Open AccessArticle

Enrichment of White Wine Vinegar with Aromatic Plants: The Impact on Aromatic, Polyphenolic, and Sensory Profiles

Marin Krapac

^1,*

Nikola Major

^1,*

Tomislav Plavša

¹,

Ana Jeromel

²,

Ivana Tomaz

and

Danijela Poljuha

Institute of Agriculture and Tourism, Karla Huguesa 8, HR-52440 Poreč, Croatia

Department of Viticulture and Enology, Faculty of Agriculture, University of Zagreb, Svetošimunska 25, HR-10000 Zagreb, Croatia

Authors to whom correspondence should be addressed.

Appl. Sci. 2024, 14(16), 6909; https://doi.org/10.3390/app14166909

Submission received: 9 July 2024 / Revised: 2 August 2024 / Accepted: 5 August 2024 / Published: 7 August 2024

(This article belongs to the Special Issue Natural Products and Bioactive Compounds)

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Figure 1
Scheme of vinegar production and analysis. "> Figure 2
Differences in the odorant series (herbal, floral, fruity, sweet, spicy, camphor-like, and unpleasant) of the flavored vinegars (shown as a bar graph) compared to the control treatment (shown on the x-axis) expressed as percentage changes. The odor series is represented by the sum of mean values of all compounds of the same odorant series where a significant difference between treatments was determined. "> Figure 3
Principal component analysis (PCA) for vinegars: (a) treatments (cases); (b) aromatic groups—blue letters; phenolic groups—green letters (variables). Abbreviations: Alc—alcohols, Acd—acids, Est—esters, Ter—terpenes, Otha—miscellaneous aromas, Ant—anthocyanins, Fla—flavones, FlaOL—flavonols, Fla-3-ol—flavan-3-ol, Dhf—dihydroflavonols, HbA—hydroxybenzoic acids, HcA—hydroxycinnamic acids, HppA—hydroxyphenylpropanoic acids, Stil—stilbenes, Hba—hydroxybenzaldehydes, Ty—tyrosols. "> Figure 4
Comparison of the odor properties of flavored vinegars (elderflower, rosemary, and thyme) and the control treatment. An analysis of variance (ANOVA) was performed to determine if there was a significant difference among the odor properties of the vinegars. Odor properties marked with asterisks (**, p ≤ 0.01; ***, p ≤ 0.001) show significant differences. ">

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Abstract

Featured Application

Considering the weaker representation of white wine vinegar on the global market, its flavoring expands the range of products used in the culinary arts and gives additional value to the initial product. Rosemary, thyme, and elderflower contribute to the specific aromaticity of flavored white wine vinegar as well as its nutraceutical value. Due to the small amount of plant material needed for flavoring, the production of flavored vinegar could be economically viable.

Abstract

The food industry is developing intensively, and products that, with their characteristics, enrich the food taste and aroma are widely used in the culinary arts. White wine vinegar is often used as a food condiment and as dressing in salads. This research aims to explore the impact of the maceration of selected aromatic plants on the organoleptic properties, bioactive compounds, and sensory profile of white wine vinegar. The plants selected for white wine (cv ‘Malvazija istarska’) vinegar aromatization were rosemary (Rosmarinus officinalis L.) and thyme (Thymus serpyllum L.) dried leaves and black elder (Sambucus nigra L. ssp. nigra) flowers (elderflowers). Vinegar flavored with rosemary had more pronounced pinewood and herbal aromas, while spicy aromas dominated the vinegar with thyme. The elderflower-flavored vinegar, on the other hand, was characterized by a floral and fruity aroma. Among the analyzed vinegars, white wine vinegar flavored with elderflower had the highest polyphenolic content.

Keywords:

elderflower; thyme; rosemary; vinegar aromatization; bioactive compounds

1. Introduction

The production and consumption of wine vinegar are widespread worldwide, and the Mediterranean basin is home to a wine vinegar tradition that has lasted for centuries [1]. Traditional wine vinegar from Italy (balsamic vinegar or Aceto balsamico) or Spain (Sherry vinegar or Vinagre de Jerez) is widely recognized and highly valued on the global market [2]. Red wine vinegar is produced all around the globe, while white wine vinegar (WWV) is predominately produced in Italy and Turkey [3].

Nowadays, by diversifying and improving traditional food products with better organoleptic characteristics and nutraceutical value, the palette is expanding, contributing to a better market position. Consumers recognize functional foods, which, besides their nutritional value, have a positive effect on human health. Bioactive compounds, such as polyphenols, contribute to the health benefits of functional foods primarily because of their antioxidant and anti-inflammatory effects [4]. Wine vinegar is recognized as a functional food because of its antimicrobial, antioxidant, and antidiabetic effects [3].

Aromatic plants are useful food additives that improve food’s organoleptic and sensory characteristics [5]. To the best of our knowledge, there are only a few studies in which aromatic plants were used to improve the organoleptic characteristics of WWV. Some researchers investigated the use of fruits [6,7,8], herbs [6], vegetables [6], and mushrooms [6] for wine vinegar aromatization.

Aromatic plants are rich in volatile and polyphenolic compounds, which contribute to their odor, taste, and health properties [9]. The composition and amount of volatile and polyphenolic compounds depend on the aromatic plant species [10,11,12,13] and the growing conditions [14].

Plants are abundant in terpenes, which are a diverse class of organic compounds contributing to their aroma, flavor, and defense mechanisms [15]. They are synthesized from isoprene units and classified based on the number of these units, including monoterpenes, sesquiterpenes, diterpenes, triterpenes, and tetraterpenes [16]. In plants, terpenes play crucial roles in attracting pollinators, deterring herbivores, and inhibiting the growth of competing vegetation through allelopathy [17]. Many terpenes have antimicrobial, anti-inflammatory, and antioxidant properties, making them valuable in medicine and food preservation [18]. Monoterpenes like limonene and linalool are widely used in perfumery and cosmetics for their pleasant scents [19]. Sesquiterpenes and diterpenes contribute to the flavor and aroma profiles of various foods and beverages [20].

The main volatile compounds in rosemary leaves are verbenone, α-thujene, bornyl acetate, and camphor [21]; those in thyme leaves are p-cymene [22], while those in the elderflowers are dominated by hotrienol, linalool oxide, and α-terpineol [23,24].

