30CH) to 6.5 g/100 mL (DF10A), and, in the case of the base wine vinegars, of 6.7–6.9 g/100 mL. Therefore, this type of macerated wine vinegar would be considered a food condiment according to the regulations. Regarding the residual alcohol content of vinegar, it is stated that it should be at most 0.5% (v/v), except for wine vinegars that could have a maximum of 1.5% (v/v). In this study, the values for all the samples were found to meet the criteria given in the vinegar standard. Regarding ash content, important for vinegar characterization and quality evaluation (Masino et al., 2008), the values for macerated samples ranged from 1.64 g/L in the case of FF10CH to 4.27 g/L DF20A (Table 2). These values agreed with the ranges of ash content previously reported in fig vinegars (Sengun, 2013) and they were, in many cases, higher than the values obtained by other researchers in wine vinegars (Gerbi et al., 1998). In second place, the influence of the different conditions considered in this study on physicochemical parameters was evaluated. Regarding the factor “amount of fig added (%)”, almost all parameters showed significant differences between the various percentages studied, showing the same increasing trend with the increase of the amount of figusedformaceration(Table2). Hence, some important parameters such as the total content of sugars (g/L), polyphenols and ash increased with the maceration of vinegars with fig. This was expected, as fresh and, mostly, dried figs had already a high content of these compounds, as reported by other authors (Slatnar et al., 2011), so it might be though that they add to the vinegar during the maceration. In all the cases, the ash content increases with the increase of the percentage of fig macerated, explained by the fact that fig fruit is a rich source of mineral content (Sengun, 2013). This percentage was also, in general, statistically higher when dried figs were used instead of fresh figs, as could be expected. Only the parameters total acidity and L* showed significantly lower values in all those samples where the fig content was higher (Table 2). For the first parameter, acidity, this decrease could be explained by the fact that the addition of fig for maceration could produce a dilution effect. It could be highlighted that a decrease of acidity was observed in all cases, and this was a sharper decline in the products obtained by the maceration of fresh figs with high percentage of fruit. Moreover, the luminosity parameter (L*) decreased with the fig maceration due to the natural dark color of figs, thereby obscuring the original vinegar. Moreover, in relation to residual alcohol, slight decreases were observed in most of samples in the maceration processes. On the other hand, the tonality (Abs 420/520 nm) was the only parameter that showed a different trend: its values increased with the maceration of dried figs, but decreased with the addition of fresh figs. This was expectable due to the different color that dried and fresh figs presented, as the first ones show a higher tonality. Regarding the type of fig used, fresh or dried, almost all the physicochemical parameters showed higher values for the vinegars macerated with the latter than for those macerated with the former (Table 2). This fact may be due to the dry process of figs, which produces a concentration of fig components; therefore, they can provide more substances to the wine vinegar during the maceration process. Furthermore, regarding the influence of the fig addition type (crushed or chopped), pairwise comparisons were made for each quantity of fig added (10CH-10CR; 20CH-20CR; 30CH-30CR). In this case, the difference was more relevant in the color aspects of the samples (p<0.05), and greatest differences, statistically significant, were found in the comparison of the addition types for the 10% amount of fig added. Thus, for samples with chopped fruit, the highest values were obtained in parameters such 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License A COMPREHENSIVE CHARACTERIZATION STUDY 8951 TABLE 2 Physicochemical parameters of base wine vinegar samples and wine vinegar macerated with figs under different conditions. Base wine vinegar Fresh fig (FF) Dried fig (DF) YV AV FF10CH FF20CH FF30CH FF10CR FF20CR FF30CR DF10Y DF20Y DF10A DF20A Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Residual alcoholic content 0.30 –0.30 –0.30 –0.20 –0.20 –0.30 –0.20 –0.30 –0.20 –0.20 –<0.2 –<0.2 – Dry extract 11.24 0.07 11.37 0.01 28.38 0.42 47.54 1.22 66.56 2.85 28.66 0.18 48.61 0.97 68.09 1.90 73.28 0.88 140.84 0.66 73.88 0.19 139.01 0.35 Ashes 1.52 0.02 2.11 0.01 1.64 0.03 2.03 0.01 2.44 0.07 1.68 0.02 2.08 0.01 2.65 0.04 2.61 0.08 3.98 0.12 2.96 0.04 4.27 0.13 pH 2.59 0.01 2.64 0.01 2.84 0.01 2.99 0.00 3.13 0.01 2.85 0.00 3.00 0.01 3.12 0.01 3.05 0.03 3.21 0.01 3.05 0.00 3.22 0.00 Total acidity 6.71 0.00 6.86 0.02 6.44 0.02 5.82 0.04 5.25 0.00 6.40 0.02 5.79 0.04 5.51 0.43 6.44 0.20 6.33 0.06 6.53 0.08 6.27 0.05 Total sugars 1.91 0.01 1.96 0.00 <25 – 45.00 1.41 61.50 3.54 <25 – 45.50 0.71 64.50 2.12 60.50 0.71 122.50 2.12 59.50 0.71 117.50 0.71 TPI 5.87 0.01 10.77 0.01 6.88 0.03 8.14 0.23 9.74 0.38 6.79 0.17 8.30 0.14 10.27 0.14 16.49 0.25 28.02 0.19 18.99 0.18 30.98 0.23 Total polyphenols 65.38 0.01 94.21 0.00 73.98 0.15 94.18 6.01 117.89 4.86 76.27 0.91 91.93 3.79 116.56 0.72 87.01 1.45 128.03 1.54 97.03 0.99 135.37 1.19 Methanol <20 –31.02 0.03 121.80 2.63 188.30 5.23 304.44 1.34 127.24 1.87 209.81 26.32 350.00 0.78 121.22 0.18 222.66 7.74 131.56 1.90 224.58 7.89 Acetoin 376.00 0.00 349.00 0.00 233.50 21.92 255.50 19.09 293.50 9.19 233.00 7.07 272.00 16.97 306.00 1.41 248.50 16.26 