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.

Characterization of the odor compounds in human milk by DHS/GC × GC-O-MS: A feasible and efficient method.

Odor analysis of human milk (HM) is often challenging. Here, a new strategy for the analysis of odorants in HM using dynamic headspace sampling combined with comprehensive two-dimensional gas chromatography-olfactometry-mass spectrometry (DHS/GC × GC-O-MS) was established based on the comparison of different extraction methods and instrument modes. Overall, DHS/GC × GC-O-MS was proved to be able to provide higher extraction efficiency and better analytical results of the odor-active compounds (OACs) in HM, meanwhile, the salt addition during the extraction further promoted the release of the odorants. Twenty key OACs in HM were identified by flavor dilution analysis and odor activity calculation, of which 1-octen-3-one, 2,3-butanedione, (E)-2-nonenal, and nonanal contributed significantly to the odor of HM. In addition, 2,3-pentanedione was detected as a key OAC in HM for the first time. This study provided a powerful analytical strategy for the comprehensive odor analysis of HM.

Characterization of key aroma-active compounds in blue honeysuckle (Lonicera caerulea L.) berries by sensory-directed analysis.

Blue honeysuckle (Lonicera caerulea L.) berries are nutritionally rich and unique in flavor. However, its aroma compounds have not been known well. In this study, the key aroma-active compounds in 8 different varieties of blue honeysuckle berries were studied by sensory-directed analysis. Sensory evaluation suggested that the aroma profile of blue honeysuckle berry was fruity, floral, grassy, sweet, and sour. A total of 68 aroma compounds were detected by two-dimensional comprehensive gas chromatography-olfactometry-mass spectrometry analysis (GC × GC-O-MS). Then, aroma extraction dilution analysis (AEDA) and odor activity value (OAV) showed that 12 compounds were indicated to be the major aroma contributors. According to the principal component analysis (PCA) results, eight varieties were divided into three categories for their differences on alcohols and terpenoids content. Finally, the aroma recombination and omission experiments determined that linalool, hexanal, eucalyptol, octanal, nonanal, and ethyl 2-methylbutyrate were the key aroma-active compounds in blue honeysuckle berries.

Aroma Identification and Classification in 18 Kinds of Teas (Camellia sinensis) by Sensory Evaluation, HS-SPME-GC-IMS/GC × GC-MS, and Chemometrics.

Tea (Camellia sinensis) is one of the most popular beverages worldwide. Many types of tea products continuously emerge in an endless stream; so, the classification of tea becomes more difficult. Aroma is a vital indicator of tea quality. The present study deals with the identification of aroma compounds in 18 different kinds of tea belonging to three typical tea varieties, including green tea, oolong tea, and black tea, using GC-IMS and GC × GC-O-MS. Moreover, the clustering of all 18 tea samples and the in depth correlation analysis between sensory evaluation and instrumental data were performed using the PCA and OPLS-DA. The results revealed that in all 18 kinds of tea, a total of 85 aroma compounds were detected by GC-IMS, whereas 318 were detected by GC × GC-O-MS. The PCA result revealed that green tea, oolong tea, and black tea could be clearly separated based on their peak areas. The OPLS-DA result showed that a total of 49 aroma compounds with VIP value > 1.0 could be considered as the potential indicators to quickly classify or verify tea types. This study not only compared the aroma differences across different types of teas, but also provided ideas for the rapid monitoring of tea quality and variety.

Odor changes in breast milk during different storage temperatures and times using GC × GC-O-MS.

Breastfeeding is generally the preferred way that most mothers will choose. It is common to store expressed breast milk in the refrigerator in many families. However, there is a phenomenon that infants may refuse to consume stored breast milk, presumably due to changes in odor. Thus, the odor changes in breast milk stored at 4 °C for 72 h and at -20 °C for 60 d were studied. Compared with fresh breast milk, 7 and 16 odor compounds were newly detected by SPME and GC × GC-O-MS when breast milk was stored at 4 and -20 °C, respectively. The concentration of (E)-2-decenal, octanal, hexanal, 1-octen-3-ol, 2-pentylfuran, lauric acid, decanoic acid and hexanoic acid significantly increased after storage at 4 °C for 36 h and -20 °C for 30 d. In addition, the proportion of acids increased, whereas that of aldehydes decreased during storage. Chemometric analysis with OPLS-DA suggested that breast milk should be stored at 4 °C for less than 36 h and at -20 °C for less than 30 d for maximum preservation of the original odors.

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.

Variation of Aroma Components of Pasteurized Yogurt with Different Process Combination before and after Aging by DHS/GC-O-MS.

