In Situ Oral Metabolism Analysis of Astringent Compounds in Tea by Paper Spray Mass Spectrometry, Electrospray Mass Spectrometry, Turbidimetry, and Sensory Evaluation.

The phenolic compounds (PCs) are the primary components responsible for the astringency of tea infusions, and this astringency is intricately linked to the in situ oral metabolism of PCs in saliva. Initially, a total of 54 PCs were identified in tea infusions by electrospray mass spectrometry (ESI-MS). Subsequently, an in vivo metabolism analysis of PCs during varying drinking times and oral locations was conducted by both paper spray mass spectrometry (PS-MS) and sensory evaluation. The metabolism of PCs within oral saliva was a prolonged process, the residual PCs were distributed across diverse oral regions after drinking tea infusion, and the higher residual PC content reflected the stronger astringency intensity. Furthermore, an in vitro metabolism analysis of PCs under varied reaction temperatures and durations was performed by ESI-MS and turbidimetry. As the reaction time extended, more PCs in tea was interacting with saliva. Moreover, the higher temperatures facilitated this interaction between PCs and saliva. Therefore, this investigation establishes a foundation for further elucidating the mechanisms underlying astringency formation.

Discovery and Flavor Characterization of High-Grade Markers in Baked Green Tea.

Green tea is a popular beverage around the world and possesses a unique flavor. The flavor qualities of green tea are closely related to its grade and this relationship has not yet been studied. Three baked green teas with similar flavor were studied, namely, Huangshan Maofeng, Taiping Houkui, and Shucheng Xiaolanhua. A total of 34 odor compounds were identified by solid phase microextraction (SPME) combined with two-dimensional comprehensive gas chromatography-olfactometry-mass spectrometry analysis (GC×GC-O-MS). The results of the clustering analysis showed that the content of D-limonene and linalool in the high-grade (Grade A) tea was much higher than the content in other grades, so they were identified as odor markers of Grade A baked green tea. The taste components of different grades of green tea infusion were analyzed by high-performance liquid chromatography-mass spectrometry (HPLC-MS) and HPLC. A combination of clustering analysis, principal component analysis (PCA), and orthogonal partial least squares discrimination analysis (OPLS-DA) indicated that galloylglucose, digalloylglucose, trigalloyglucose, strictinin, and gallic acid could be used as taste markers of Grade A baked green tea. Therefore, the results in this paper reveal the substances responsible for the odor and taste markers of high-grade baked green tea.

Comparison of Different Volatile Extraction Methods for the Identification of Fishy Off-Odor in Fish By-Products.

This study was conducted to analyze volatile odor compounds and key odor-active compounds in the fish soup using fish scarp and bone. Five extraction methods, including solid-phase microextraction (SPME), dynamic headspace sampling (DHS), solvent-assisted flavor evaporation (SAFE), stir bar sorptive extraction (SBSE), liquid-liquid extraction (LLE), were compared and SPME was finally selected as the best extraction method for further study. The volatile odor compounds were analyzed by gas chromatography-olfactometry-mass spectrometry (GC-O-MS) and comprehensive two-dimensional gas chromatography-olfactometry-mass spectrometry (GC × GC-O-MS) techniques, and the key odor-active compounds were identified via aroma extract dilution analysis (AEDA) and relative odor activity value (r-OAV) calculation. A total of 38 volatile compounds were identified by GC-O-MS, among which 10 were declared as odor-active compounds. Whereas 39 volatile compounds were identified by GC × GC-O-MS, among which 12 were declared as odor-active compounds. The study results revealed that 1-octen-3-one, 2-pentylfuran, (E)-2-octenal, 1-octen-3-one, hexanal, 1-octen-3-ol, 6-methylhept-5-en-2-one, (E,Z)-2,6-nondienal and 2-ethyl-3,5-dimethylpyrazine were the key odor-active compounds in the fish soup.

Characterization of Key Aroma-Active Compounds in Rough and Moderate Fire Rougui Wuyi Rock Tea (Camellia sinensis) by Sensory-Directed Flavor Analysis and Elucidation of the Influences of Roasting on Aroma.

Rougui Wuyi rock tea (WRT) with the premium aroma is a subcategory of oolong tea. Roasting is a unique process that provides a comprehensive aroma to WRT. The key aroma-active compounds of rough Rougui WRT (RR) and Rougui WRT with moderate fire (RM) were characterized by sensory-directed flavor analysis. A total of 80 aroma-active compounds were identified by gas chromatography-olfactometry-time-of-flight-mass spectrometry (GC-O-TOF-MS) and two-dimensional comprehensive gas chromatography-olfactometry-mass spectrometry (GC × GC-O-MS), and 42 of them revealing high flavor dilution (FD) factors (16-4096) during aroma extract dilution analysis were quantitated. Finally, the aroma recombination and omission experiments confirmed 26 odorants as key aroma-active compounds in Rougui WRT. Roasting enhanced the aroma of roasted, woody, burnt/smoky, and cinnamon-like odor impressions in RM evoked by 2- and 3-methylbutanal, furaneol, 3-methylbutanoic acid, propanoic acid, methional, ß-myrcene, 2-pentylfuran, 5- and 6-methyl-2-ethylpyrazine, and furfural. In contrast, hexanal, linalool, (Z)-3-hexen-1-ol, (Z)-4-heptenal, (E)-2-heptenal, geraniol, pentanal, and ß-nerolidol were responsible for the more intense floral, fruity, and grassy/fresh leaf-like aroma attributes in RR.