228.00 7.07 257.50 41.72 272.5036.06 Optical density 0.22 0.00 0.47 0.01 0.30 0.00 0.47 0.07 0.66 0.04 0.27 0.00 0.50 0.02 0.79 0.03 0.90 0.05 1.77 0.01 1.03 0.00 1.95 0.02 Color intensity 0.31 0.00 0.67 0.00 0.69 0.01 1.22 0.18 1.79 0.11 0.60 0.00 1.30 0.02 2.10 0.04 1.18 0.06 2.35 0.01 1.38 0.02 2.64 0.02 Tonality 3.53 0.04 3.04 0.00 0.79 0.01 0.69 0.03 0.63 0.00 0.77 0.01 0.69 0.03 0.69 0.02 3.99 0.01 3.89 0.10 3.80 0.09 3.70 0.03 L* 95.70 0.00 89.87 0.01 84.61 0.01 73.91 3.54 66.23 1.58 87.72 0.01 72.82 0.37 61.33 0.05 86.31 0.60 75.19 0.71 83.60 0.56 71.64 0.08 a* −0.56 0.01 1.17 0.00 24.05 0.26 36.92 0.22 49.24 1.33 27.24 0.43 38.44 0.61 46.62 0.61 3.41 0.62 13.16 0.20 4.78 0.13 15.35 0.08 b* 14.63 0.02 38.70 0.01 12.83 0.35 17.76 0.98 25.42 1.34 10.44 0.12 19.28 0.63 27.10 1.74 47.11 1.83 69.44 0.99 50.16 0.44 70.79 0.57 Hue angle (hab) 92.20 0.01 84.35 0.01 28.09 0.91 25.69 1.37 27.41 0.56 20.96 0.08 26.64 1.11 30.15 1.27 85.87 0.59 79.27 0.01 84.56 0.10 77.76 0.16 Chroma (C*) 14.63 0.00 38.87 0.01 27.26 0.07 40.97 0.23 55.37 1.62 29.17 0.44 43.01 0.26 53.93 1.40 47.24 1.87 70.68 1.01 50.39 0.45 72.44 0.54 Note: Units of physicochemical parameters: Residual alcoholic strength (%v/v); Dry extract (g/L); Ash (g/L); pH; Total acidity (g acetic acid/100 mL); Total sugars (g/L);TPI (Abs 280 nm);. Optical density (Abs 420 nm); Total polyphenols (mg/L); Methanol (mg/L); Acetoin (mg/L). Color intensity (Abs 420+520+620 nm); Tonality (Abs 420/520 nm). Hue angle (hab); Chroma (C*). Abbreviations: YV, young wine vinegar; AV, aged vinegar; CH, chopped; CR. crushed. *The significant differences between the different variables are shown in Table S1, Supplementary Material. All physicochemical parameters were determined in triplicate for each sample. 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License 8952 A COMPREHENSIVE CHARACTERIZATION STUDY as optical density, color intensity, tonality, and b* and hab values; while for the crushed figs, significantly higher values were obtained in parameters such as L*, a* and C*. This explained that the wine vinegar samples with fresh crushed figs had a redder coloring, while those with fresh chopped figs had a more yellowish hue. Taking into consideration the influence of the base wine vinegar used in the physicochemical parameters, independently of the amount of dried fig macerate (10YV-10AV; 20YV-20AV), the results showed that the values of ash (g/L), TPI, optical density, color intensity, total polyphenols, methanol, and a* were significantly higher in the case of aged wine vinegar, while L* and hab presented an opposite trend (Table 2and Table S1). This is explained by the fact that the difference is already in the base wine vinegar, so the final products kept it. In summary, the study of the physicochemical parameters showed a wide variation in the characteristics of wine vinegars obtained according to the different production conditions considered in this work. In general, the maceration of vinegars with figs produced wine vinegars with higher sugar and total polyphenols amount, as well as a lower acidity, improving their characteristics and making them more attractive to the consumer. 3.2 Determination of the sensory profile and volatile compounds 3.2.1 Sensory profile All the samples considered in this study were described by a sensory analysis expert panel, and the selected attributes assessed were the following: fruity, caramel, nutty, wood, vanilla, ethyl acetate, acetic acid and wine character aromas, and taste balance, visual and overall impression. These sensory attributes have been defined and used previously by other researchers (Morales et al., 2006;Tesfaye et al., 2010) in similar samples, except taste balance and visual impression. The taste balance is the perception of the overall balance of the product in the mouth and visual impression is the assessment of the product’s aspect perceived by sight. For comparison purposes, the mean intensity values of the attributes of the different sample types considered in this work have been plotted as spider graphs (Figure 1). In general, regardless of the type of the fig (fresh or dried), the addition type of the fig (chopped or crushed) or the amount of fig added to the wine vinegars (10%, 20% or 30%), the sensory attributes that reached the highest values were the wine character and fruitiness, followed by others such as acetic acid, nutty, caramel, wood, ethyl acetate and vanilla, as can be seen in Figure 1. On the one hand, regardless of amount of fig employed, the main significant differences appeared with the addition of at least 20% of fig, which gave a greater complexity to the sensory profile of the original vinegars. In fact, these macerated vinegars (Figure 1) had significantly higher values of fruity attribute, and higher scores in general attributes such as overall and visual impression, as occurs with other macerated vinegars studied in the literature (Bruna-Maynou et al., 2020). These results are consistent, as it is expected, with that the higher the amount of fruit, the higher the perception of fruit attribute in this type of vinegars. Clearly, the fruity attribute is a sensory characteristic provided by the added fruit, while attributes such as ethyl acetate (glue) or wood are intrinsic to the base wine vinegar used, as they did not increase with the addition of fig (Figure 1). Similar sensory results were also observed in other vinegars macerated with other fruits (Bruna-Maynou et al., 2020). Regarding the type of fig employed (fresh or dried), there were also observed differences in the final sensory profile of the macerated vinegars, mainly with at least 20% of fig addition (Figure 1). Thus, those ones produced with dried figs showed significantly higher values for nutty and caramel attributes, while vinegars macerated with fresh figs seemed to present a better visual impression. Nutty and caramel attributes could be characteristic aromatic attributes of Maillard reaction and are typical of aged wine vinegars (Ríos-Reina et al., 2020). That is why dried figs seem to provide or enhance sensory notes in line with aged wine vinegar, which may have the effect of simulating it and, therefore a higher vinegar quality. With respect to the effect of crushing or chopping studied with fresh figs (Figure 1a,b), it did not seem to influence the final products significantly, which were relatively similar regardless of the addition type in which the fig was added (chopped, CH, or crushed, CH). On the other hand, the use of an aged or a young wine vinegar as base material seemed to have a strong influence in the final sensory profile. Figure 1c,d showed that the sensory profile between both base wine vinegars and their maceration products were very different, agreeing with the difference of the sensory profile of each base wine vinegar. In fact, when the wine vinegar used for the maceration of the dried fruit was compared (young -Y- and aged -A- ), the mean intensity values of the attribute wood showed significant differences between both samples, as expected. Moreover, when a dried fig was added at 20% to young wine vinegar, the attributes caramel and nutty increased (Figure 1c) with respect to the base young wine vinegar even reaching scores very similar to the aged base vinegar as well as the aged vinegars macerated. These did not occur when a fresh fig was added to the base young wine vinegar (Figure 1a). These sensory descriptors have been related to 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License A COMPREHENSIVE CHARACTERIZATION STUDY 8953 FIGURE 1 Spider graphs of the sensory profile of the mean values of the attributes of the samples studied. Attributes marked with a red * were those with significant differences between the amount of frig added; a green * were those with significant differences between the type of fig added (fresh or dried); a blue * were those with significant differences between the base wine vinegar (young or aged). vinegar aging time in wood (Callejón et al., 2008b), but also they could also be related to figs submitted to dry. For example, the enhancing of the caramel attribute could be related to the fact that the dried fig has a high percentage of sugars, and they caramelize during the drying process. In addition, a greater composition of volatile compounds, formed during the drying process of the figs, could contribute to the presence of these attributes (nutty and caramel) in them (Palassarou et al., 2017). However, when comparing the aged wine vinegar macerated with dried figs (DFA) and the aged base wine vinegar (A) (Figure 1d), the fruity attribute was the only one that was significantly higher in the macerated samples, but nutty and caramel did not significantly increase, which could be masked by the sensory properties of the aged base wine vinegar used. All these sensory results revealed that, during the maceration process, several volatile compounds from the figs are transferred to the vinegar, increasing the fruity character, whereas some losses or masking of volatile compounds from the base wine vinegar, mainly responsible for the wine and wood character, may have occurred. That explains that the use of aged wine vinegar as the base material, which already has a complex aroma, instead of young vinegar, will lead to less change in the sensory profile, mainly in those attributes related to the vinegar and not to the fruit. This will be discussed in the following section by the study of the volatile profile of each sample. 3.2.2 Profile of volatile compounds In this study, a total of 74 volatile compounds were considered. The mean values of their relative peak area, as well as their standard deviation and statistical results of the analysis of variance (ANOVA) are shown in Tables 3and 4. Among these 74 volatile compounds, nine were acetic acid esters, four acids, ten alcohols, two aldehydes, four C13-norisoprenoids, eight ethyl esters, two hydrocarbons, four indenes, three ketones, five lactones, three volatile phenols, 15 terpenes and five were classified as “others”. In this section, different comparisons were made between all study conditions and the volatile compounds determined. In general, results showed, as it can be expected from the sensory assessment, that most of the volatile compounds exhibit significant differences in the comparisons performed (p<0.05) (Tables 3and 4). Thus, 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License 8960 A COMPREHENSIVE CHARACTERIZATION STUDY TABLE 4 (Continued) Base wine vinegar Dried fig Base wine vinegar Dried fig Tukey results of base vinegar YV T DF10Y T DF20Y T AV T DF10A T DF20A T 10% 20% N Volatile compounds LRI ID Odor descriptionaMean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD YV AV YV AV Alcohols 14 Isobutanol 1096 ARuber, sweat 0.09 0.00 0.09 0.00 0.11 0.09 0.09 0.00 0.07 0.01 0.06 0.00 15 2-Methyl-1-butanol 1211 A Green, rancid, alcohol 2.57 0.00 2.52 0.46 1.71 0.23 2.81 0.00 b 1.80 0.06 a 1.72 0.02 a 16 3-Methyl-1-butanol 1215 ARancid 2.17 0.00 2.54 0.47 1.72 0.22 2.77 0.10 b1.83 0.05 a1.71 0.07 a 17 1-Hexanol 1361 A Herbal, pungent 0.00 0.00 0.00 0.00 0.00 0.00 0.01 0.01 0.00 0.00 0.01 0.00 18 3-Ethoxy-1-propanol 1385 A0.02 0.00 0.03 0.00 0.02 0.00 0.05 0.00 b0.03 0.00 a0.03 0.00 a 19 (E)-3-Hexen-1-ol 1388 B1Grass, green, leaf, herb 0.00 0.00 0.01 0.00 0.00 