Characterization of aroma compounds in apple cider using solvent-assisted flavor evaporation and headspace solid-phase microextraction

The aroma-active compounds in two apple ciders were identified using gas chromatography-olfactometry (GC-O) and GC-mass spectrometry (MS) techniques. The volatile compounds were extracted using solvent-assisted flavor evaporation (SAFE) and headspace solid-phase microextraction (HS-SPME). On the basis of odor intensity, the most important aroma compounds in the two apple cider samples were 2-phenylethanol, butanoic acid, octanoic acid, 2-methylbutanoic acid, 2-phenylethyl acetate, ethyl 2-methylbutanoate, ethyl butanoate, ethyl hexanoate, 4-ethylguaiacol, eugenol, and 4-vinylphenol. Sulfur-containing compounds, terpene derivatives, and lactones were also detected in ciders. Although most of the aroma compounds were common in both ciders, the aroma intensities were different. Comparison of extraction techniques showed that the SAFE technique had a higher recovery for acids and hydroxy-containing compounds, whereas the HS-SPME technique had a higher recovery for esters and highly volatile compounds.     

Effect of emulsion characteristics on the release of aroma as detected by sensory evaluation,static headspace gas chromatography,and electronic nose

The effects of emulsion structure and composition of the matrix on the release of linalool (nonpolar) and diacetyl (polar) were studied using sensory evaluation, static headspace gas chromatography, and an electronic nose. The matrices used were water, rapeseed oil, and eight oil-in-water emulsions differing in oil volume fraction (0.05/0.5), emulsifier type (sucrose stearate/modified potato starch), and homogenization pressure (100/300 bar). Fat content strongly affected the release of linalool, but it was not as critical a factor in the release of the more polar compound, diacetyl. A slight effect of the emulsifier type on the release of aromas was observed with sensory and gas chromatographic methods. The reduced droplet size, resulting from higher homogenization pressure, enhanced the release of linalool but had no effect on diacetyl. Sensory and gas chromatographic methods detected aroma changes quite similarly. The electronic nose was capable of detecting only the effect of fat on linalool.     

Comparison of nosespace,headspace, and sensory intensity ratings for the evaluation of flavor absorption by fat

The goal of this study was to better understand the correspondence between sensory perception and in-nose compound concentration. Five aroma compounds at three different concentrations increasing by factors of 4 were added to four matrixes (water, skim milk, 2.7% fat milk, and 3.8% fat milk). These were evaluated by nosespace analysis with detection by proton transfer reaction mass spectrometry (PTR-MS), using five panelists. These same panelists evaluated the perceived intensity of each compound in the matrixes at the three concentrations. PTR-MS quantification found that the percent released from an aqueous solution swallowed immediately was between 0.1 and 0.6%, depending on the compound. The nosespace and sensory results showed the expected effect of fat on release, where lipophilic compounds showed reductions in release as fat content increases. The effect is less than that observed in headspace studies. A general correlation between nosespace concentration and sensory intensity ratings was found. However, examples of perceptual masking were found where higher fat milks showed reductions in aroma compound intensity ratings, even if the nosespace concentrations were the same.     

Chemical and sensorial characteristics of espresso coffee as affected by grinding and torrefacto roast

Grinding is a critical step in the preparation of espresso coffee (EC). The addition of sugar during the torrefacto roasting process could influence the degree of brittleness and grinding. The aim of this work was to study the influence of the grinding grades (coarse, fine, and very fine) in Arabica/Robusta 20:80, natural roasted (A20:R80), and Arabica/Robusta 20:80 with 50% Robusta torrefacto roasted (A20:R80 50% torrefacto) on the chemical and sensorial characteristics of EC in order to select the optimal espresso grinding grade. A higher percentage of coarse particles was found in A20:R80 ground coffee. In both ECs, the extraction of solids and soluble and aroma compounds increased inversely with particle size. Higher foam indices and extraction yields were found in A20:R80 50% torrefacto ECs probably due to the solubilization of caramelized sugar and melanoidins. It has been suggested that the range of an acceptable extraction yield could be extended to 25% in A20:R80 50% torrefacto ECs. In conclusion, the optimal grinding grade for the obtainment of an EC with A20:R80 was fine and that for A20:R80 50% torrefacto was coarse.     