Polyphenolic compounds or phenols, the secondary plant metabolites, are responsible for the positive health properties, longer shelf life, and organoleptic characteristics of food. The most abundant phenols in the aromatic plants used in this research are isorhamnetin-3-O-hexoside, carnosic acid, carnosol, rosmanol, epirosmanol, rosmaridiphenol, rosmarinic acid, and their methoxy derivatives in rosemary [10]; rosmarinic acid, caffeoyl rosmarinic acid, eriodictyol hexoside, kaempferol-O-hexoside, kaempferol-O-hexuronide [10], caffeic acid, p-caffeic acid [25] in thyme; and quercetin-3-O-rutinoside (rutin), 5-caffeoylquinic acid 1 (chlorogenic acid), and 3-feruloylquinic acid in elderflowers [26].

The aim of this study was to determine the volatile and phenolic compounds profile as well as the sensory profile of WWV with regard to the minimum quantity of dried aromatic plants necessary to maintain the distinctive attributes of the plant species in WWV.

According to our knowledge and the available literature, this is the first research on the flavoring of WWV with dry aromatic plants such as rosemary, thyme, and elderflowers.

2. Materials and Methods

2.1. Wine and Non-Flavored Vinegar Production

For the white wine production, grapes from the autochthonous cultivar ‘Malvazija istarska’ (clone VCR 4, rootstock KOBER 5BB) were used. To prevent the negative effect of oxidation during harvesting, instead of sulfite, pre-rehydrated non-Saccharomyces yeast Metschnikowia pulcherrima (LEVEL2 INITIA™, Lallemand Inc., Niagara-on-the-Lake, ON, Canada) was applied to the grapes at a dose of 0.2 g/kg. LEVEL2 INITIA™ has a high capacity for consumption of dissolved oxygen with a partial reduction in copper content, a known catalyst of oxidation reactions. After crushing, destemming, and pressing the berries, the must was gravity-settled for 48 h at 12 °C.

The clear must (68 NTU) was inoculated with 0.3 g/L of rehydrated dry yeast Saccharomyces cerevisiae (Lalvin QA23™, Lallemand Inc., Canada). On the third day from the start of fermentation, 0.3 g/L of the yeast nutrient Fermaid E (Lallemand Inc., Canada) was added.

Alcoholic fermentation was conducted at a temperature of 17 °C. It lasted 20 days (residual sugar < 1.0 g/L) and resulted in a wine with the following chemical parameters determined according to the method of the International Organization of Vine and Wine (OIV) [27]: 11.5 vol% of alcohol, 7.00 g/L of titratable acidity (expressed as tartaric acid), and pH 3.31. After decanting from the lees, the ‘mother of vinegar’ was added to the wine as a starter culture that will enable the oxidation of ethanol into acetic acid (acetification) (Figure 1). Acetification was carried out in a stainless-steel tank (100 L) by pumping air into the tank’s base three times a day at a temperature of 28 °C until complete oxidation of ethanol into acetic acid. The procedure resulted in white, non-flavored vinegar containing 6.2 g/L of acetic acid and 0.5 vol% of alcohol, which were determined using the OIV method for vinegar [28]. The vinegar was clarified with 1.0 g/L of bentonite (Mastervin Compact, Enologica Vason S.p.A.) before flavoring with herbs, and sulfite (potassium metabisulfite) was added as a preservative in a dose of 0.05 g/L.

2.2. Herbs and Vinegar Flavoring Procedure

Dried herbs were used for vinegar flavoring: rosemary (Rosmarinus officinalis L.) and thyme (Thymus serpyllum L.) leaves, and black elder (Sambucus nigra L. ssp. nigra) flowers (elderflowers). Fresh rosemary and thyme leaves and elderflowers were naturally dried in a dark and airy place until they had a consistent dry weight. A preliminary experiment was conducted to establish the optimal herbal dosage for each plant species in a sensory ranking test. The preliminary dosages of dry herbs used were 2, 4, 10, 20, and 40 g/L, while the maceration duration was 2, 4, and 8 days. Out of the tested dosages and maceration duration, the following were selected according to the best sensory rank: (a) rosemary—4 g/L and four days of maceration, thyme—4 g/L and four days of maceration, and elderflower—20 g/L and four days of maceration. The dried herbs were macerated at 20 °C in 5 L light-tight glass jars with hermetic lids in three repetitions (Figure 1). At the end of the maceration process, the herbs were sieved, and the vinegars were stored at 15 °C in 0.5 L bottles until analysis. The wine vinegar without herbal addition was used as a control.

2.3. Volatile Compounds Analysis

Volatile compound analysis employed solid-phase microextraction–gas chromatography/mass spectrometry (SPME-GC/MS). A total of 1 mL of the sample was combined with 3 mL of deionized water spiked with the internal standard, 2-octanol, in a 10-milliliter headspace vial and immediately capped. SPME extraction utilized an autosampler (AOC6000, Shimadzu, Kyoto, Japan) featuring a heated agitator set at 60 °C and an 80 µm DVB/C-WR/PDMS Smart SPME fiber (Shimadzu, Kyoto, Japan). Fiber preconditioning lasted 10 min, sample incubation lasted 30 min, and sample extraction lasted 40 min. Volatile compound separation occurred on a Rxi 5-MS column (Restek, Bellefonte, PA, USA). The SPME fiber was desorbed over 10 min in the injector port maintained at 250 °C with a splitless helium column flow of 1 mL per minute and a temperature program as follows: hold at 40 °C for 5 min, ramp to 220 °C at 10 °C/min, ramp to 300 °C at 15 °C/min, and hold at 300 °C for 5 min (GC2030, Shimadzu, Kyoto, Japan). MS parameters (TQ8040NX, Shimadzu, Kyoto, Japan) included an ion source temperature of 280 °C, interface temperature of 300 °C, electron impact ionization, and a mass scan range from 40 to 350 m/z. Kovat’s retention index for each compound was calculated against a mix of standard alkanes using the same temperature program. Compounds were identified utilizing both the Kovat’s index and the NIST17 database. The obtained peak areas were normalized against the internal standard and expressed as mg/L.

