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Aroma dramatically impacts the overall flavor profiles and consumer acceptance; therefore, it is necessary to conduct a comprehensive analysis of the aroma characteristics of apples. In this study, the aroma differences among four popular apple varieties ("Ruixue", "Liangzhi", "Crystal Fuji," and "Guifei") were compared using two extraction methods (headspace-solid phase microextraction, and solvent-assisted flavor evaporation) coupled with gas chromatography-mass spectrometry-olfactometry (GC-MS-O) and two-dimensional gas chromatography-quadrupole mass spectrometry (GC × GC-qMS). A total of 82 odorants were identified via GC-MS-O, and 143 volatiles were identified by GC× GC-qMS. Among them, 41 key aroma-active compounds (butanal, ethyl acetate, 3-methylbutanal, methyl butanoate, 2-methylpropyl acetate, ethyl 2-methylbutanoate, ethyl 3-methylbutanoate, butyl acetate, hexanal, 2-methylbutyl acetate, 1-butanol, 2-methylpropyl butanoate, 3-methylbutyl acetate, ( E )-2-hexenal, butyl butanoate, butyl 2-methylbutanoate, hexyl acetate, hexyl butanoate, hexyl, 2-methylbutanoate, 1-octen-3-ol, 3-methylthiopropanol, 1,3-octanediol, linalyl acetate, and so on) with high odor activity values (OAVs) and AI value (odor activity values ≥1 or aroma intensity ≥3) were identified. Partial least-squares-discriminant analysis showed that Ruixue exhibited a high "fruity" note, Guifei and Crystal Fuji had the greatest "wood," "floral," and "sweet" notes, while Liangzhi presented a significant "green" note. This study provided flavor chemistry support for the apple quality control and production.

Whisky, brandy, rum, and Chinese baijiu are popular distilled spirits globally, and the volatile components play an essential role in the aroma of these distilled liquors. Volatile compounds in whisky, brandy, rum, and three main aroma types of Chinese baijiu (strong, light, and sauce) were investigated using comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS). Two significant variable detection approaches, the variable importance in the projection (VIP) and nonparametric test (Mann-Whitney U test), were compared to determine the volatile markers among these samples. It was found that the VIP model was more efficient in screening significant variants than the U test. A total of 117 common markers were selected by both the VIP and U test methods with potential aroma contributions. Esters and acids were the main aroma markers for baijiu, diethyl esters were the main aroma markers for brandy, whereras pyrazines, lactones, and furans were the main aroma markers for whisky. Based on the chosen markers, different unknown distilled liquors were successfully classified in the model validation. This study provided a feasible methodology for spirit sample speculation based on volatile composition obtained by GC×GC-TOFMS., (© 2023 Institute of Food Technologists.)

Processing is the crucial factor for green tea aroma quality. In this study, the aroma dynamic changes throughout the manufacturing process of chestnut-like aroma green tea were investigated with gas chromatography electronic nose (GC-E-Nose), gas chromatography-ion mobility spectrometry (GC-IMS), and comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOFMS). GC-IMS identified 33 volatile compounds while GC × GC-TOFMS identified 211 volatile components. Drying exerted the greatest influence on the volatile components of chestnut-like aroma green tea, and promoted the generation of heterocyclic compounds and sulfur compounds which were commonly generated via the Maillard reaction during the roasting stage. A large number of heterocyclic compounds such as 1-methyl-1H-pyrrole, pyrrole, methylpyrazine, furfural, 2-ethyl-5-methylpyrazine, 1-ethyl-1H-pyrrole-2-carboxaldehyde, and 3-acetylpyrrole were newly formed during the drying process. This study also validated the suitability of GC-E-Nose combined with GC-IMS and GC × GC-TOFMS for tracking the changes in volatile components of green tea throughout the manufacturing process., (Copyright © 2022. Published by Elsevier Ltd.)