0.00 0.01 0.00 b 0.00 0.00 a 0.00 0.00 a B A 20 2-Ethyl-1-hexanol 1495 B1Citrus, fresh 0.05 0.00 0.06 0.00 0.03 0.01 0.08 0.01 b0.06 0.00 ab 0.04 0.00 a 21 1-Nonanol 1668 A Floral, rose 0.02 0.00 0.02 0.01 0.01 0.00 0.01 0.00 0.01 0.00 0.01 0.00 22 Benzyl alcohol 1891 ACherry, fruit 0.15 0.00 0.17 0.02 0.05 0.06 0.35 0.00 b0.22 0.00 a0.22 0.01 a 23 2-Phenylethanol 1929 A Floral, rose, sweet 7.02 0.06 7.65 1.13 5.06 0.80 8.18 0.00 b 5.64 0.18 a 5.49 0.03 a Aldehydes 24 Benzaldehyde 1511 A Cherry 0.40 0.00 1.20 0.19 1.36 0.54 1.76 0.01 b 0.55 0.03 a 0.51 0.44 a B A 25 2,5-Dimethyl-benzaldehyde 1810 C2.88 0.02 4.53 0.93 2.37 0.90 2.72 0.01 b2.70 0.00 b2.39 0.07 a C13-Norisoprenoids 26 2,4,4-Trimethyl-3-(3- methylbutyl)cyclohexen-2-one 1735 C0.32 0.00 a0.55 0.07 b0.39 0.06 ab 0.54 0.00 b0.45 0.02 ab 0.40 0.04 a 27 (Z)-β-Damascenone 1756 B1Apple, compotem quince 0.00 0.00 a0.11 0.02 b0.10 0.00 b0.01 0.00 a 0.08 0.00 b 0.12 0.00 c 28 (E)-β-Damascenone 1823 AFloral, rose, sugar 0.01 0.01 a0.92 0.21 b0.90 0.02 b0.05 0.00 a0.72 0.05 b0.98 0.03 c 29 β-Ionone 2014 C Floral, woody, sweet fruity 0.00 0.00 a0.01 0.00 b0.02 0.00 c0.01 0.00 a 0.03 0.00 b 0.05 0.01 b A B A B (Continues) 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License A COMPREHENSIVE CHARACTERIZATION STUDY 8961 TABLE 4 (Continued) Base wine vinegar Dried fig Base wine vinegar Dried fig Tukey results of base vinegar YV T DF10Y T DF20Y T AV T DF10A T DF20A T 10% 20% N Volatile compounds LRI ID Odor descriptionaMean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD YV AV YV AV Ethyl esters 30 Ethyl isovalerate 1055 AAcid strawberry, banana 1.37 0.12 c0.77 0.05 b0.34 0.01 a1.91 0.28 b0.42 0.05 a0.28 0.01 a B A B A 31 Ethyl 2-butanoate 1147 B1Pungent, musty, caramellic 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 32 Ethyl sorbate 1499 B1Fruity, sweet, pineapple 0.06 0.01 b0.04 0.01 ab 0.01 0.00 a0.03 0.00 b0.01 0.00 a0.01 0.00 a 33 Ethyl 2-hydroxy-4-methylvalerate 1532 B1Blackberry, fruity 0.01 0.00 0.03 0.01 0.02 0.00 0.26 0.00 b 0.20 0.00 a 0.20 0.00 a A B 34 Ethyl 3-hydroxybutyrate 1580 B1Fruity, grape 0.28 0.00 0.33 0.06 0.26 0.04 0.42 0.01 c0.30 0.00 a0.32 0.00 b 35 Ethyl phenylacetate 1781 A Floral, honey, rose 0.40 0.00 b0.30 0.08 ab 0.17 0.00 a0.65 0.02 b 0.29 0.01 a 0.25 0.00 a A B 36 Diethyl 2-hydroxy-3-methylsuccinate 1859 C0.01 0.00 0.01 0.00 0.01 0.00 0.05 0.00 0.05 0.00 0.05 0.00 A B A B 37 Ethyl hexadecanoate 2237 A Waxy, creamy, milk 0.01 0.00 a0.03 0.01 ab 0.03 0.01 b0.01 0.00 0.02 0.00 0.05 0.05 Hydrocarbures 38 Tetradecane 1395 A Mild waxy 0.06 0.00 0.06 0.01 0.04 0.01 0.05 0.00 0.03 0.01 0.05 0.02 39 Pentadecane 1498 AWaxy 0.06 0.00 a0.08 0.00 b0.04 0.01 a0.05 0.00 0.04 0.00 0.05 0.01 B A Indenes 40 1-Methylene-1H-indene 1730 B11.24 0.01 1.27 0.23 0.55 0.21 0.73 0.01 0.58 0.06 0.59 0.15 41 1-Ethylidene-1H-indene 1844 B10.10 0.00 0.11 0.01 0.05 0.02 0.08 0.00 b 0.06 0.00 ab 0.05 0.00 a B A 42 1,1,3-Trimethyl-1H-indene 1908 C0.00 0.00 0.01 0.00 0.01 0.00 0.00 0.00 a0.00 0.00 a0.01 0.00 b 43 3-(2-Methyl-propenyl)-1H-indene 2178 C 0.02 0.00 0.01 0.01 0.01 0.00 0.17 0.00 c 0.06 0.01 b 0.03 0.00 a A B A B Ketones 44 Acetoin 1279 A Milk, dairy 1.09 0.00 1.11 0.11 0.78 0.19 1.12 0.00 b 0.59 0.04 a 0.59 0.01 a B A 45 6-Methyl-3,5-heptadiene-2-one 1590 B1Green, herbal 0.00 0.00 a0.04 0.00 b0.06 0.01 b0.01 0.00 a0.03 0.00 b0.05 0.00 c 46 6-Pentyl-2H-pyran-2-one 2203 B1Coconut, creamy 0.17 0.01 b0.13 0.02 b0.07 0.01 a0.01 0.00 0.03 0.00 0.01 0.00 B A B A Lactones 47 (Z)-Oaklactone 1900 C Spicy, vanilla 0.06 0.01 0.05 0.01 0.03 0.00 0.15 0.00 b 0.13 0.00 a 0.13 0.00 a A B A B 48 (E)-Oaklactone 1973 B3Coconut, spicy 0.29 0.00 0.29 0.07 0.21 0.03 0.72 0.00 b0.47 0.00 a0.46 0.01 a A B 49 ƴ-Nonalactone 2046 A Milk, cream, vanilla 0.03 0.00 a0.07 0.01 b0.08 0.01 b0.10 0.00 a 0.11 0.00 a 0.14 0.01 b A B A B 50 4-Methyl-5-penta-1,3- dienyltetrahydrofuran-2-one 2177 CFruity 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 B A 51 4-Methyl-5-penta-1,3- dienyltetrahydrofuran-2-one 2204 C Fruity 0.00 0.00 a 0.01 0.01 b 0.01 0.00 b 0.02 0.00 c 0.01 0.00 b 0.00 0.00 a Volatile phenols 52 4-Methylguaiacol 1964 B1Sweet, vanilla 0.06 0.00 b0.06 0.01 ab 0.03 0.01 a0.09 0.00 b 0.05 0.00 a 0.05 0.00 a 53 4-Ethylguaiacol 2040 A Cinnamon, clove, hazelnut 0.15 0.01 0.13 0.03 0.09 0.01 0.49 0.00 c0.27 0.00 b0.24 0.01 a A B A B 54 4-Ethylphenol 2195 A Tempera, leather 0.16 0.00 b0.14 0.03 ab 0.08 0.01 a0.35 0.00 c 0.19 0.01 b 0.13 0.00 a A B (Continues) 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License 8962 A COMPREHENSIVE CHARACTERIZATION STUDY TABLE 4 (Continued) Base wine vinegar Dried fig Base wine vinegar Dried fig Tukey results of base vinegar YV T DF10Y T DF20Y T AV T DF10A T DF20A T 10% 20% N Volatile compounds LRI ID Odor descriptionaMean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD Mean ±SD YV AV YV AV Others 55 3,6-Dimethyl-2,3,3a,4,5,7a- hexahydrobenzofuran 1516 C0.00 0.00 a0.01 0.00 b0.01 0.00 b0.01 0.00 0.01 0.00 0.02 0.01 56 Methyl salicylate 1767 A Minty 0.08 0.00 b0.07 0.01 b0.04 0.01 a0.17 0.00 b 0.07 0.01 a 0.07 0.00 a 57 i-Propyl 12-methyl-tridecanoate 2041 C0.20 0.00 0.20 0.06 0.11 0.01 0.13 0.04 0.09 0.02 0.06 0.02 58 Diphenyl sulfide 2270 B1Sulfurous 0.35 0.02 c0.22 0.00 b0.12 0.02 a0.28 0.00 b 0.09 0.01 a 0.08 0.00 a B A 59 2,5-Dihydro-thiophene 2306 C0.23 0.01 0.14 0.07 0.10 0.01 0.63 0.00 b0.25 0.15 a0.24 0.01 a A B Terpenes 60 Myrcene 1144 A Spicy, herbaceous 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 61 (Z)-p-Mentha-2,8-dien-1-ol 1198 C Mint 0.00 0.00 a0.04 0.01 b0.04 0.00 b0.00 0.00 a 0.03 0.00 b 0.05 0.01 b 62 Terpinolene 1267 B1Herbal 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.01 