Pasteurized yogurt is a healthy yogurt that can be stored in ambient temperature conditions. Dynamic headspace sampling (DHS) combined with gas chromatography-olfactory mass spectrometry (GC-O-MS), sensory evaluation, electronic nose (E-nose), and partial least squares discriminant analysis (PLS-DA) were used to analyze the flavor changes of pasteurized yogurt with different process combinations before and after aging. The results of odor profiles showed that the sensory descriptors of fermented, sweet, and sour were greatly affected by different process combinations. The results of odor-active compounds and relative odor activity value (r-OAV) showed that the combination of the production process affected the overall odor profile of pasteurized yogurt, which was consistent with the sensory evaluation results. A total of 15 odor-active compounds of 38 volatile compounds were detected in pasteurized yogurt samples. r-OAV results revealed that hexanal, (E)-2-octenal, 2-heptanone, and butanoic acid may be important odor-active compounds responsible for off-odor in aged, pasteurized yogurt samples. PLS-DA and variable importance of projection (VIP) results showed that butanoic acid, hexanal, acetoin, decanoic acid, 1-pentanol, 1-nonanal, and hexanoic acid were differential compounds that distinguish pasteurized yogurt before and after aging.

FAPD: An Astringency Threshold and Astringency Type Prediction Database for Flavonoid Compounds Based on Machine Learning.

Astringency is a puckering or velvety sensation mainly derived from flavonoid compounds in food. The traditional experimental approach for astringent compound discovery was labor-intensive and cost-consuming, while machine learning (ML) can greatly accelerate this procedure. Herein, we propose the Flavonoid Astringency Prediction Database (FAPD) based on ML. First, the Molecular Fingerprint Similarities (MFSs) and thresholds of flavonoid compounds were hierarchically clustering analyzed. For the astringency threshold prediction, four regressions models (i.e., Gaussian Process Regression (GPR), Support Vector Regression (SVR), Random Forest (RF), and Gradient Boosted Decision Tree (GBDT)) were established, and the best model was RF which was interpreted by the SHapley Additive exPlanations (SHAP) approach. For the astringency type prediction, six classification models (i.e., RF, GBDT, Gaussian Naive Bayes (GNB), Support Vector Machine (SVM), k-Nearest Neighbor (kNN), and Stochastic Gradient Descent (SGD)) were established, and the best model was SGD. Furthermore, over 1200 natural flavonoid compounds were discovered and built into the customized FAPD. In FAPD, the astringency thresholds were achieved by RF; the astringency types were distinguished by SGD, and the real and predicted astringency types were verified by t-Distributed Stochastic Neighbor Embedding (t-SNE). Therefore, ML models can be used to predict the astringency threshold and astringency type of flavonoid compounds, which provides a new paradigm to research the molecular structure-flavor property relationship of food components.

Characterization of the aroma profiles of cold and hot break tomato pastes by GC-O-MS, GC × GC-O-TOF-MS, and GC-IMS.

GC × GC-O-TOF-MS and GC-IMS have attracted increasing attention in complex food flavor analysis due to their high resolution and sensitivity. However, very few studies have attempted to identify the aroma components of tomato pastes through these techniques. Herein, the present study comprehensively characterized the aroma profiles of cold and hot break tomato pastes using SAFE-GC-O-MS, SAFE-GC × GC-O-TOF-MS, and HS-GC-IMS for the first time. A total of 274 volatile compounds were identified, far more than previously reported. About 87 % of these compounds can be identified by GC × GC-O-TOF-MS, exceeding 6 times that of GC-O-MS. Notably, 10 aroma-active compounds and 9 volatiles were identified by GC × GC-O-TOF-MS and HS-GC-IMS for the first time. The AEDA and OAVs results indicated that ß-damascenone, linalool, 3-ethylbutanoic acid, and nonanal were the most powerful aroma-active compounds. These findings will provide deeper insights into improving the sensory quality of tomato paste.

Optimization and Preparation of Tallow with a Strong Aroma by Mild Oxidation.

This study was performed to extract and separate the volatiles with solid-phase microextraction (SPME), and was conducted to analyze volatile odor compounds qualitatively and quantitatively in the production of a strong aroma tallow by mild oxidation. A total of 51 odor compounds were detected in the tallow smelted under different conditions. It was found that the high proportion of aldehydes was an important feature of the aroma components in the oxidized melted tallow, such as 1-hexanal, heptanal, nonanal, octanal, benzaldehyde, etc. Through the determination of various indicators, sensory evaluation, and the gas chromatography-olfaction-mass spectrometry (GC-O-MS) analysis and, in combination with response surface methodology, the optimal process parameters for oxidative smelting of tallow were determined as follows: a reaction temperature of 149.61 °C, a reaction time of 31.68 min, and an airflow rate of 97.44 L/h. The accelerated oxidation test further verified the quality of the oxidized tallow.