Characterization of aroma compounds responsible for the rosy/floral flavor in Cheddar cheese

The aroma-active compounds that contribute to the rosy/floral flavor in Cheddar cheese were characterized using both instrumental and sensory techniques. Two cheeses (>12 months old) with rosy/floral flavor and two Cheddar cheeses of similar ages without rosy/floral flavors were selected. After direct solvent extraction/solvent-assisted flavor evaporation and separation into neutral/basic and acidic fractions, samples were analyzed by gas chromatography-olfactometry with aroma extract dilution analysis. Selected compounds were quantified using internal standard methodology. Some of the intense aroma-active compounds in the neutral basic fraction of the rosy/floral cheeses included 2-phenethanol (rosy), phenylethyl acetate (rosy), and phenylacetaldehyde (rosy/floral). Quantification, threshold analysis, and sensory analysis of model cheeses confirmed that increased concentrations of phenylacetaldehyde and phenylacetic acid caused rosy/floral flavor when spiked into Cheddar cheese.     

Aloe exudate: characterization by reversed phase HPLC and headspace GC-MS

From the leaves of aloe, a succulent plant, a dried exudate commonly called aloe can be obtained, which is used as a natural drug for its cathartic effect and is widely employed as a bittering agent in alcoholic beverages. This investigation provides a tentative characterization of several commercial aloe exudates carried out both by reversed phase HPLC and by headspace GC-MS analysis. By means of HPLC the derivatives were evaluated, and by GC-MS the volatile fraction was investigated. Qualitative and quantitative differences among the constituents in various samples of different origins were found. In particular, these were evident in the HPLC profile of Kenya aloe and an Aloe barbadensis sample, which exuded a high content of isoaloeresin D and aloins, whereas GC-MS analysis showed the presence of anisole exclusively in Kenya aloe samples. Moreover, the results obtained by means of the latter technique suggested a reason for the prevailing use of Mosselbay and Port Elizabeth aloes in bitter spirits formulation.     

Characterization of the key aroma compounds in rape honey by means of the molecular sensory science concept

By application of aroma extract dilution analysis (AEDA) on the volatile fraction isolated by solvent extraction and solvent-assisted flavor evaporation (SAFE) from unifloral rape honey harvested in July 2009, 28 odor-active areas could be detected within a flavor dilution factor (FD) range of 4-2048. The highest FD factors were found for (E)-β-damascenone (cooked apple-like), phenylacetic acid (honey-like), 4-methoxybenzaldehyde (aniseed-like), 3-phenylpropanoic acid (flowery, waxy), and 2-methoxy-4-vinylphenol (clove-like). Twenty-three odorants were then quantitated by application of stable isotope dilution assays, and their odor activity values (OAV, ratio of concentration to odor threshold) were calculated on the basis of newly determined odor thresholds in an aqueous fructose-glucose solution. The highest OAVs were calculated for (E)-β-damascenone, 3-phenylpropanoic acid, phenylacetic acid, dimethyl trisulfide, and phenylacetaldehyde. Quantitative measurements on a rape honey produced in 2011 confirmed the results. A model mixture containing the 12 odorants showing an OAV ≥ 1 at the same concentrations as they occurred in the rape honey was able to mimick the aroma impression of the original honey. The characterization of the key odorants in rape flowers from the same field suggested 3-phenylpropanoic acid, phenylacetic acid, and three further odorants to be transferred via the bees into the honey.     

Changes in volatile compounds and overall aroma profile during storage of coffee brews at 4 and 25 degrees C

In this work, the chemical changes occurring in the volatile fraction of Arabica coffee brews during storage at 4 and 25 degrees C for 30 days have been characterized for the first time by means of HS-GC-MS. A total of 47 compounds were identified and quantified: 2 sulfur compounds, 7 aldehydes, 3 esters, 15 furans, 5 ketones, 1 alcohol, 2 thiophenes, 4 pyrroles, 1 pyridine, 5 pyrazines, 1 alkene, and 1 acid. No new volatile compounds were detected at the end of the storage time. The changes observed are, in general, slower and less pronounced at refrigeration temperature. Storage also affects the sensory characteristics of the stored coffee brews, which lose part of their aroma intensity and freshness, acquiring some nondesirable notes such as rancid aroma, mainly during storage at 25 degrees C. Furthermore, seven aroma indices have been proposed as indicators of coffee brew staling, which show a good correlation with some sensory attributes, not only for aroma but also overall sensory quality. Consequently, they could be considered useful to monitor both the "age" and the sensory quality of stored coffee brews.     