0.00 63 Nerol oxide 1464 C Green, herbal 0.00 0.00 a0.05 0.00 b0.05 0.00 b0.00 0.00 a 0.04 0.00 b 0.06 0.01 b 64 (E)-Linalool oxide 1473 AFruit, flower, strawberry 0.05 0.00 a0.11 0.01 b0.12 0.00 b0.12 0.00 a0.14 0.00 ab 0.21 0.04 b 65 Linalool 1547 A Citrus, floral 0.01 0.00 0.03 0.01 0.02 0.00 0.01 0.00 0.01 0.00 0.07 0.07 66 Myrcenol 1615 A Floral, lavender 0.01 0.00 b0.00 0.00 anp np a0.02 0.00 c0.01 0.00 b0.00 0.00 a A B 67 (Z)-Ocimenol 1660 B10.02 0.01 0.01 0.00 0.01 0.00 0.05 0.00 0.03 0.00 0.02 0.00 A B A B 68 (E)-Ocimenol 1684 B10.03 0.00 b0.01 0.01 ab 0.01 0.00 a0.09 0.00 c0.05 0.00 b0.04 0.00 a A B 69 α-Terpineol 1707 A Terpenic, citrus 0.01 0.00 0.04 0.02 0.05 0.02 0.03 0.00 0.03 0.00 0.13 0.12 70 Geranyl vinyl ether 1720 C0.01 0.00 0.01 0.00 0.00 0.00 0.02 0.00 0.01 0.00 0.04 0.00 71 Geraniol 1860 A Floral, sweet, rosy 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.01 0.01 72 2,6-Dimethyl-2,7-octadiene-1,6-diol 2226 C0.00 0.00 a0.00 0.00 a0.01 0.00 b0.00 0.00 0.00 0.00 0.01 0.00 73 Geranyl isovalerate 2251 C Fruity, apple, blueberry 0.02 0.00 0.02 0.00 0.02 0.00 0.05 0.01 b 0.03 0.00 a 0.03 0.00 a 74 2,6-Dimethyl-2,7-octadiene-1,6-diol 2292 C0.00 0.00 np np 0.01 0.00 0.00 0.00 0.00 0.00 0.00 0.00 Note: LRI: Experimental linear retention index values estimated by linear regression. ID: reliability of identification: A. mass spectrum and LRI agreed with standards; B. mass spectrum agreed with mass spectral data base and LRI agreed with the literature data; C. mass spectrum agreed with mass spectral data base; Literature reference agreed with LRI data: 1National Center for Biotechnology Information (2004); 2Choi et al. (2002); 3Campo et al. (2006). References are included in the Reference section. aOdor description reported in literature and databases. Abbreviations: Mean, mean area values relative to the internal standard; SD, standard deviation; YV, young wine vinegar; AV, aged wine vinegar; DF, dried fig; 10%–20%: amount of dried figs used; T: Tukey’s test. Different letters in the same row indicates statistically significant differences (p<0.05): lowercase (a, b, c) indicates statistically significant differences between young wine vinegar without fruit and young wine vinegar with fruit in different amounts; lowercase italic (a, b, c) indicates statistically significant differences between aged wine vinegar without fruit and aged wine vinegar with fruit in different amounts; capital letter (A, B, C) indicates statistically significant differences between pairs of samples with the same amount of dried fig but different base wine vinegar (YV-AV). All samples were analyzed in duplicate. 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License A COMPREHENSIVE CHARACTERIZATION STUDY 8963 FIGURE 2 Scores (a) and loadings (b) plots obtained by the PCA model developed considering the relative area of volatile compounds and the scores of the sensory attributes of all the samples under study. AV, aged vinegar; DF, dried fig; FF, fresh fig; YV, young vinegar. only two volatile compounds, 1-hexanol and 1-nonanol, did not show these differences in any of the comparisons. Moreover, in general, the effect of maceration processes produced increases on some volatile compounds and the apparition of others that were not detected in the base wine vinegars. Thus, from the total of volatile compounds, some were not detected in any base wine vinegar, but increased with the amount of fig added for maceration (Tables 3and 4). Among them, (Z)-p-mentha-2,8-dien-1-ol and 1,1,3-trimethyl-1H-indene were not present in the base aged and young wine vinegar, so they could be compounds that may proceed from the fig or are produced during the maceration process with fig. 3.2.3 Multivariate analyses of sensory and volatile profiles This study contemplates the comparison and assessment of many different factors to better study and explores the effect of different vinegar maceration conditions with figs in the volatile profile of these products and their relationship with the sensory profiles, so a multivariate approach was used. Thus, for this purpose, three PCA models were performed merging the relative peak area values of volatile compounds and the scores of the sensory attributes, considering different sets of samples in order to easily study the influence of each factor: all the samples (Figure 2); only vinegars macerated with fresh fig (Figure S2a,b); and only vinegars macerated with dried fig (Figure S2c,d). Influence of macerating with different amounts (%) and types of figs (FF or DF) The scores plot of the PCA model made with all the samples (Figure 2a) shows that samples from dried (DF) and fresh figs (FF) and the percentage of fig used could be differentiated according to their volatile and sensory profiles. Thus, the combination of the first and second principal components (PC1 and PC2), with a total of 67.79% of explained variance, separated the samples according to the percentage of fig added. The base wine vinegars were in the extremely positive part of PC1 and vinegars macerated with higher amount of fig in the negative part of PC1. It was also considered the type of fig used for maceration. The samples macerated with dried figs (DF) were mainly in the positive side of PC1 and PC2, and the ones macerated with fresh figs (FF), in the negative side of PC1 and PC2. The base wine vinegar used also showed an influence on the volatile and sensory profiles, mainly explained by PC2. These results agreed with the ANOVA results of the sensory attributes (Figure 1), as well as of the volatile compounds (Tables 3and 4), since according to the volatile significant changes, the factor “amount