Wuliangye baijiu is one of the most famous Chinese liquors with a protected geographical indication. This study used LiChrolut ® EN-based solid-phase extraction (SPE) and fractionation combined with comprehensive two-dimensional chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) to unveil its volatile composition. The volatiles were isolated with LiChrolut ® EN-based SPE and traditional liquid-liquid extraction (LLE). The neutral/basic fractions from LLE and the SPE were fractionated on a LiChrolut ® EN SPE column and analyzed by comprehensive GC×GC-TOFMS. Compared with LLE, more esters and alcohols were detected in the SPE-based extraction. The SPE fractionation and GC×GC-TOFMS analysis resulted in the identification of about 500 volatile compounds in more than 3000 peaks of the Wuliangye baijiu. The approach simplifies the complex baijiu composition into functional group-based fractions for reliable identification and analysis. This study provided a confidence volatile identification approach for Chinese baijiu based on the SPE fractionation GC×GC-TOFMS.

Wuliangye baijiu is one of the most famous baijiu in China, with a rich, harmonic aroma profile highly appreciated by consumers. Thousands of volatiles have been identified for the unique aroma profile. Among them, fatty acid esters have been identified as the main contributors to the aroma profile. In addition, many non-ester minor compounds, many of which are more polar than the esters, have been identified to contribute to the characteristic aroma unique to Wuliangye baijiu. The analysis of these minor compounds has been challenging due to the dominance of esters in the sample. Thus, it is desirable to fractionate the aroma extract into subgroups based on functional group or polarity to simplify the analysis. This study attempts a new approach to achieve simultaneous volatile extraction and fractionation using tandem LiChrolut EN and silica gel solid-phase extraction (SPE) columns. A baijiu sample (10 mL, diluted in 40 mL of water) was first passed through the LiChrolut EN (1.0 g) column. The loaded LiChrolut EN column was then dried with air and coupled with a silica gel (5.0 g) SPE column with anhydrous Na 2 SO 4 (10.0 g) in between. The volatile compounds were eluted from the LiChrolut EN column and simultaneously fractionated on the silica gel column based on polarity. The simultaneous extraction and fractionation technique enabled the fractionations of all fatty acid esters into less polar fractions. Fatty acids, alcohols, pyrazines, furans, phenols, hydroxy esters, and other polar compounds were collected in more polar fractions. This technique was used to study the volatile compounds in Wuliangye, Moutai, and Fengjiu baijiu. In addition to fatty acid esters, many minor polar compounds, including 2,6-dimethylpyrazine, 2-ethyl-6-methylpyrazine, 2-ethyl-3,5-dimethylpyrazine, p -cresol, and 2-acetylpyrrole, were unequivocally identified in the samples. The procedure is fast and straightforward, with low solvent consumption.

Smoke-derived taint has become a significant concern for the U.S. wine industry, particularly on the west coast, and climate change is anticipated to aggravate it. High volatile phenols such as guaiacol, 4-methylguaiacol, 4-ethylguaiacol, 4-ethylphenol, and o -, p -, m -cresols have been suggested to be related to smoke-exposed grape and wine. This paper describes an analytical approach based on ethylene glycol/polydimethylsiloxane (EG/PDMS)-stir bar sorptive extraction-gas chromatography-mass spectrometry (SBSE-GC-MS) to quantify or estimate the concentrations of some smoke-related volatile phenols in wines. Correlation coefficients with R 2 ≥ 0.990 were obtained. This method can quantify most smoked-related volatile phenols down to 0.5 μg/L in wine in selective ion monitoring mode. Recovery for the targeted volatile phenols ranged from 72.2% to 142.4% in the smoke-tainted wine matrix, except for 4-vinylguaiacol. The standard deviations of the volatile phenols were from 0 to 23% in smoke-tainted wine. The approach provides another tool to evaluate wine smoke exposure and potential smoke taint.