2.4. Targeted Analysis of Polyphenolic Compounds

The targeted compounds were identified and quantified by comparing their retention times and characteristic precursor/product ions to analytical standards (Extrasynthese, Genay, France) using an LC-ESI-QqQ system. This system comprised a controller (Shimadzu SCL-40), a degasser (Shimadzu Nexera DGU-405), two solvent delivery units (Shimadzu Nexera LC-40DX3, Kyoto, Japan), an autosampler (Shimadzu Nexera SIL-40CX3, Kyoto Japan), a thermostated column compartment (Shimadzu Nexera CTO-40C, Kyoto, Japan), and a QqQ mass spectrometer (Shimadzu LCMS8045, Kyoto, Japan). For reversed phase separation, 1 µL of the sample was injected onto a C18, 2.1 mm × 150 mm, 2.7 µm core–shell column (Agilent Poroshell C18, Palo Alto, CA, USA) maintained at 37 °C. A linear binary gradient elution of mobile phase A (water/0.1% formic acid) and mobile phase B (acetonitrile/0.1% formic acid) was employed at a flow rate of 0.30 mL/min: 0 min to 0.75 min: 98% A; 0.75 min to 15 min: 98% A to 50% A; 15 min to 15.1 min: 50% A to 0% A; 15.1 min to 20 min: 0% A; 20 min to 20.1 min: 0% A to 98% A; 20.1 min to 25 min: 98% A. The characteristic precursor/product ion pairs and method-validation parameters are presented in Supplementary Table S1.

2.5. Sensory Analysis

Seven experts participated in the sensory evaluation panel (four women and three men). We conducted a sensory analysis of vinegar twice. The first time, a preliminary tasting (ranking method) was used to determine the dose of dry herbs (2, 4, 10, 20, and 40 g/L) and the length of maceration (2, 4, and 8 days). We singled out marketable and commercially interesting treatments: rosemary (4 g/L and four days of maceration), thyme (4 g/L and four days of maceration), and elderflower (20 g/L and four days of maceration). The quantitative descriptive analysis was performed in triplicate on the flavored WWVs and the control. The intensities of each attribute (wine character, ethyl acetate, pungent, herbal, piney, fruity, floral, spicy, and general impression) were assessed on a scale from 0 (not noticeable) to 10 (very strong).

2.6. Statistical Analysis

One-way analysis of variance (ANOVA) was used to compare the means (aromatic and phenolic compounds n = 3; sensory analysis n = 7) at the level of significance of p ≤ 0.05. If significant, homogenous groups were determined using Fischer’s least significant difference (LSD) test. To obtain further insight into the data, principal component analysis (PCA) was performed on the data set. Statistical data analysis was performed with Statistica v. 13.2 software (Tibco Inc., Palo Alto, CA, USA).

3. Results

3.1. Aromatic Profile

Table 1 shows the aromatic profile of the obtained vinegar using 34 compounds divided into 5 groups: alcohols, acids, esters, terpenes, and other aromatic components. In the group of alcohols and acids, no significant changes were recorded in the concentrations of individual compounds, except for amyl vinyl carbinol, which was significantly higher in rosemary and thyme-flavored vinegars. Out of seven analyzed esters, a significant decrease was recorded in two of them, namely, 2-phenylethyl acetate for elderflower and rosemary-flavored vinegar and ethyl hexanoate for all flavored treatments in comparison to the control treatment. The highest increase compared to the control treatment was observed in the group of terpenes: rosemary-flavored vinegar (15-fold increase), thyme-flavored vinegar (11-fold increase), and elderflower-flavored vinegar (6-fold increase). Furthermore, there was a noticeable difference in the distribution of individual terpenes for each plant species. In rosemary-flavored vinegar, the following contributed the most to the total value of terpenes: γ-terpinene, 2-carene, camphor, D-carvone, eucalyptol, fennel, isoterpinolene, terpinen-4-ol, α-terpineol, and endo-borneol. In elderflower-flavored vinegar, the following contributed the most to the total value of terpenes: hortineol, linalool oxide, and linalool, while in thyme-flavored vinegar, the main representatives were p-cymene and p-thymol. In the group of other aromatic compounds, a significant increase compared to the control treatment was recorded only in the elderflower-flavored vinegar treatment.

3.2. Odorant Series

A bar chart (Figure 2) displays the odorant series. The odorant series (herbaceous, floral, fruity, sweet, spicy, camphor-like, and unpleasant) is represented by the sum of the mean values of all compounds of the same odorant series where a significant difference between treatments was determined (Table 1). The individual odorant series for each flavored vinegar is expressed as a percentage of change compared to the same aromatic series of the control treatment. The control treatment is represented by the 0-axis on the bar chart. The greatest single contribution to the overall aromatic profile of all flavored vinegars was made by the compounds that define the spicy aromatic series, and that was especially pronounced in thyme-flavored vinegar. Observing the arrangement of the other odorant series, it is evident that camphor-like, sweet, and herbaceous were the most pronounced in rosemary-flavored vinegar. On the other hand, elderflower-flavored vinegar was defined by an odorant series of floral characters.

3.3. Polyphenolic Profile

The polyphenolic profile of vinegars is shown in Table 2. Fifty-one compounds are divided into eleven polyphenolic sub-groups, namely, anthocyanin, flavones, flavonols, flavan-3-ol, dihydroflavonols, hydroxybenzoic acids, hydroxycinnamic acids, hydroxyphenylpropanoic acids, stilbenes, hydroxybenzaldehydes, and tyrosols. Elderflower-flavored vinegar has significantly higher concentrations of total anthocyanins, flavonols, hydroxybenzoic acids, hydroxycinnamic acids, hydroxybenzaldehydes, and tyrosols. The leading representatives of these phenolic sub-groups are malvidin-3-O-glucoside, quercetin, isorhamnetin-4′-O-glucoside, protocatechuic acid, p-hydroxybenzoic acid, chlorogenic acid, vanillin, and hydroxytyrosol. Sub-group flavones have significantly higher concentrations in vinegars flavored with rosemary and thyme. The most abundant compounds of this subgroup are apigenin-4-O-glucoside in rosemary-flavored vinegar, luteolin-7-O-glucoside in thyme-flavored vinegar, and luteolin-7-O-rutinoside, equally represented in both treatments.