Volatile compounds of selected strawberry varieties analyzed by purge-and-trap headspace GC-MS

Six strawberry (Fragaria x ananassa Duch.) varieties, Senga Sengana, Jonsok, Polka, Korona, Bounty, and Honeoye, were studied in relation to composition of their volatile headspace compounds collected by dynamic purge-and-trap concentration. Also, the influence of cultivation technique on the volatile compounds was tested by comparing conventionally and organically cultivated strawberry varieties. In addition, the effect of geographical origin on strawberry volatiles was investigated. The emphasis of this study was lay in the industrial utilization of strawberry. A total of 52 different volatile compounds were determined from frozen strawberries grown in 1997 and 1998. In addition to individual compounds, total areas of chromatogram profiles were compared. The major esters were found to be methyl butanoate, ethyl butanoate, methyl hexanoate, and ethyl hexanoate. With the application of principal component analysis and analysis of variance to the data matrix, the varieties were classified into three groups. Var. Honeoye was most different from the others. Organic cultivation had no effect on strawberry volatiles.     

Precursors of chicken flavor. II. Identification of key flavor precursors using sensory methods

Sensory evaluation was used to identify flavor precursors that are critical for flavor development in cooked chicken. Among the potential flavor precursors studied (thiamin, inosine 5'-monophosphate, ribose, ribose-5-phosphate, glucose, and glucose-6-phosphate), ribose appears most important for chicken aroma. An elevated concentration (added or natural) of only 2-4-fold the natural concentration gives an increase in the selected aroma and flavor attributes of cooked chicken meat. Assessment of the volatile odor compounds by gas chromatography-odor assessment and gas chromatography-mass spectrometry showed that ribose increased odors described as "roasted" and "chicken" and that the changes in odor due to additional ribose are probably caused by elevated concentrations of compounds such as 2-furanmethanethiol, 2-methyl-3-furanthiol, and 3-methylthiopropanal.     

Influence of water pressure on the final quality of arabica espresso coffee. Application of multivariate analysis

Water pressure is one of the most important factors which influence the final quality of espresso coffee (EC). However, few studies dealing with this issue have been found. The aim of this work was to study the effect of water pressure on the final quality of Arabica ECs as well as to classify ECs prepared at different pressures (7, 9, and 11 atm) according to their physicochemical and sensory characteristics, key odorants, by means of multivariate analysis. Statistically, principal component 1 (PC1) separated ECs prepared at 7 and 9 atm from ECs prepared at 11 atm and included the main foam and taste characteristics as well as some key odorants and flavor compounds. ECs prepared at 7 and 9 atm were separated by principal component 2 (PC2). Coffees prepared at 9 atm showed consistency of foam and a high percentage of key odorants related to freshness and fruity, malty, and buttery flavors. A simple discriminate function was obtained by discriminate analysis, allowing the classification of ECs prepared at three pressures into their respective groups with a success rate of 100%.     

Evaluation of aroma compounds contributing to muskmelon flavor in Porapak Q extracts by aroma extract dilution analysis

The flavor of the Miyabi variety of Japanese muskmelon was extracted according to the Porapak Q column method (PQM) and evaluated by using aroma extract dilution analysis (AEDA) method. The overall odor of the PQM extracts was perceived as having a natural muskmelon-like odor, suggesting that the PQM was able to extract volatile compounds in muskmelon fruit without degradation of original flavor. Forty-six odorant compounds [Kovats index (KI), 961 < or = KI < or = 2605] were found by GC-sniffing in PQM extracts, confirming the effectiveness of PQM in trapping a wide range of volatile compounds in muskmelon flavor. The 46 odorants could be divided into three groups on the basis of their odor attributes: fruity note (KI < 1300); green, grassy, or cucumber-like note (1300 < KI < 2020); and sweet note (KI > 2020). When the original extracts were diluted in AEDA analysis, seven odorants could still be detected by GC-sniffing at a flavor diluation (FD) factor of 128 or above: one had a fruity note (compound 3); four had a cucumber-like, green, or grassy note (compounds 12, 17, 21, and 23); and two had a sweet note (caramel-like or yakitori-like) (compounds 32 and 34).     