Rapid visualized characterization of phenolic taste compounds in tea extract by high-performance thin-layer chromatography coupled to desorption electrospray ionization mass spectrometry.

Phenolic compounds are the important taste source of tea infusion. In this paper, the phenolic compounds in tea extracts were separated by high-performance thin-layer chromatography (HPTLC), and then in-situ determined by desorption electrospray ionization mass spectrometry (DESI-MS). Total 44 phenolic compounds in tea extracts were accurately confirmed by NIST library as well as reference substances. The clustering results of heat-map can better reflect the differences of phenolic compounds in different categories and subcategories of teas. Besides, the contents of hydrolyzable tannins, including galloylglucose, digalloylglucose, trigalloyglucose and strictinin, were positively correlated with the grades of green tea. The method validation and quantification results of exemplified five phenolic compounds in teas were also obtained, and LODs, LOQs and recoveries were ranging between 1.5-15.9 µg/mL, 5.1-53.1 µg/mL, and 79%-117.6%, respectively. Moreover, HPTLC-DESI-MS can save tenfold analytical time compared to HPLC-MS. Therefore, HPTLC-DESI-MS was a rapid, efficient characterization method of phenolic compounds in tea extracts.

Differences of characteristic aroma compounds in Rougui tea leaves with different roasting temperatures analyzed by switchable GC-O-MS and GC × GC-O-MS and sensory evaluation.

Roasting, an important process to refine Wuyi Rock tea, could impart different types of aroma to the final products. This study focuses on the differences in aroma characteristics among three kinds of refined teas, named light fire (LF), moderate fire (MF), and high fire (HF). A combination of solid phase microextraction (SPME) and a switchable system between GC-O-MS and GC × GC-O-MS was utilized to identify the odorants. In total, 97 aroma-active compounds could be smelled at the sniffing port, comprising alcohols, aldehydes, ketones, esters, heterocycles, and terpenes. However, only 52 obtained r-OAV >1. Significant differences were uncovered by the application of principal component analysis (PCA) and partial least squares regression (PLSR). Thereby, MF and HF had a more similar aroma profile, while in LF samples, alcohols, aliphatic aldehydes and some ketones were responsible for the aroma profile, such as (E,E)-2,4-hexadienal, octanal, hexanal, (E,Z)-2,6-nonadienal, (E)-ß-ionone, 3-octen-2-one etc. Strecker aldehydes had a great impact on the aroma of MF, including 2-methylpropanal, 2-methylbutanal, 3-methylbutanal etc. Some N-heterocyclic compounds also affected the overall aroma, for instance, 6-methyl-2-ethylpyrazine. In HF, the majority of aroma compounds increased with increasing roasting temperature, especially N-heterocyclic compounds as well as furfural and 5-methyl-2-furancarboxaldehyde, which are all closely related to the Maillard reaction. Besides, 5-methyl-2-(1-methylethenyl)-4-hexen-1-ol, trans-linalooloxide and 2-nonanone also remarkably influenced the aroma of HF. In addition, it was supposed that most amino acids that participated in the Maillard reaction during roasting were decomposed from the compounds that combined with tea polyphenols and amino acids.

Structural identification of sour compounds in wine and tea by ambient ionization mass spectrometry according to characteristic product ion and neutral loss.

Sourness is an important food taste for human. A rapid, accurate method was used to generalize the structure similarity and diversity of sour compounds. Based on the product ion and neutral loss of sour compounds, ambient ionization techniques combined with quadrupole-Orbitrap mass spectrometry (AI-Q-Orbitrap) was employed. According to the behavior of sour compounds in the process of high collision dissociation (HCD) of MS/MS, three fragmentation pathway schemes were proposed: (1) charge-driven fragmentation and CO2 loss, (2) six-membered ring rearrangement and Cα-Cß cleavage, and (3) elimination rearrangement and H2O, CO2 and CO loss in succession. Besides, structure information about characteristic product ions and characteristic neutral losses was summarized. Finally, multi-class sour compounds including monoacids, diacids, polyacids and phenolic acids in wine and tea were identified and compared. Therefore, sour compounds and their structure information can be determined by AI-MS based on characteristic product ion and neutral loss.

Sensory-guided identification of bitter compounds in Hangbaizhi (Angelica Dahurica).