Aroma-active compounds in northern highbush blueberries "Bluecrop" ( Vaccinium corymbosum "Bluecrop") and "Elliott" ( Vaccinium corymbosum "Elliott") were isolated using solvent extraction followed by solvent-assisted flavor evaporation. The aroma-active compounds were compared by aroma extract dilution analysis (AEDA) on a polar and a chiral column and odor activity values (OAVs). The results showed that both cultivars had similar aroma-active compounds, but the flavor dilution (FD) factors and OAV values varied, responsible for the subtle aroma differences. AEDA (FD ≥ 64) suggested that the important aroma-active compounds in both cultivars could be ethyl 2-methylbutanoate, ethyl 3-methylbutanoate, (Z)-3-hexenal, 1-octen-3-one, (Z)-3-hexen-1-ol, methional, linalool, (E,Z)-2,6-nonadienal, 2-methylbutanoic acid, α-terpineol, (E,E)-2,4-nonadienal, β-damascenone, geraniol, geranyl acetone, o -cresol, eugenol, and vanillin. Different isomers can have different sensory thresholds and attributes. Enantiomer analysis revealed that although S-(+)-linalool was dominant in blueberry, R-(-)-linalool had a higher FD value and OAVs than that of the (S)-isomer. The S-(-)-α-terpineol was slightly elevated than R-(+)-α-terpineol in both cultivars.

The drying technology is crucial to the quality of Congou black tea. In this study, the aroma dynamic characteristics during the variable-temperature final firing of Congou black tea was investigated by electronic nose (e-nose) and comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOFMS). Varying drying temperatures and time obtained distinctly different types of aroma characteristics such as faint scent, floral aroma, and sweet fragrance. GC × GC-TOFMS identified a total of 243 volatile compounds. Clear discrimination among different variable-temperature final firing samples was achieved by using partial least squares discriminant analysis (R2Y = 0.95, Q2 = 0.727). Based on a dual criterion of variable importance in the projection value (VIP > 1.0) and one-way ANOVA (p < 0.05), ninety-one specific volatile biomarkers were identified, including 2,6-dimethyl-2,6-octadiene and 2,5-diethylpyrazine with VIP > 1.5. In addition, for the overall odor perception, e-nose was able to distinguish the subtle difference during the variable-temperature final firing process., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

Qingke liquor is a very famous Tibetan alcoholic beverage made from "Qingke", hull-less highland barley, which is exclusively grown in Qinghai-Tibetan Plateau with an average altitude of 4000 m. Qingke liquor made in such an area whose quality or characteristics is a result of its geographic environment, including natural and human culture. In this study, the aroma compounds in two Qingke liquors made from highland barley grown at different elevations (QKH, high elevation, and QKL, low elevation) were compared by aroma extract dilution analysis (AEDA), aroma intensity (Osme), odor activity values (OAVs, ratio of concentration to odor threshold), and aroma recombination. Results revealed ethyl acetate, ethyl 2-methyl propanoate, ethyl butanoate, ethyl 3-methyl butanoate, ethyl pentanoate, ethyl hexanoate, ethyl octanoate, 3-methylbutanal, 3-methyl-1-butanol, 1-octen-3-ol, β-damascenone, 2,3-butanedione (diacetyl), acetoin, and 2-methoxyphenol (OAV ≥ 10) as important aroma active compounds to Qingke liquors. However, QKH had higher OAVs for most of the compounds than that of QKL. An aroma recombination study confirmed the analysis of aroma-active compounds in Qingke liquor, whereas the aroma emission test demonstrated 3-methylbutanal as the key aroma compound for both Qingke liquors.