Flavor Wheel Construction and Sensory Profile Description of Human Milk.

To explore the flavor characteristics of human milk, we constructed a three-tiered human milk flavor wheel based on 53 sensory descriptors belonging to different sensory categories. Fifteen sensory descriptors were selected using M-value and multivariate statistical methods, and the corresponding references were set up to realize qualitative and quantitative sensory evaluation of the human milk samples. To ensure the accuracy and reliability of the sensory evaluation, the performance of the sensory panelists was also tested. The sensory profile analysis indicated that the established sensory descriptors could properly reflect the general sensory properties of the human milk and could also be used to distinguish different samples. Further investigation exposed that the fat content might be an important factor that influence the sensory properties of human milk. To the best of our knowledge, this is the first report on the flavor wheel of human milk.

Characterization of Key Odor-Active Off-Flavor Compounds in Aged Pasteurized Yogurt by Sensory-Directed Flavor Analysis.

The purpose of this study was to determine the key odor-active compounds contributing to the off-flavor of aged pasteurized yogurt (APY) using sensory-directed flavor analysis. Additionally, different extraction methods were compared to determine their effects on the volatile compounds, including dynamic headspace sampling (DHS), solid-phase microextraction, and stir bar sorptive extraction, and DHS was found to be suitable for this study. The results showed that comprehensive two-dimensional gas chromatography-olfactometry-mass spectrometry analysis (GC × GC-O-MS) had more advantages in separating and identifying the volatile compounds than the traditional GC-O-MS. A total of 17 odor-active compounds were determined in the fresh pasteurized yogurt and APY samples by DHS coupled with GC × GC-O-MS. The dynamic headspace dilution analysis demonstrated that 2-heptanone and hexanal were the most vital components in APY with the highest flavor dilution factor. Furthermore, the spiking and omission experimental results revealed that the odor-active compounds, such as 2-heptanone, butanoic acid, pentanoic acid, hexanal, and (E)-2-heptenal, were the key odor-active off-flavor contributors in APY. Therefore, these compounds could be used as potential indicators to determine the freshness of pasteurized yogurt.

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.

Analysis and Comparison of Aroma Compounds of Brown Sugar in Guangdong, Guangxi and Yunnan Using GC-O-MS.

Guangdong, Guangxi and Yunnan are the three provinces in China that yield the most brown sugar, a brown-red colored solid or powdered sugar product made from sugar cane. In the present study, the differences between odor compounds of brown sugar from Guangdong, Guangxi, and Yunnan provinces in China were compared and analyzed by gas chromatography-olfactometry-mass spectrometry (GC-O-MS). A total of 80 odor compounds, including 5 alcohols, 9 aldehydes, 8 phenols, 21 acids, 14 ketones, 5 esters, 12 pyrazines, and 6 other compounds, were detected. The fingerprint analysis of the brown sugar odor compounds showed 90% similarity, indicating a close relationship among the odor properties of brown sugar in each province. Moreover, the orthogonal partial least squares discriminant analysis (OPLS-DA) was performed to identify the compounds contributing to the volatile classification of the brown sugar from three provinces, which confirmed that OPLS-DA could be a potential tool to distinguish the brown sugar of three origins.

Identification of novel saltiness-enhancing peptides from yeast extract and their mechanism of action for transmembrane channel-like 4 (TMC4) protein through experimental and integrated computational modeling.

Excessive consumption of sodium salt is one of the important inducers of cardiovascular and cerebrovascular diseases. The reduction of physical labor and attention to health make research on low-sodium salt imminent. Ultrafiltration, gel filtration, preparative high-performance liquid chromatography, and liquid chromatography with tandem mass spectrometry were employed for further purification and identification of the salty enhancing peptides in yeast extracts. Moreover, human transmembrane channel-like 4 (TMC4) was constructed and evaluated by computer-based methods, and salt-enhancing peptides were identified based on its allosteric sites. PN, NSE, NE and SPE were further determined to be salty enhancing peptides through sensory evaluation, and their taste mechanism was investigated. The results presented here suggest that silicon screening focused on TMC4 allosteric sites and sensory evaluation experiments can greatly increase the discoverability and identifiability of salty enhancer peptides, and this strategy is the first to be applied to the development of salty enhancer peptides.