As a traditional Chinese medicine, Angelica dahurica (Fisch. ex Hoffm.) Benth. et Hook. f. ex Franch. et Sav. cv. Hangbaizhi (Hangbaizhi) is not only used for the curative treatment of diseases such as the common cold and toothache, but also is an important spice that is used to increase the aroma and remove the unpleasant odor in many foods. Hangbaizhi has however, been reported to cause a bitter taste. In this study, the bitter compounds in Hangbaizhi after three common processes (boiling, frying and boiling after frying) were studied. Six bitter compounds (oxypeucedanin hydrate, bergapten, xanthotoxol, imperatorin, isoimpinellin and oxypeucedanin) were identified by high performance liquid chromatography (HPLC)-diode array detection (DAD)-electrospray ionization (ESI)-tandem mass spectrometry (MS) and sensory evaluation. The contribution of these bitter compounds was ranked by taste dilution analysis (TDA). Upon the assessment of methods to reduce the bitter flavor, it was found that baijiu (Chinese liquor) pretreatment was more effective than water-pretreatment.

Comparison and Identification of the Aroma-Active Compounds in the Root of Angelica dahurica.

Solid-phase microextraction (SPME), purge and trap (P&T), stir bar sportive extraction (SBSE), and dynamic headspace sampling (DHS) were applied to extract, separate and analyze the volatile compounds in the roots of Hangbaizhi, Qibaizhi, and Bobaizhi and the GC-O-MS/MS (AEDA) was utilized for the quantification of key aroma compounds. Totals of 52, 54, and 43 aroma-active compounds extracted from the three samples by the four extraction methods were identified. Among these methods, the SPME effectively extracted the aroma compounds from the A. dahurica. Thus, using the SPME methods for quantitative analysis based on external standards and subsequent dilution analyses, totals of 20, 21, and 17 aroma compounds were detected in the three samples by the sniffing test, and sensory evaluations indicated that the aromas of A. dahurica included herb, spice, and woody. Finally, principal component analysis (PCA) showed that the three kinds A. dahurica formed three separate groups, and partial least squares discriminant analysis (PLS-DA) showed that caryophyllene, (-)-ß-elemene, nonanal, and ß-pinene played an important role in the classification of A. dahurica.

Characterization of Key Aroma-Active Compounds in Black Garlic by Sensory-Directed Flavor Analysis.

Black garlic is a new garlic product produced through fermentation of fresh garlic and is very popular in Asia countries due to its health benefits. Its key aroma-active compounds were characterized by gas chromatography-olfactometry-mass spectrometry (GC-O-MS), gas chromatography-time-of-flight mass spectrometry (GC-TOFMS), and sensory evaluation. In total 52 aroma compounds were identified, and 15 of them with high flavor dilution (FD) factors based on aroma extract dilution analysis (AEDA) were selected and quantitated. Finally, 9 key aroma-active compounds, including acetic acid (sour), allyl methyl trisulfide (cooked garlic), Furaneol (caramel), diallyldisulfide (garlic), diallyltrisulfide (sulfur), (E,Z)-2,6-nonadien-1-ol (cucumber), 3-methylbutanoic acid (sweat), 5-heptyldihydro-2(3H)-furanone (apricot), and diallyl sulfide (garlic), were determined through aroma recombination and omission experiment. In addition to the sulfur-containing compounds, heterocyclic compounds were the major aroma contributors in black garlic. Sensory evaluation revealed that the flavor profile of black garlic mainly consisted of sulfur, sour, sweet, fresh, sauce, gasoline, and roasted odors.

Comparison of flavour fingerprint, electronic nose and multivariate analysis for discrimination of extra virgin olive oils.

Flavour is a special way to discriminate extra virgin olive oils (EVOOs) from other aroma plant oils. In this study, different ratios (5, 10, 15, 20, 30, 50, 70 and 100%) of peanut oil (PO), corn oil (CO) and sunflower seed oil (SO) were discriminated from raw EVOO using flavour fingerprint, electronic nose and multivariate analysis. Fifteen different samples of EVOO were selected to establish the flavour fingerprint based on eight common peaks in solid-phase microextraction-gas chromatography-mass spectrometry corresponding to 4-methyl-2-pentanol, (E)-2-hexenal, 1-tridecene, hexyl acetate, (Z)-3-hexenyl acetate, (E)-2-heptenal, nonanal and α-farnesene. Partial least square discrimination analysis (PLS-DA) was used to differentiate EVOOs and mixed oils containing more than 20% of PO, CO and SO. Furthermore, better discrimination efficiency was observed in PLS-DA than PCA (70% of CO and SO), which was equivalent to the correlation coefficient method of the fingerprint (20% of PO, CO and SO). The electronic nose was able to differentiate oil samples from samples containing 5% mixture. The discrimination method was selected based on the actual requirements of quality control.