of fig added for maceration” seemed to be the most influential one in the final volatile profile, in which 61 volatile compounds showed significant differences (Tables 3and 4), followed by the factor “type of fig used” (dried of fresh) with 24 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License 8964 A COMPREHENSIVE CHARACTERIZATION STUDY volatile compounds with significant differences (data not shown). On the one hand, regarding the effect of the amount of fig added for maceration, by looking at the loadings (Figure 2b), it can be seen again that the sensory attributes fruity, caramel, taste, visual and overall impression were more related to macerated vinegars with fig than with the base wine vinegars, and specially with samples macerated with a higher percentage of fig, as expected. In contrast, as it was observed before, wine, woody, acetic acid, and ethyl acetate attributes were more related to the base wine vinegars not macerated with figs. Moreover, regarding the volatile profile, in general terms and independently of the type of fig added and the base wine vinegar used, it could be seen in the loadings plot (Figure 2b) that most of the volatilecompoundsstudiedwereplaced in the positiveside of PC1, where the base wine vinegars were placed. This is explained by the fact that most of them presented a significant decrease in their values with only an addition of 10% of macerated fig (Tables 3and 4), which could be due to the dilution effect that could occur with the addition of fresh figs, or even by reactions that could occur between fig and vinegar compounds in the case of fresh and dry figs. Thus, 11 volatile compounds showed this trend in all the samples, both dried and fresh figs, and in young and aged base wine vinegar (Tables 3and 4), being more present in the base wine vinegars, and commonly described in wine vinegars (Ríos-Reina et al., 2019). These compounds were: four acetic acid esters (ethyl acetate, isobutyl acetate, isoamyl acetate and 3-(methylthio)propyl acetate), two volatile phenols (4-methylguaiacol and 4-ethylphenol), 3 ethyl esters (ethyl isovalerate, ethyl sorbate and ethyl phenylacetate) and two others (diphenyl sulphide and methyl salicylate). In contrast, there was a lower number of compounds that showed an increasing trend with the addition of fig (Tables 3and 4), which could be acquired from the fruit added to the plain vinegar for maceration. These compounds were seven: one ketone (6-methyl-3,5- heptadiene-2-one); two C13-norisoprenoids ((Z)- and (E)- β-damascenone); three terpenes ((Z)-p-mentha-2,8-dien- 1-ol, nerol oxide and (E)-linalool oxide); and one indene (1,1,3-trimethyl-1H-indene). Among them, 6-methyl-3,5- heptadiene-2-one was the only one that increased significantly over with the addition of the minimum percentage used. Thus, this compound (numbered as 45), a ketone described with green attributes, was one of the volatile compounds placed in the negative side of PC1 in the scores plot, near fruity attribute (Figure 2b) and where the macerated vinegars were placed (Figure 2a), being therefore more related to them. According to the literature, various compounds from this chemical group are strongly presented in figs (Russo et al., 2017). Moreover, 1,1,3- trimethyl-1H-indene or (Z)-p-mentha-2,8-dien-1-ol, which also increased with fig addition, were not detected in base wine vinegars, as mentioned above, and were only presented in macerated vinegars (Tables 3and 4). Regarding the other four compounds that increased with fig addition, (E)-linalool oxide and β-damascenone have been described also as fig volatile compounds (Grison- Pigé et al., 2002), being the latter also described as the ‘key’ compound of dried fig aroma (Palassarou et al., 2017). On the other hand, regarding the effect of using fresh or dried fig in the vinegar maceration, its influence is different on the volatile profile of the final product depending on the percentage added. Thus, for a better understanding of these differences, Figure S1 was drawn considering volatile compounds with statistically significant difference between fresh and dried fig for the same macerating conditions. As can be observed, ten volatile compounds showed significant differences between using fresh or dried figs when only a 10% is added to the base vinegar (Figure S1a), while 15 of them (Figure S1b)showedsignificant differences with a maceration with 20% of figs. Among both percentages added (10% or 20%), there were only two compounds of all the above mentioned in common and showed significant differences among the use of fresh and dried figs: diethyl 2-hydroxy-3-methylsuccinate (36) and ƴnonalactone (49). These two compounds showed a greater presence in the dried figs (Figure 2a and Figure S1)and were related with nutty aroma according to the PCA loadings plot (Figure 2b). This last compound, ƴ-nonalactone, has an odor reminiscent of coconut, and due to its low threshold (Nakamura et al., 1988), it could contribute to the final aroma of these vinegars. It is one of the aroma constituents in apricots, peaches, pineapples, and coconut (Nakamura et al., 1988). On the contrary, in the maceration with fresh figs, the volatile compounds with higher significant amount were mainly terpenes, as can be observed in Figure 2, where almost all these terpenes showed negative PCA loading values as the fresh fig samples. Among these compounds were terpinolene (62), linalool (65), ocimenol isomers (67, 68), 2,6-dimethyl-2,7-octadiene-1,6-diol isomers (72, 74) and α-terpineol (69). These compounds could contribute to the vinegar with fruity nuances (Tables 3and 4), agreeing with the PCA loadings. Influence of