Characterization of key aroma-active compounds in Hanyuan Zanthoxylum bungeanum by GC-O-MS and switchable GC × GC-O-MS.

The present study sought to characterize the composition of volatile aroma compounds and key aroma-active compounds of dried Hanyuan Zanthoxylum bungeanum. The volatile aroma compounds were analyzed by the solid-phase microextraction (SPME) combined with gas chromatography-olfactometry-mass spectrometry (GC-O-MS) and two-dimensional comprehensive gas chromatography-olfactometry-mass spectrometry (GC × GC-O-MS). The key aroma-active compounds were analyzed by the aroma extract dilution analysis and odor activity value. A total of 72 volatile compounds were identified by GC-O-MS, of which 28 were aroma-active. Meanwhile, 116 volatile compounds were identified by GC × GC-O-MS, of which 43 were aroma-active. These results revealed that myrcene, (+)-limonene, (E)-ß-ocimene, ß-cubebene, Germacrene D, cineole, linalool, and linalyl acetate were the key aroma-active compounds of dried Hanyuan Zanthoxylum bungeanum.

Reduction of sodium chloride: a review.

Sodium chloride (NaCl) is an enjoyable condiment. However, evidence is accumulating to indicate that an excessive intake of Na+ in food may lead to an increased risk of cardiovascular and cerebrovascular diseases. Previous systematic reviews have focused on replacing NaCl with other metal salts (e.g. KCl). However, new salty flavor enhancers (yeast extract, taste peptides, and odor compounds) have yet to be reviewed. This systematic review evaluates the methods for, and feasibility, of NaCl reduction. It defines NaCl reduction and considers the methods used for this purpose, especially the use of flavor enhancers (yeast extract, taste peptides, and odor compounds). © 2022 Society of Chemical Industry.

Detection of odor difference between human milk and infant formula by sensory-directed analysis.

Infants who accustomed to consume human milk can hardly adapt to the odor of infant formula in a short time and prefer the odor of human milk. In this study, the sensory-directed analysis was used to investigate the odor differences between human milk and infant formula. Aroma extraction dilution analysis (AEDA) results showed that carbonyl compounds and alcohols were the most important components with the higher dilution factors (FD) in human milk and infant formula. There were 14 key aroma active compounds (OAV ≥ 1) in human milk, like octanal, linalool, benzaldehyde, and furfural, while 11 in infant formula, like hexanal, 1-octen-3-one, (E)-2-octenal, and octanal. The aroma recombination and omission experiment further revealed that compounds such as (E)-2-decenal, linalool, 2-furanmethanol, 2-pentylfuran, (E,E)-2,4-heptadienal, nonanal, (E)-2-nonenal, and 1-octen-3-one were the major reason for the odor difference between human milk and infant formula.

Characterization of odor-active compounds in moso bamboo (Phyllostachys pubescens Mazel) leaf via gas chromatography-ion mobility spectrometry, one- and two-dimensional gas chromatography-olfactory-mass spectrometry, and electronic nose.

The leaf of moso bamboo (Phyllostachys pubescens Mazel) is rich in odorant compounds, which is important natural materials for the production of flavor. It also contains phenolic acids, amino acids and peptides, which is a potential source of natural bioactive compounds. The study of odor-active compounds in bamboo leaves can provide a basis for the discovery of natural flavor. The leaf, stem, and powder of moso bamboo were analyzed by gas chromatography-ion mobility spectrometry (GC-IMS). Main odor-active compounds in moso bamboo leaf were analyzed and characterized by (1) a gas chromatography olfactory mass spectrometry (GC-O-MS), (2) two-dimensional gas chromatography olfactory mass spectrometry (GC × GC-O-MS) and (3) electronic nose (E-nose). Based on aroma extract dilution analysis (AEDA), 13 key odor-active compounds with high flavor dilution (FD) factor (≥27), including 3-methyl-1-butanol, (E)-2-hexenal, ethyl hexanoate, (Z)-4-heptenenal, 6-methyl-5-hepten-2-one, octanal, ethyl (Z)-3-hexenoate, 1-hexanol, (Z)-3-hexen-1-ol, (E, E)-2,4-heptadienal, (Z)-2-hexen-1-ol, 1-octen-3-ol and benzaldehyde, were further analyzed. The compounds detected by the above four methods were (E)-2-hexenal, 6-methyl-5-hepten-2-one, octanal, (E, E)-2,4-heptadienal, 1-octen-3-ol and benzaldehyde, and all of which were the main and potential odorants of moso bamboo leaf.

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.