3.4. Principal Component Analysis (PCA)

Principal component analysis (PCA) was applied to the data set consisting of treatments as cases (a) and data for total values of aromatic (Table 1) and phenolic (Table 2) groups as variables (b). The first three principal components (PC) had an eigenvalue greater than 1, cumulatively explaining 87.08% of the variability among the data. The analysis of eigenvectors showed that the greatest effect on the first main component (PC 1) had anthocyanins, flavones, flavonols, flavan-3-ol, dihydroflavonols, hydroxybenzoic acids, hydroxycinnamic acids, hydroxyphenylpropanoic acids, stilbenes, hydroxybenzaldehydes, tyrosols from the phenolic group, and other aromas as a representative of compounds from the aromatic group. Terpenes, esters, and alcohols from the aromatic group and flavones and dihydroflavonols from the phenolic group had the greatest effect on the second main component (PC 2), while hydroxyphenylpropanoic acids and stilbenes showed the greatest effect on the third main component (PC 3).

Figure 3 shows the results for the first two principal components, which together explain 76.63% of the total variability (PC1 53.04%, PC2 23.59%).

The first principal component (PC 1) showed the separation of two groups: group 1 (elderflower) and group 2 (rosemary, thyme, and control). Group 1 is located at the negative end of PC 1 and is characterized by a higher content of anthocyanins; flavonols; flavan-3-ol; hydroxybenzoic acids; hydroxycinnamic acids; and miscellaneous aromatic components: anisole, benzaldehyde, and benzeneacetaldehyde. Within group 2, the separation by the second principal component (PC 2) is noticeable. The rosemary and thyme treatments were grouped on the positive sides of PC 1 and PC2 and were characterized by a higher content of alcohol and terpenes within the aromatic components, as well as flavones and dihydroflavonols. The control treatment is located on the positive side of PC 1 and the negative side of PC 2 and is defined by a higher content of esters.

3.5. Sensory Analysis

The radar chart (Figure 4) shows the sensory profile of vinegars. There is a significant difference in seven of the nine observed properties (p ˂ 0.05). Comparing individual treatments, it is evident that the control treatment is inferior in all positive properties. In the case of flavored vinegars, each plant species gave the vinegar a specific and recognizable scent characteristic: elderflower floral and fruity, rosemary herbal and pinewood, and thyme spicy sensation. Furthermore, all flavored vinegars had higher values for the general impression with a reduced pungent sensation.

4. Discussion

The global market for specialty vinegars, which include balsamic, sherry, and red wine vinegar, is growing significantly [29]. Flavoring white wine vinegar (WWV) with aromatic plants can raise its market value and increase consumption.

In comparison to red wine vinegar, WWV has lower polyphenolic content [30], and an increase in the polyphenolic content could be obtained by adding aromatic plants. In this study, we found that flavored WWVs had a higher polyphenolic content than the unflavored WWV.

Numerous studies have detected polyphenols as bioactive compounds that have a beneficial effect on human health. Kumar and Pandey [31] suggest that, among polyphenols, flavonoids have antioxidative, anti-inflammatory, and anticancer activities. In our study, WWVs flavored with rosemary and thyme had higher concentrations of flavones, while elderflower-flavored WWVs had a higher concentration of flavonols.

Except polyphenols, other compounds, like p-cymene, have pharmacological properties [32], and this aromatic compound was significantly higher in the WWVs flavored with thyme than in unflavored WWV.

Our results showed that each of the investigated plant species used for aromatization in this research contributed to the specific vinegar odor, aromatic, and polyphenolic profiles.

The major aromatic groups in the WWV were esters, and ethyl hexanoate was the main volatile compound in the unflavored WWV. In the flavored WWVs, terpenes were compounds that mainly contributed to the volatile profile and showed significant differences in content between the treatments.

The most abundant terpenes in the WWVs flavored with rosemary were camphor, endo-borneol, and eucalyptol, such as those found by Cejudo-Bastante et al. [6] in the research of commercial aromatized vinegars. Of the sixteen analyzed terpenes, the values of ten of them (camphor, α-terpineol, endo-borneol, fenchol, isoterpinolene, γ-terpinen, eucalyptol, terpinen-4-ol, 2-carene, and D-carvone) were highest in the WWVs aromatized with rosemary. Camphor, α-terpineol, and eucalyptol in the rosemary extracts were found by Mena et al. [21] and Lakušić et al. [33], but the different composition of the volatile compounds compared to our results may be related to the rosemary chemotype [21] and growing conditions [34].

The main terpenes in the WWVs flavored with thyme were p-thymol and p-cymene, and the same volatiles were also found by Satyal et al. [35] in French chemotypes of thyme, while Dauqan and Abdullah [36] found β-myrcene and thymol to be the main volatile compounds in the thyme essential oil.

WWVs flavored with elderflower had the significantly highest values of the terpenes hotrienol, linalool oxide, and β-ocimene, and other volatile compounds like anisole and benzeneacetaldehyde. Jørgensen et al. [37] detected hotrienol as a terpene that contributes to the characteristic elderflower odor, while linalool and β-ocimene contribute floral notes to the vinegar. The floral and fruity notes were the most expressed in the WWVs flavored with elderflower in this research. Kaack et al. [24] detected the highest hotrienol and linalool concentrations in the elderflower, which is in accordance with the results for these volatile compounds in the WWVs flavored with elderflowers in our study.

Each plant species gave its own specific sensory characteristics to the flavored WWVs. Herbal and pine notes were noticeable in rosemary. Volatiles α-terpineol and endo-borneol contribute to the pine notes, camphor camphoruous, and eucalyptol herbal and eucalyptus notes [21]. The main volatile in thyme was p-thymol, which is a carrier of the spicy and herbal notes, while hotrienol and anisol were responsible for the floral and fruity notes in elderflower.

In all aromatized WWVs, there was a notable reduction in pungent smell intensity. This decrease is likely due to the enhanced aromatic profile of the flavored WWVs, resulting in a more favorable overall impression compared to the control vinegar.

The group of polyphenolic compounds, anthocyanins, were present only in the elderflower WWVs, and were not detected in rosemary, thyme, or unflavored WWVs. Among anthocyanins, malvidin was the compound with the highest concentration.

The most abundant group of phenolic compounds in the WWVs flavored with elderflower were flavonols, while flavones were found in significantly higher concentrations in WWVs flavored with rosemary (apigenin-4-O-glucoside and apigenin-7-O-glucoside) and thyme (luteolin-7-O-glucoside).

The highest polyphenolic compound concentrations (7 of 19 detected flavonols) were detected in the elderflower compared to other flavored WWVs, probably because of the higher dose of the added plant material (20 g/L) compared to the other WWVs (4 g/L).