maceration with different types of fresh fig addition (crushed or chopped) After studying the effect of the addition of different amounts and types of figs to the vinegars, the influence of addition type of fresh fig, crushed by mixer (CR) or chopped (CH) by knife, was studied. If Figure 2a is observed, it seemed that CR and CH had not an effect 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License A COMPREHENSIVE CHARACTERIZATION STUDY 8965 in the volatile and sensory profile of the samples, with the crushed and chopped samples with the same amount of fig placed closed to each one in the scores plot, and only separated by the percentage of fig amount. However, when a new PCA model was developed including only fresh fig samples (Figure S2a,b), by looking at the scores plot (Figure S2a), it could be seen that there were some differences between the use of crushed or chopped figs, explained by PC2. This agreed with the statistical results showed in Table 3, where it can be observed that the factor “fig’s addition type” (crushed or chopped) affected significantly to 8 volatile compounds (benzyl alcohol, ethyl hexadecanoate,1-methylene-1H-indene,3-(2-methyl- propenyl-1Hindene, linalool, geranyl vinyl ether, geraniol and geranyl isovalerate) having five of them (ethyl hexadecanoate, 1-methylene-1H-indene, linalool, geraniol and geranyl isovalerate) higher values in crushed samples (p<0.05) (Table 3). Influence of the use of different base wine vinegar (young vs aged) The differences according to the base wine vinegar used, young (YV) or aged wine vinegar (AV), was assessed only in vinegars macerated with dried figs, due to the addition of fresh figs to aged vinegars did not show, in a preliminary sensory test, any difference in the final product obtained. On the one hand, both in the overall PCA model (Figure 2a) and in a new PCA performed only with the dried fig samples (Figure S2c,d), it could be observed that the use of an aged or young base vinegar affected the volatile and sensory profiles. Thus, samples made with young and aged vinegars were separated by PC1 which explained a 49.28% of variance (Figure S2c). It is also shown that the addition of higher amounts of fig manifests higher differences in the final macerated vinegar when a young vinegar is used as a base than with the aged one, maybe due to the strong volatile and sensory notes that has the latter. The loadings plot of this PCA model (Figure S2d)showed that samples made with aged vinegar showed a higher relation, and therefore, higher scores of sensory attributes such as visual and overall impression, wine character, caramel, nutty andwoody, as well as taste balance, agreeing with the statistical sensory results (Figure 1). Regarding the volatile profile, the loadings plot also showed a higher relation between many volatile compounds from the ethyl esters, terpenes, and lactones’ families, and samples made with aged vinegar (Figure S2d). Thus, the results showed a correlation coefficient about −0.9 between the majority of the terpenes and the sensory note of acetic acid, and a correlation coefficient around 0.7 for fruity notes, that is explained by the decrease of acidity of the sample macerated and the increase of fruity notes at the same time that the higher presence of terpenes in macerated wine vinegars. Indeed, by looking at the statistical results showed in Table 4(by comparing the same percentage of fig added), the factor “aging of the base vinegar used” showed 29 volatile compounds with significant differences between the macerated young and aged wine vinegars (Table 4). In this case, 17 of them had significantly higher relative areas in the aged base wine vinegar samples with respect to the young base wine vinegars. This fact means that, although in the aged vinegars they could decrease significantly with the addition of more figs, their values were still significantly higher than in the macerated young vinegars. This is the case, for example, of the group of lactones, such as (Z)-oaklactone (47), (E)-oaklactone (48) and Ƴ- nonalactone (49), which are compounds characteristic of wood and aging of vinegars. Thus, this compounds have been described as typical odorants of vinegars with a longer aging time such as Gran Reserva ones (Callejón et al., 2008a) due to they could be transferred from the wood of the barrel itself during aging. In addition, a significantly positive correlation (>0.9) was observed between the lactones (Z)-oaklactone, (E)-oaklactone, and ƴ-nonalactone and the sensory attributes wood and vanilla, that agreed with the above discussed fact that both volatile compounds and sensory attributes are characteristic of wood and aging of vinegars and were, therefore, more presented in macerated aged wine vinegars. To the contrary, the resting 12 volatile compounds (out of the 29 above mentioned) presented significantly higher values in macerated young vinegars than in macerated aged ones (Table 4). It should be highlighted ethyl isovalerate (30), isovaleric acid (12) and 6-pentyl-2H-pyran-2-one (46) for showing up in significant higher values in both percentages studied in macerated young vinegars than in macerated aged vinegars. This was again expected due to these compounds were already presented in the raw base young vinegar in higher values than in the raw base aged vinegar. On the other hand, by looking at the scores plot of Figure 2, it could be also observed that DF10Y was placed close to its base young vinegar (YV), while the DF20Y was more separated; this demonstrates again that the relevant change occurs with fig maceration at 20% and was mainly observed when a young vinegar was used as a base. Moreover, a