Effect of beta-cyclodextrin on aroma release and flavor perception

Binding and release of volatile compounds to and from beta-cyclodextrin were measured in model aqueous systems using static equilibrium headspace and dynamic headspace dilution. Beta-cyclodextrin decreased the static equilibrium headspace for some volatiles (e.g., ethyl octanoate and decanone) due to binding, but dilution studies demonstrated that binding was readily reversible. Dynamic release of hydrophobic volatile compounds was similar to that observed from emulsions. When beta-cyclodextrin was added to fat free yogurt, the release of a commercial lemon flavoring was modified and was similar to release from a regular fat yogurt. Sensory difference testing confirmed the release results. The data demonstrate that beta-cyclodextrin can be used to modify flavor delivery in both model and real systems; the effects in the latter are sensorially significant.     

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

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

Headspace GC and sensory analysis characterization of the influence of different milk additives on the flavor release of coffee beverages

Previous investigations of coffee flavor have been confined to the analysis of the aroma substances. These investigations showed that about 30 volatile compounds were substantially responsible for the coffee flavor. The aim of this study was to investigate the influence of different milk additives and one coffee whitener on the release of flavor impact compounds from coffee beverages. For the investigation of these effects an external static headspace technique was developed. With this technique the most potent odorants of the coffee beverage were determined. Analyses were performed by gas chromatography/olfactometry, flame ionization detection, and mass spectrometric detection. In addition, sensory studies of the odor profiles were performed. Milk and vegetable products as additives for coffee beverages affected the release of aroma substances in the brew through their lipid, protein, and carbohydrate components. All beverages with an additive showed reduced, but typical, odor profiles for each additive.     

Characterization of the key aroma compounds in soy sauce using approaches of molecular sensory science

Application of aroma extract dilution analysis (AEDA) to the volatiles isolated from a commercial Japanese soy sauce revealed 30 odor-active compounds in the flavor dilution (FD) factor range of 8-4096, among which 2-phenylethanol showed the highest FD factor of 4096, followed by 3-(methylsulfanyl)propanal (methional), the tautomers 4-hydroxy-5-ethyl-2-methyl- and 4-hydroxy-2-ethyl-5-methyl-3(2H)-furanone (4-HEMF), 4-hydroxy-2,5-dimethyl-3(2H)-furanone (4-HDF), and 3-hydroxy-4,5-dimethyl-2(5H)-furanone (sotolone), all showing FD factors of 1024. Thirteen odorants were quantified by stable isotope dilution assays, and their odor activity values (OAVs) were calculated as ratio of their concentrations and odor thresholds in water. Among them, 3-methylbutanal (malty), sotolone (seasoning-like), 4-HEMF (caramel-like), 2-methylbutanal (malty), methional (cooked potato), ethanol (alcoholic), and ethyl 2-methylpropanoate (fruity) showed the highest OAVs (>200). An aqueous model aroma mixture containing 13 odorants, which had been identified with the highest OAVs, in concentrations that occur in the soy sauce showed a good similarity with the overall aroma of the soy sauce itself. Heat treatment of the soy sauce resulted in a clear change of the overall aroma. Quantitation of selected odorants revealed a significant decrease in sotolone and, in particular, increases in 2-acetyl-1-pyrroline, 4-HDMF, and 4-HEMF induced by heating.     