Among flavonoles, quercetin and chlorogenic acid were most abundant in elderflower-flavored WWV, among flavonoles and hydroxycinnamic acids, respectively. Previous investigations of the elderflower phenolic profile demonstrated caffeoylquinic acid (chlorogenic acid) and quercetin-3-rutinoside (rutin) [26,38] as the main phenolic compounds. In our research, chlorogenic acid and quercetin were the main phenolics in the WWVs flavored with elderflower. Chlorogenic acid was not detected in the unflavored WWV, and this phenolic compound is related to the plant material used for the WWV flavoring.

Total flavonols, followed by total hydroxycinnamic acids, were the groups of phenolic compounds with the highest concentration in elderflower methanol extracts and sabesa (a beverage made of water with added sucrose and citric and acetic acid) in Mikulič Petkovšek et al. [26], as well as in our research.

The variations in aromatic and phenolic compound concentrations between our and other studies could be attributed to differences in the growing [34,35,39] or drying conditions [23], extraction or maceration solvent [26], detection method, and variations in the chemotypes [21] of aromatic plants.

As the PCA has shown, the main contribution of elderflower to WWV was the substantial increase in all polyphenolic groups, except for flavones, which is consistent with the increased dosage used in its preparation as well as the polyphenolic profile of elderflower as shown by Mikulic-Petkovsek et al. [40]. Besides the increase in polyphenolic compounds, the sensory analysis has shown a distinct floral aroma of the elderflower-infused WWV compared to the other investigated WWVs, which is a direct effect of aroma compounds present in elderflower [41]. Similarly, the PCA showed that thyme and rosemary maceration contributed to the elevated terpenes, esters, and alcohols, as well as flavones and dihydroflavonols in WWV, but with distinct volatile and sensory profiles, characteristic for each plant species.

In our investigation, thyme-infused WWV exhibited spicy and herbaceous notes characteristic of the herb and described by Stahl-Biskup and Venskutonis [42]. On the other hand, rosemary-infused WWV is characterized by pinewood and herbal notes, which is in line with the work of Diaz-Maeroto et al. [43]. Consistent with the smaller dosage of thyme and rosemary compared to elderflower, the polyphenolic enrichment of the herb-infused WWV is evident compared to the control WWV, albeit in lower abundance if compared to the elderflower macerated WWV in our study. Both thyme and rosemary macerated WWVs were shown to be rich in flavones, more precisely in luteolin, apigenin, baicalein, and their glycosides. This is in line with the investigation by Mena et al. [21] on rosemary and Slimestad et al. [44] on both rosemary and thyme polyphenolic profiles.

To the best of our knowledge, this is the first research that uses dried herbal parts of black elder, rosemary, and thyme as a material for maceration in white wine vinegar and analyzes the volatile and polyphenolic compounds, as well as the sensory profile of the obtained flavored vinegars.

5. Conclusions

This study showed significant differences in volatile and phenolic compounds as well as sensory profiles between flavored WWVs and unflavored WWV.

Plants used to flavor WWV improve its aromatic and sensory profile, as well as the nutraceutical value, as the polyphenolic compounds increase. The sensory characteristics specific to the plant species used for flavoring were noticeable in the respective flavored WWV. Terpenes are the main source of aromatic compounds in flavored WWVs, and the concentrations of individual compounds vary depending on the plant species. Hotrienol and anisole were volatiles mostly present in WWV flavored with elderflowers, while α-terpineol, camphor, and endo-borneol were the main terpenes in the rosemary-flavored WWV. In the WWV flavored with thyme, p-thymol and p-cymene were the most present terpenes. Polyphenolic compound content was higher in the flavored WWVs, especially in elderflower, due to the higher dosage used. Flavonols were the main phenols in the WWV flavored with the elderflower, while flavones were mostly present in the WWVs flavored with rosemary and thyme. Chlorogenic acid was not detected in the unflavored WWV, and its presence in the flavored WWVs is directly related to the plant material used for aromatization. Flavored WWVs exhibit a more intense and complex aroma and flavor, leading to a superior overall sensory score compared to the control WWV.

Because of the relatively small quantities of aromatic plants added to the WWV, this research could contribute to the implementation of this practice in vinegar production and its economic reasonability. Newly developed products contribute to the diversity of culinary offerings and have the potential to drive up the demand for flavored white wine vinegar.

Supplementary Materials

The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/app14166909/s1, Table S1. Analysis parameters of polyphenolic compounds.

Author Contributions

Conceptualization, M.K. and T.P.; methodology, M.K., T.P., N.M. and A.J.; validation, N.M.; formal analysis, N.M., T.P. and I.T.; investigation, M.K. and T.P.; resources, M.K. and T.P.; data curation, T.P.; writing—original draft preparation, M.K. and T.P.; writing—review and editing, A.J. and D.P.; visualization, D.P.; project administration, M.K.; funding acquisition, M.K. All authors have read and agreed to the published version of the manuscript.

Funding

The project ‘Enrichment of white wine vinegar from the Istrian Malvasia variety with wild herbs’ was funded by the Region of Istria (grant No. U-0147-2022-89).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The data generated during the current study are available from the corresponding authors upon reasonable request.

Acknowledgments

The authors would like to thank Slavica Dudaš for the plant material used for the experiments and Kristina Grozić for help in creating the graphical abstract.

Conflicts of Interest

The authors declare no conflict of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript; or in the decision to publish the results.

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Figure 1. Scheme of vinegar production and analysis.

Figure 2. Differences in the odorant series (herbal, floral, fruity, sweet, spicy, camphor-like, and unpleasant) of the flavored vinegars (shown as a bar graph) compared to the control treatment (shown on the x-axis) expressed as percentage changes. The odor series is represented by the sum of mean values of all compounds of the same odorant series where a significant difference between treatments was determined.

Figure 3. Principal component analysis (PCA) for vinegars: (a) treatments (cases); (b) aromatic groups—blue letters; phenolic groups—green letters (variables). Abbreviations: Alc—alcohols, Acd—acids, Est—esters, Ter—terpenes, Otha—miscellaneous aromas, Ant—anthocyanins, Fla—flavones, FlaOL—flavonols, Fla-3-ol—flavan-3-ol, Dhf—dihydroflavonols, HbA—hydroxybenzoic acids, HcA—hydroxycinnamic acids, HppA—hydroxyphenylpropanoic acids, Stil—stilbenes, Hba—hydroxybenzaldehydes, Ty—tyrosols.