Complications in the analysis of volatile sulfur compounds (VSC) in wine using solid-phase microextraction (SPME) arise from sample variability. Constituents of the wine matrix, including ethanol, affect the volatility and adsorption of sulfur volatiles on SPME fiber coatings (Carboxen- polydimethylsiloxane(PDMS); DVB-Carboxen-PDMS and DVB-PDMS), which can impact sensitivity and accuracy. Here, several common wine sulfur volatiles, including hydrogen sulfide (H 2 S), methanethiol (MeSH), dimethyl sulfide (DMS), dimethyl disulfide (DMDS), dimethyl trisulfide (DMTS), diethyl disulfide (DEDS), methyl thioacetate (MeSOAc), and ethyl thioacetate (EtSOAc) are analyzed, using SPME followed by gas chromatography (GC), using a system equipped with a pulsed-flame photometric detection (PFPD) system, at various ethanol concentrations in a synthetic wine matrix. Ethyl methyl sulfide (EMS), diethyl sulfide (DES), methyl isopropyl sulfide (MIS), ethyl isopropyl sulfide (EIS), and diisopropyl disulfide (DIDS) are evaluated as internal standards. The absorption of volatile compounds on the SPME fiber is greatly affected by ethanol. All compounds exhibit a stark decrease in detectability with the addition of ethanol, especially between 0.0 and 0.5% v / v . However, the ratio of interested sulfur compounds to the internal standard becomes more stable when the total alcohol concentration exceeds 2%. EMS was found to best resemble DMS. EIS and DES were found to best resemble DMDS, MeSOAc, and EtSOAc. DIDS was found to best resemble DEDS, DMTS, H 2 S, and MeSH.

The analysis of volatile sulfur compounds using headspace solid-phase microextraction (HS-SPME) is heavily influenced by matrix effects. The effects of a wine matrix, both non-volatile and volatile components (other than ethanol) were studied on the analysis of several common sulfur volatiles found in wine, including hydrogen sulfide (H 2 S), methanethiol (MeSH), dimethyl sulfide (DMS), dimethyl disulfide (DMDS), dimethyl trisulfide (DMTS), diethyl disulfide (DEDS), methyl thioacetate (MeSOAc), and ethyl thioacetate (EtSOAc). Varying levels of devolatilized wine and common wine volatiles (acids, esters, alcohols) were added to synthetic wine samples to act as matrices. Sulfur standards were added and analyzed using gas chromatography with pulsed-flame photometric detection (GC-PFPD). Five internal standards were used to find best representatives of each compound despite matrix effects. Sensitivity remained stable with the addition of devolatilized wine, while addition of volatile components decreased sensitivity. DMS was found to be best measured against EMS; DMDS and the thioacetates were best measured against DES; H 2 S, MeSH, DEDS, and DMTS were best measured against DIDS. The method was used to quantitate the volatile sulfur compounds in 21 wines with various ethanol contents and volatile profiles.

Developmental changes in the carotenoids and volatile compounds of Pinot noir grape berries were investigated in this study from pea size to harvest during 2012. HPLC analysis showed continued decrease of lutein, β-carotene, neochrome a and neoxanthin continued to decrease during berry development, with rapid decrease of lutein and (9'z)-neoxanthin occurred two weeks before véraison. Neochrome b and violaxanthin accumulated at early development and started to decrease two weeks before véraison. Volatile analysis demonstrated that total β-damascenone, TDN and vitispirane all increased dramatically, especially at later stage of ripening, whereas the changes for α-ionone and β-ionone were not obvious. The correlation between carotenoids and C13-norisoprenoids in the grape berries was compound-dependent, suggesting dependency on enzyme activity and specificity. In addition, C6-alcohols accumulated before véraison and decreased towards maturation, and 3-isobutyl-2-methoxyprazine decreased with increasing maturity., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