Characterization of some Allium hybrids by aroma precursors, aroma profiles, and alliinase activity

Various Allium hybrids, obtained by the crossbreeding of Allium cepa (onion) as the mother plant and six taxonomically distant wild species obtained by embryo rescue, were investigated with special respect to their individual profiles of cysteine sulfoxides as well as enzymically and nonenzymically formed aroma substances. Alliinase (EC 4.4.1.4) catalyzes the conversion of odorless (+)-S-alk(en)yl-L-cysteine sulfoxides into volatile thiosulfinates. These thiosulfinates were converted to a variety of sulfides by steam distillation. SPME-gas chromatography (GC) and high-performance liquid chromatography (HPLC) used for the analysis of aroma components and their precursors permitted a high sample throughput, so that numerous gene bank accessions and Allium breeding materials were analyzed within a comparatively short time. Cysteine sulfoxides as well as alliinase activity were found in all investigated samples at different levels, but (+)-S-methyl-L-cysteine sulfoxide (methiin) was the most abundant sulfoxide present. (+)-S-(trans-1-Propenyl)-L-cysteine sulfoxide (isoalliin) is typical for onion and was found in all investigated hybrids. The pattern of the other cysteine sulfoxides depended strongly on the parent plants used. The profile of aroma components corresponded with the related pattern of aroma precursors (cysteine sulfoxides). Successful hybridization was proven by randomly amplified polymorphic DNA analysis. Together with these established marker techniques, HPLC and SPME-GC analysis provide support to breeding projects designed to improve the health and aroma properties of Allium hybrids.     

Characterization of the key aroma compounds in apricots (Prunus armeniaca) by application of the molecular sensory science concept

An aroma extract dilution analysis applied on an aroma distillate prepared from fresh apricots revealed (R)-gamma-decalactone, (E)-beta-damascenone, delta-decalactone, and (R/S)-linalool with the highest flavor dilution (FD) factors among the 26 odor-active compounds identified. On the basis of quantitative measurements performed by application of stable isotope dilution assays, followed by a calculation of odor activity values (OAVs), beta-ionone, (Z)-1,5-octadien-3-one, gamma-decalactone, (E,Z)-2,6-nonadienal, linalool, and acetaldehyde appeared with OAVs >100, whereas in particular certain lactones, often associated with an apricot aroma note, such as gamma-undecalactone, gamma-nonalactone, and delta-decalactone, showed very low OAVs (<5). An aroma recombinate prepared by mixing the 18 most important odorants in concentrations as they occurred in the fresh fruits showed an overall aroma very similar to that of apricots. Omission experiments indicated that previously unknown constituents of apricots, such as (E,Z)-2,6-nonadienal or (Z)-1,5-octadien-3-one, are key contributors to the apricot aroma.     

Optimization of extraction of apple aroma by dynamic headspace and influence of saliva on extraction of volatiles

The dynamic headspace procedure of aroma extraction was optimized on Gala apples (Malus domestica). Two parameters affecting the extractability of compounds were studied: temperature and purge time. The influence of artificial saliva was also included. An increase in purge time and temperature caused an increase in the extraction of volatiles from the apple matrix. The optimum point of extraction was 40 degrees C and 70 min of purge. The study also showed that the addition of saliva influenced the extraction of volatile compounds, but this effect was different from one compound to another. To verify that the headspace extracts presented a global odor representativeness of fresh apple under these conditions of extraction, eight assessors compared the odor of extracts with fresh fruit odor for three different cultivars. With regard to the sensory profiles of extracts, the optimal conditions of extraction were suitable for extraction of volatile compounds, even if cooked apple odor appeared in some extracts. The similarity marks of extracts were low but acceptable.     

Development of rancidity in wheat germ analyzed by headspace gas chromatography and sensory analysis

Wheat germ is susceptible to oxidation due to its high content of unsaturated oil. Volatile compounds in stored wheat germ were evaluated using dynamic headspace gas chromatography (HS-GC) and sensory analysis. Preliminary comparisons were also made between freshly prepared wheat germ and wheat germ subjected to microwave heating at 45 and 55 degrees C prior to storage at room temperature. The progress of oxidation was followed in untreated wheat germ for 4 weeks and in heat-treated wheat germ for 7 weeks by HS-GC and sensory evaluation. Significant (p < 0.05) changes in rancid odor and flavor were observed in the untreated wheat germ after 3 weeks, whereas no corresponding difference was observed in the microwave-heated wheat germ after 7 weeks of storage. Identification of a total of 36 volatile compounds was performed according to their mass spectra and Kovats indices. The major volatiles were hexanal, alpha-pinene, 1-hexanol, and 3-carene. In addition to analysis of a short period of storage, 30 volatile compounds were identified from the headspace of wheat germ stored for >1 year.