Figure 4. Comparison of the odor properties of flavored vinegars (elderflower, rosemary, and thyme) and the control treatment. An analysis of variance (ANOVA) was performed to determine if there was a significant difference among the odor properties of the vinegars. Odor properties marked with asterisks (**, p ≤ 0.01; ***, p ≤ 0.001) show significant differences.

Table 1. Aromatic profiles of vinegars.

Compounds (mg/L)	Treatments (Mean ± SD)				O.s. ^†	Sig.
Compounds (mg/L)	Control	Elderflower	Rosemary	Thyme	O.s. ^†	Sig.
Alcohols
1-Nonanol	0.99 ± 0.10	1.10 ± 0.16	0.95 ± 0.13	0.72 ± 0.24	2	n.s.
2,3-Butanediol	1.29 ± 1.12	1.84 ± 0.16	1.51 ± 0.64	0.98 ± 0.87	3	n.s.
2-Phenylethanol	0.76 ± 0.63	1.05 ± 0.01	0.95 ± 0.05	0.97 ± 0.05	2	n.s.
Amyl vinyl carbinol	0.03 ± 0.00 ^b	0.06 ± 0.00 ^b	1.95 ± 0.17 ^a	1.68 ± 0.25 ^a	7	***
Isoamyl alcohol	0.97 ± 0.11	1.05 ± 0.06	0.92 ± 0.04	0.91 ± 0.06	7	n.s.
Ʃ alcohols	4.04	5.10	6.28	5.26		n.s.
Acids
Isovaleric acid	0.74 ± 0.53	1.04 ± 0.08	0.88 ± 0.13	0.63 ± 0.31	7	n.s.
2-Methylbutanoic acid	0.37 ± 0.48	1.16 ± 0.18	0.91 ± 0.138	0.93 ± 0.33	7	n.s.
Ʃ acids	1.11	2.20	1.79	1.56		n.s.
Esters
2-Phenylethyl acetate	1.13 ± 0.13 ^a	0.89 ± 0.01 ^b	0.91 ± 0.04 ^b	1.08 ± 0.03 ^a	2	***
3-(Methylthio)propyl acetate	1.14 ± 0.19	0.96 ± 0.10	0.99 ± 0.09	0.86 ± 0.11	1	n.s.
Butyl acetate	1.17 ± 0.24	0.96 ± 0.08	0.96 ± 0.04	0.96 ± 0.05	3	n.s.
Diethyl succinate	0.98 ± 0.09	1.14 ± 0.03	0.89 ± 0.06	0.74 ± 0.46	3	n.s.
Ethyl heptanoate	1.09 ± 0.17	1.17 ± 0.15	0.93 ± 0.10	0.94 ± 0.07	1, 3	n.s.
Ethyl hexanoate	2.14 ± 0.32 ^a	0.75 ± 0.05 ^bc	0.96 ± 0.12 ^b	0.44 ± 0.05 ^c	3	***
Isoamyl acetate	1.22 ± 0.17	0.99 ± 0.00	0.96 ± 0.04	1.07 ± 0.13	3	n.s.
Ʃ esters	8.87 ^a	6.86 ^b	6.60 ^b	6.09 ^b		**
Terpenes
γ-Terpinen	0.037 ± 0.10 ^c	0.09 ± 0.01 ^c	2.11 ± 0.17 ^a	1.71 ± 0.11 ^b	3	***
2-Carene	0.04 ± 0.01 ^c	0.10 ± 0.01 ^c	1.95 ± 0.10 ^a	1.52 ± 0.11 ^b	3	***
Camphor	n.d.	n.d.	2.57 ± 0.11 ^a	0.06 ± 0.00 ^b	6	***
D-Carvone	n.d.	0.01 ± 0.00 ^c	1.53 ± 0.08 ^a	0.56 ± 0.03 ^b	1,5	***
Eucalyptol	0.02 ± 0.00 ^b	0.03 ± 0.00 ^b	2.10 ± 0.09 ^a	0.06 ± 0.00 ^b	1,6	***
Fenchol	0.58 ± 0.14 ^b	0.46 ± 0.02 ^b	2.29 ± 0.16 ^a	0.42 ± 0.03 ^b	3,6	***
Isoterpinolene	0.13 ± 0.04 ^d	0.50 ± 0.03 ^c	2.24 ± 0.21 ^a	0.80 ± 0.03 ^b	1	***
Linalool	0.10 ± 0.01 ^c	1.34 ± 0.06 ^a	1.27 ± 0.14 ^ab	1.05 ± 0.18 ^b	2,3,4	***
p-Cymene	0.03 ± 0.00 ^c	0.03 ± 0.00 ^c	1.06 ± 0.06 ^b	2.74 ± 0.07 ^a	1,3	***
Terpinen-4-ol	0.01 ± 0.00 ^c	0.02 ± 0.00 ^c	2.08 ± 0.18 ^a	1.35 ± 0.16 ^b	1,2,5	***
α-Terpineol	0.17 ± 0.02 ^b	0.29 ± 0.01 ^b	2.57 ± 0.19 ^a	0.32 ± 0.04 ^b	2,4	***
endo-Borneol	0.01 ± 0.00 ^c	0.02 ± 0.00 ^c	2.51 ± 0.15 ^a	0.68 ± 0.04 ^b	6	***
Linalool oxide	0.38 ± 0.09 ^b	2.58 ± 0.23 ^a	0.63 ± 0.14 ^b	0.55 ± 0.13 ^b	2	***
p-Thymol	n.d.	0.23 ± 0.01 ^b	0.20 ± 0.03 ^b	5.82 ± 0.16 ^a	5	***
β-Ocimene	0.13 ± 0.02 ^c	1.46 ± 0.04 ^a	1.14 ± 0.17 ^b	1.08 ± 0.08 ^c	1,4	***
Hotrienol	0.05 ± 0.00 ^b	4.05 ± 0.26 ^a	0.08 ± 0.02 ^b	0.10 ± 0.02 ^b	1,2,3	***
Ʃ terpenes	1.68 ^d	11.21 ^c	26.34 ^a	18.82 ^b		***
Other
Acetoin Acetate	0.85 ± 0.50	1.03 ± 0.01	0.90 ± 0.10	0.94 ± 0.13	3	n.s.
Anisole	0.01 ± 0.01 ^b	4.34 ± 0.10 ^a	0.02 ± 0.00 ^b	0.01 ± 0.01 ^b	5	***
Benzaldehyde	1.11 ± 0.16 ^a	1.17 ± 0.01 ^a	0.93 ± 0.07 ^b	0.93 ± 0.03 ^b	3	**
Benzeneacetaldehyde	0.94 ± 0.27 ^b	1.72 ± 0.05 ^a	0.72 ± 0.02 ^b	0.71 ± 0.05 ^b	1	***
Ʃ others	2.92 ^b	8.26 ^a	2.57 ^b	2.58 ^b		***