The influence of cluster-zone leaf removal on Pinot noir vine growth and fruit chemical and volatile composition was investigated in 3 years. Different severities of leaf removal (0%, 50%, 100%) were imposed during the pea-size stage of development from the cluster zone. Results show that cluster-zone leaf removal had little influence on vine growth, crop load, or grape maturity in terms of total soluble solids (TSS), pH or titratable acidity (TA) at harvest. However, 100% leaf removal resulted in higher concentrations of quercetin glycoside in grapes compared to 0% leaf removal. The 100% leaf removal also increased concentrations of petunidin- and malvidin-3-monoglucoside anthocyanins in two out of 3 years (2010 and 2012) by an average of 62% and 53%, respectively. In addition, 100% leaf removal resulted in higher concentrations of β-damascenone, and some bound-form terpenoids. The increases in β-damascenone were positively correlated to the increased sunlight exposure., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Laboratory screening bioassays and field trapping experiments of spotted wing drosophila flies, Drosophila suzukii (Matsumura) (Diptera: Drosophilidae), were conducted to determine the attractiveness of 17 compounds as well as to compare attractant efficiency during peak fruit ripeness and postharvest captures late in the season. Compounds structurally related to each of the fermentation products acetic acid, ethanol, ethyl acetate, and 2-phenethyl alcohol were screened for attractiveness compared with a soap water control in greenhouse cage bioassays. The compounds determined to be attractive in the greenhouse bioassay (methanol, ethanol, propanol, formic acid, acetic acid, ethyl acetate, propyl acetate, phenethyl acetate, phenethyl propionate, and phenethyl butyrate) were individually tested in the field added to apple cider vinegar (ACV). The acids were also tested individually in neutralized ACV (NACV; pH ≍7). Combinations of the compounds were tested in NACV. The capture numbers in ACV traps were not significantly increased by the addition of any of the compounds tested, although significant deterrent effects of some of the compounds allowed differences between treatments to be observed. Compounds that are most prevalent in wine and vinegar (methanol, ethanol, acetic acid, and ethyl acetate) as well as phenethyl propionate and phenethyl butyrate were less deterrent than the other compounds tested in the field. Captures during peak fruit ripeness were compared with the postharvest period when fruit hosts were not available or were overripe. Although the total number of flies captured late in the season was lower, the trends in treatment performance were similar, indicating a consistent performance of these baits from peak fruit ripeness through postharvest.

The effect of deficit irrigation and a kaolin-based, foliar reflectant particle film (PF) on grape composition and volatile compounds in Merlot grapes was investigated over two growing seasons in semi-arid, south-western Idaho. Vines were provided with differential amounts of water based on their estimated crop evapotranspiration (ET(c)) throughout berry development, and particle film was applied to half of the vines in each irrigation main plot. Free and bound volatile compounds in grapes were analyzed using stir bar sorptive extraction-gas chromatography-mass spectrometry (SBSE-GC-MS). The concentrations of free C(6) compounds (hexanal, trans-2-hexenal, and 1-hexanol) decreased, and bound terpene alcohols (nerol and geraniol) and C(13)-norisoprenoids (β-damascenone, 3-hydroxy-β-damascenone, 1,1,6-trimethyl-1,2-dihydronaphthalene, and 3-oxo-α-ionol) increased in berries each year in response to severity of vine water stress. Concentrations of C(13)-norisoprenoids and bound forms of nerol and geraniol were positively correlated with their concentrations in the corresponding wines. Particle film application had minimum effect on free and bound volatile composition in the grapes, and there was no interactive effect between particle film and deficit irrigation. However, particle film application enhanced the total amount of berry anthocyanins., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

The volatile composition and sensory attributes of Merlot wines produced from vines under differing levels of water stress, with or without a foliar, kaolin-based particle film, were analyzed by stir bar sorptive extraction-gas chromatography-mass spectrometry (SBSE-GC-MS) and sensory evaluation. Vines were irrigated over consecutive vintages with 100, 70, or 35% of their estimated water requirements (ET(c)), or 35% until color change then 70% until harvest (35-70% ET(c)). Neither of the treatments consistently influenced ester concentrations or their relative amounts, though their concentrations varied from year to year. However, deficit irrigation had an effect on the concentration of terpene alcohols and norisoprenoids. Wines produced from vines under water deficit contained higher amounts of citronellol, nerol, geraniol, and β-damascenone, but linalool and β-ionone were not affected by deficit irrigation. Particle film did not affect volatile composition in the wine. Untrained panelists in 2007 and 2008 distinguished between wines from vines that received 100 or 35% ET(c) and between wines from vines that received 35 or 35-70% ET(c). Trained sensory panelists detected differences among wines for aroma, flavor, taste, and mouthfeel; however, significant interactive effects between particle film application and vine water status hindered interpretation of independent main effects.