higher separation of macerated aged wine vinegars could be observed from their base aged vinegar than of the macerated young wine vinegars from their base young vinegar, which means that the final macerated products made with dried figs, and aged wine vinegars produced a higher change in the final volatile and sensory profile of the samples than the maceration of a young vinegar with dried figs. In fact, this could be seen in the results presented 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License 8966 A COMPREHENSIVE CHARACTERIZATION STUDY in Table 4, where a greater number of compounds showed significant differences between the base and the macerated vinegars when an aged wine vinegar was used (i.e. 51 volatile compounds) than when a base young vinegar was employed (i.e. 29 volatile compounds). These results showed that the raw base wine vinegar used also have an important influence on the samples, as well as the amount of fruit added to them. Finally, many of the acetic acid esters and acids showed negative correlation coefficients for the fruity attribute and positive correlation coefficients for the ethyl acetate sensory attribute, which can be explained by the chemical odor that these compounds have. 4 CONCLUSIONS This study demonstrated the significant impact of macerating wine vinegars with figs on their physicochemical, volatile, and sensory profiles. The effects were influenced by the quantity and type of fig (fresh or dried) used, as well as the base wine vinegar, and whether the fig was crushed or chopped. Increasing the percentage of fig led to notable changes, such as the increase of the total content of sugars and polyphenols, the tonality, the fruity notes, the visual parameter, taste and overall impression. Conversely, certain volatile compounds decreased with higher fig content, particularly those closely associated with the base vinegar. Notably, macerated vinegars exhibited unique volatile compounds, mainly terpenes and ketones, such as (Z)- p-mentha-2,8-dien-1-ol, or β-damascenone, among others, which increased with greater fig addition. Moreover, vinegars macerated with dried figs displayed heightened nutty and caramel nuances and superior physicochemical properties compared to those with fresh figs, resembling aged wine vinegar. Additionally, the choice of base vinegar, aged or young, significantly influenced the final properties of the macerated vinegar, reflecting differences inherent to the base vinegar, so the final products kept similar conditions. Overall, the study highlights that macerating wine vinegars with figs enhances fruity notes and overall sensory appeal, supported by changes in tonality, sugar, polyphenol content, acidity, and specific volatile compounds, potentially making these products more appealing to consumers. AUTHOR CONTRIBUTIONS M. P. Segura-Borrego: Investigation; writing—original draft; formal analysis; data curation; software. P. Ramírez: Conceptualization; visualization; supervision. R. Ríos-Reina: Investigation; writing—original draft; methodology; software; formal analysis; data curation. M. L. Morales: Conceptualization; investigation; validation; visualization; writing—review and editing; supervision. R.M. Callejón: Conceptualization; supervision; resources; writing—review and editing; visualization; validation. J. M. León Gutiérrez: Investigation; validation; methodology; formal analysis; software; data curation; writing—original draft; visualization. ACKNOWLEDGMENTS This work was supported by the project Ref. AT21_00018 of the Andalusian Plan for Research, Development and Innovation (PAIDI 2020) and by the Andalusian Institute of Agricultural and Fisheries Research and Training (IFAPA) and the European Rural Development Fund (ERDF, EU) through the project “Transferencia y Cooperación en Vitivinicultura Andaluza (TRANSVITI)” (PP.TRA.TRA2019.007). The authors would like to thank the PIF scholarship of the University of Seville (VIPPIT-2019-IV.3) and would also like to thank to the “VI Plan Propio de Investigación y Transferencia” of the University of Seville for Dr. Ríos- Reina current contract (Contract number USE-24,706-G). The researchers are also grateful to aid for knowledge transfer activities, on a competitive basis, within the scope of the Andalusian Plan for Research, Development and Innovation (PAIDI 2020), Ref. AT21_00018. This study was also part funded by the Andalusian Institute of Agricultural and Fisheries Research and Training (IFAPA) and the European Rural Development Fund (ERDF, EU) through the project “Transferencia y Cooperación en Vitivinicultura Andaluza (TRANSVITI)” (PP.TRA.TRA2019.007). CONFLICT OF INTEREST STATEMENT The authors declare no conflicts of interest. DATA AVAILABILITY STATEMENT Data will be made available on request. ORCID RaquelMaría Callejón https://orcid.org/0000-0001- 5285-4575 REFERENCES Bruna-Maynou, F. J., Castro, R., Rodríguez-Dodero, M. C., Barroso, C. G., & Durán-Guerrero, E. (2020). Flavored Sherry vinegar with citric notes: Characterization and effect of ultrasound in the maceration of orange peels. Food Research International,133, 109165. https://doi.org/10.1016/j.foodres.2020.109165 Caliskan, O. (2015). Mediterranean Figs (Ficus carica L.) functional food properties. In The Mediterranean Diet: An Evidence-Based Approach, (pp. 629–637). 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Journal of Food Science,89, 8945–8968. https://doi.org/10.1111/1750-3841.17485 17503841, 2024, 12, Downloaded from https://ift.onlinelibrary.wiley.com/doi/10.1111/1750-3841.17485 by Readcube (Labtiva Inc.), Wiley Online Library on [01/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License