† Odorant series: 1—herbaceous; 2—floral; 3—fruity; 4—sweet; 5—spicy; 6—camphor-like; 7—unpleasant. Means ± SD with different superscript letters (a, b, c, d) for each compound in the same row differ significantly (p ≤ 0.05); n.s. non-significant; **. p ≤ 0.01; ***. p ≤ 0.001; n.d. not detected.

Table 2. Polyphenolic profile of vinegars.

Compounds (mg/L)	Treatments (Mean ± SD)				Sig.
Compounds (mg/L)	Control	Elderflower	Rosemary	Thyme	Sig.
Anthocyanins
Cyanidin-3-O-glucoside	n.d.	0.05 ± 0.00	n.d.	n.d.
Malvidin-3-O-glucoside	n.d.	14.32 ± 3.90	n.d.	n.d.
Petunidin-3-O-glucoside	n.d.	0.15 ± 0.00	n.d.	n.d.
Ʃ anthocyanins	n.d.	14.52	n.d.	n.d.
Flavones
Apigenin	n.d.	n.d.	0.28 ± 0.01 ^b	1.00 ± 0.02 ^a	***
Apigenin-4-O-glucoside	0.03 ± 0.04 ^c	0.20 ± 0.03 ^c	16.45 ± 0.82 ^a	2.11 ± 0.32 ^b	***
Apigenin-7-O-glucoside	n.d.	0.02 ± 0.01 ^c	2.55 ± 0.14 ^a	0.32 ± 0.04 ^b	***
Baicalein	0.39 ± 0.04 ^c	0.33 ± 0.08 ^bc	0.58 ± 0.09 ^a	0.47 ± 0.03 ^ab	***
Baicalein-7-O-glucuronide	2.16 ± 1.61	2.12 ± 0.51	3.98 ± 1.28	4.25 ± 1.27	n.s.
Luteolin	0.15 ± 0.02 ^c	0.13 ± 0.00 ^c	1.76 ± 0.01 ^b	3.02 ± 0.03 ^a	***
Luteolin-4-O-glucoside	n.d.	n.d.	0.01 ± 0.00 ^a	n.d.
Luteolin-7-O-glucoside	0.03 ± 0.02 ^c	n.d.	1.81 ± 0.07 ^b	16.95 ± 0.28 ^a	***
Luteolin-7-O-rutinoside	n.d.	0.03 ± 0.00 ^b	5.55 ± 0.70 ^a	5.31 ± 0.59 ^a	***
Ʃ flavones	2.76 ^b	2.84 ^b	32.98 ^a	33.42 ^a	***
Flavonols
Isorhamnetin	0.01 ± 0.00 ^b	16.57 ± 0.45 ^a	0.07 ± 0.04 ^b	0.01 ± 0.01 ^b	***
Isorhamnetin-3,4′-O-diglucoside	n.d.	1.96 ± 0.05 ^a	0.02 ± 0.01 ^b	n.d.	***
Isorhamnetin-3-O-glucoside	n.d.	54.11 ± 0.78 ^a	0.02 ± 0.01 ^b	n.d.	***
Isorhamnetin-3-O-rutinoside	n.d.	0.55 ± 0.10	n.d.	n.d.
Isorhamnetin-4′-O-glucoside	n.d.	98.61 ± 0.89 ^a	0.06 ± 0.02 ^b	0.01 ± 0.01 ^b	***
Kaempferol	0.28 ± 0.06 ^b	4.94 ± 0.53 ^a	n.d.	n.d.	***
Kaempferol-3-O-glucoside	0.174 ^b	8.16 ± 0.66 ^a	0.05 ± 0.03 ^b	0.11 ± 0.07 ^b	***
Kaempferol-3-O-glucuronide	n.d.	n.d.	0.12 ± 0.03 ^a	0.04 ± 0.02 ^b	***
Kaempferol-7-O-glucoside	n.d.	0.49 ± 0.66	n.d.	n.d.
Kaempferol-7-O-neohesperidine	n.d.	0.09 ± 0.10	n.d.	n.d.	n.s.
Quercetin	0.15 ± 0.08 ^b	148.62 ± 11.85 ^a	0.84 ± 0.34 ^b	0.27 ± 0.12 ^b	***
Quercetin-3,4′-O-diglucoside	0.04 ± 0.00 ^b	0.11 ± 0.01 ^a	0.04 ± 0.00 ^b	0.04 ± 0.00 ^b	***
Quercetin-3,7-O-diglucoside	n.d.	1.03 ± 0.04 ^a	n.d.	n.d.
Quercetin-3-O-glucoside	n.d.	26.94 ± 0.52 ^a	0.11 ± 0.02 ^b	n.d.	***
Quercetin-3-O-glucuronide	0.05 ± 0.00 ^d	0.07 ± 0.00 ^c	0.11 ± 0.01^a	0.09 ± 0.01 ^b	***
Quercetin-3-O-rhamnoside	0.04 ± 0.00 ^a	0.02 ± 0.00 ^b	0.04 ± 0.00 ^a	0.04 ± 0.00 ^a	***
Quercetin-3-O-rutinoside	n.d.	0.06 ± 0.01 ^a	0.03 ± 0.00 ^b	n.d.	***
Quercetin-4′-O-glucoside	0.01 ± 0.00 ^b	0.04 ± 0.01 ^a	0.01 ± 0.00 ^b	0.01 ± 0.00 ^b	***
Quercetin-7-O-glucoside	0.03 ± 0.01 ^d	5.35 ± 0.36 ^b	3.460 ± 0.26 ^c	31.68 ± 0.80 ^a	***
Ʃ flavonols	0.77 ^c	367.74 ^a	4.97 ^c	32.30 ^b	***
Flavan-3-ol
Catechin	0.04 ± 0.00 ^b	0.05 ± 0.00 ^a	0.03 ± 0.00 ^b	0.03 ± 0.00 ^b	***
Dihydroflavonols
Dihydroquercetin	0.14 ^b	0.11 ^c	0.13 ^bc	0.70 ^a	***
Hydroxybenzoic acids
Gallic acid	2.24 ± 0.06 ^b	3.64 ± 0.03 ^a	2.22 ± 0.02 ^b	2.21 ± 0.04 ^b	***
Gentisic acid	0.12 ± 0.01 ^c	0.26 ± 0.04 ^a	0.14 ± 0.03 ^bc	0.16 ± 0.01 ^b	***
p-hydroxybenzoic acid	2.47 ± 0.08 ^c	17.22 ± 0.09 ^a	2.79 ± 0.04 ^b	2.53 ± 0.08 ^c	***
Protocatehuic acid	0.77 ± 0.03 ^b	22.83 ± 0.08 ^a	0.77 ± 0.01 ^b	0.83 ± 0.07 ^b	***
Syringic acid	0.25 ± 0.02 ^b	0.27 ± 0.02 ^b	0.26 ± 0.01 ^b	0.50 ± 0.04 ^a	***
Vanillic acid	0.20 ± 0.00 ^d	2.37 ± 0.05 ^a	0.58 ± 0.03 ^b	0.28 ± 0.01 ^c	***
Ʃ hydroxybenzoic acids	6.04 ^d	46.58 ^a	6.76 ^b	6.52 ^c	***
Hydroxycinnamic acids
Caffeic acid	2.46 ± 0.07 ^d	25.22 ± 0.41 ^a	11.13 ± 0.16 ^c	13.79 ± 0.13 ^b	***
Chlorogenic acid	n.d.	219.10 ± 3.90 ^a	0.36 ± 0.04 ^b	0.26 ± 0.03 ^b	***
Ferulic acid	0.47 ± 0.01 ^d	1.13 ± 0.03 ^a	0.52 ± 0.02 ^c	0.60 ± 0.001 ^b	***
Isoferulic acid	0.18 ± 0.01	0.25 ± 0.03	0.19 ± 0.04	0.20 ± 0.02	n.s.
Neochlorogenic acid	0.17 ± 0.00 ^c	24.40 ± 0.28 ^a	0.50 ± 0.01 ^b	0.18 ± 0.00 ^c	***
p-Coumaric acid	0.35 ± 0.07 ^d	1.02 ± 0.04 ^a	0.79 ± 0.03 ^b	0.64 ± 0.03 ^c	***
Sinapic acid	0.04 ± 0.00 ^c	0.12 ± 0.00 ^a	0.06 ± 0.01 ^b	0.05 ± 0.00 ^c	***
Verbascoside	0.01 ± 0.01 ^b	0.02 ± 0.01 ^b	0.08 ± 0.04 ^a	0.02 ± 0.01 ^b	**
Ʃ hydroxycinnamic acids	3.69 ± 0.12 ^c	271.258 ± 4.13 ^a	13.63 ± 0.22 ^b	15.74 ± 0.11 ^b	***
Hydroxyphenylpropanoic acids
Dihydro-p-coumaric acid	0.39 ± 0.15	0.40 ± 0.08	0.45 ± 0.20	0.39 ± 0.16	n.s.
Other
Polydatin	0.04 ± 0.02	0.02 ± 0.01	0.03 ± 0.01	0.03 ± 0.00	n.s.
Vanillin	0.04 ± 0.01 ^c	0.16 ± 0.02 ^a	0.08 ± 0.01 ^b	0.08 ± 0.00 ^b	***
Hydroxytyrosol	0.15 ± 0.00 ^c	0.23 ± 0.00 ^a	0.18 ± 0.01 ^b	0.19 ± 0.00 ^b	***
Ʃ other	0.23 ^c	0.40 ^a	0.29 ^b	0.30 ^b	***