Glycosidically bound volatiles and precursors in genotypes representing the pedigree for 'Marion' blackberry were investigated over two growing seasons. The volatile precursors were isolated using a C18 solid-phase extraction column. After enzymatic hydrolysis, the released volatiles were analyzed using stir bar sorptive extraction gas chromatography-mass spectrometry (GC-MS) and direct microvial insert thermal desorption GC-MS. The most abundant volatile precursors in the genotypes were alcohols, followed by shikimic acid derivatives. High amounts of furanone glycosides were also detected, while norisoprenoids only existed in a small amount in blackberries. The volatile precursor composition in the genotypes in the 'Marion' pedigree was very similar to their free volatile distribution. 'Logan' and 'Olallie' predominantly had bound norisoprenoids. Wild 'Himalaya' predominated with terpene alcohol and furaneol glycosides, whereas 'Santiam' and 'Chehalem' contained a high level of terpene alcohol glycosides. A similar inheritance pattern was also observed for some volatile precursors in the genotypes in the 'Marion' pedigree. A high content of linalool, hydroxylinalool, and alpha-ionol glycosides in 'Olallie' and a low content in 'Chehalem' resulted in a moderate level in their offspring 'Marion', while a low content of (E)-linalool oxide precursor in 'Olallie' and a high content in 'Chehalem' also resulted in a moderate level in 'Marion'. However, the concentration of furaneol glycosides in 'Marion' exceeded that of its two parents.

The distribution of volatile constituents in ancestral genotypes of 'Marion' blackberry's pedigree was investigated over two growing seasons. Each genotype in the pedigree had a specific volatile composition. Red raspberry was dominated by norisoprenoids, lactones, and acids. 'Logan' and 'Olallie' also had a norisoprenoid dominance but at much lower concentrations. The concentration of norisoprenoids in other blackberry genotypes was significantly lower. Terpenes and furanones were predominant in wild 'Himalaya' blackberry, whereas terpenes were the major volatiles in 'Santiam'. 'Marion', a selection from 'Chehalem' and 'Olallie', contained almost all of the volatile compounds in its pedigree at moderate amount. The chiral isomeric ratios of 11 pairs of compounds were also studied. Strong chiral isomeric preference was observed for most of the chiral compounds, and each cultivar had its unique chiral isomeric distribution. An inherent pattern was observed for some volatile compounds in the 'Marion' pedigree. Raspberry and 'Logan' had a very high concentration of beta-ionone, but was reduced by half in 'Olallie' and by another half in 'Marion' as the crossing proceeded. A high content of linalool in 'Olallie' and a low content in 'Chehalem' resulted in a moderate content of linalool in their progeny 'Marion'. However, the concentration of furaneol in 'Marion' was higher than in its parents. A high content of (S)-linalool in 'Olallie' and a racemic content of (S)-,(R)-linalool in 'Chehalem' resulted in a preference for the (S)-form in 'Marion'.

The impact of deficit irrigation during berry development on Merlot wine volatile composition was investigated in this study. Own-rooted Merlot vines grown in a commercial vineyard in Idaho were supplied with 100 or 35% of their estimated crop evapotranspiration needs throughout the berry development. Wines were produced from those grapes from the 2002, 2003, and 2004 growing seasons. Volatile compounds in the wines were analyzed using the stir bar sorptive extraction-gas chromatography-mass spectrometry technique. The results demonstrated that despite vintage differences in volatile composition, in each of 3 years of this study, deficit irrigation during berry development had a consistent effect on wine volatile composition. Wine produced from deficit-irrigated vines had increased amounts of vitispiranes, beta-damascenone, guaiacol, 4-methylguaiacol, 4-ethylguaiacol, and 4-vinylguaiacol relative to wine produced from well-watered vines. Deficit irrigation had no effect on the concentrations of other measured volatiles such as esters and terpenes.