Means ± SD with different superscript letters (a, b, c, d) for each compound in the same row differ significantly (p ≤ 0.05); n.s. non-significant; **. p ≤ 0.01; ***. p ≤ 0.001; n.d. not detected.

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Krapac, M.; Major, N.; Plavša, T.; Jeromel, A.; Tomaz, I.; Poljuha, D. Enrichment of White Wine Vinegar with Aromatic Plants: The Impact on Aromatic, Polyphenolic, and Sensory Profiles. Appl. Sci. 2024, 14, 6909. https://doi.org/10.3390/app14166909

AMA Style

Krapac M, Major N, Plavša T, Jeromel A, Tomaz I, Poljuha D. Enrichment of White Wine Vinegar with Aromatic Plants: The Impact on Aromatic, Polyphenolic, and Sensory Profiles. Applied Sciences. 2024; 14(16):6909. https://doi.org/10.3390/app14166909

Chicago/Turabian Style

Krapac, Marin, Nikola Major, Tomislav Plavša, Ana Jeromel, Ivana Tomaz, and Danijela Poljuha. 2024. "Enrichment of White Wine Vinegar with Aromatic Plants: The Impact on Aromatic, Polyphenolic, and Sensory Profiles" Applied Sciences 14, no. 16: 6909. https://doi.org/10.3390/app14166909

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Enrichment of White Wine Vinegar with Aromatic Plants: The Impact on Aromatic, Polyphenolic, and Sensory Profiles

Abstract

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Abstract

1. Introduction

2. Materials and Methods

2.1. Wine and Non-Flavored Vinegar Production

2.2. Herbs and Vinegar Flavoring Procedure

2.3. Volatile Compounds Analysis

2.4. Targeted Analysis of Polyphenolic Compounds

2.5. Sensory Analysis

2.6. Statistical Analysis

3. Results

3.1. Aromatic Profile

3.2. Odorant Series

3.3. Polyphenolic Profile

3.4. Principal Component Analysis (PCA)

3.5. Sensory Analysis

4. Discussion

5. Conclusions

Supplementary Materials

Author Contributions

Funding

Institutional Review Board Statement

Informed Consent Statement

Data Availability Statement

Acknowledgments

Conflicts of Interest

References

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