Headspace Solid-phase Microextraction Gas Chromatography Research Articles

Improving Quality Profiles of Summer-Autumn Tea Through the Synergistic Fermentation with Three Fungal Strains

The co-fermentation of summer-autumn tea with Aspergillus niger and Eurotium cristatum effectively reduces bitterness and astringency, enhances flavor and quality, and increases market appeal and economic value. This study investigated the dynamic changes in metabolites, flavor characteristics and quality indicators of summer-autumn tea during fermentation. Using headspace solid-phase microextraction gas chromatography (HS-SPME-GC-MS), 96 key metabolites were identified, significantly enhancing the tea's aroma and flavor. On the fourth day of fermentation, the content of ester catechins (EGCG, ECG) decreased by 79.44% and 79.57%, respectively, while non-ester catechins (EGC, C, EC) increased by 175.47%, 228.18%, and 138.73%, respectively. Additionally, the gallic acid content increased by 755.58%, along with rises in free amino acids and soluble sugars. Sensory evaluation focused on taste, soup color, and aroma, resulting in a total score of 80.67. The intensity of astringency, bitterness, and sourness in the tea infusion gradually decreased, while sweetness, umami, and aroma intensified. These findings underscore the significant role of the synergistic action of the three strains in developing the unique flavor profile of summer-autumn tea during fermentation. This research lays the foundation for quality control and resource development in the processing of summer-autumn tea.

Characterization of the flavor profile of four major Chinese carps using HS-SPME-GC–MS combined with ultra-fasted gas chromatography-electronic nose

The four major Chinese carps are highly popular for their distinctive nutritional benefits. However, the differences in flavor among these carps remain unclear. This study investigated the flavor profiles of these carps using headspace solid-phase micro-extraction gas chromatography–mass spectrometry (HS-SPME-GC/MS) combined with ultra-fasted gas chromatography electronic nose (GC E-nose). The four major Chinese carps had high protein content (16.68–18.61 %) and low fat levels (0.42–1.29 %). A total of 45 volatile compounds were identified in these carps. Both the GC E-nose and HS-SPME-GC–MS results consistently showed significant flavor profiles differences among these carps, with Ctenopharyngodon Idella (CI) exhibiting the most pronounced distinctions compared to the other three species. Based on VIP >1 and p < 0.05, 10 key compounds including 2-Nonanone, Cyclodecanol, Eugenol, 1,3-Cyclooctadiene, etc., largely contributed to the distinctive overall flavor profile of four major Chinese carps derived mainly from amino acid and fatty acid metabolism.

The dynamic changes and correlations between biochemical properties, flavor and microbial community during fermentation of asparagus by-products

Asparagus by-products are the promising resource that urgently need to be re-valorized. This study investigated the dynamic changes in physicochemical properties, organic acids, free amino acids, volatile flavor compounds, microbial succession, and their correlations during 7-day spontaneous fermentation of asparagus by-products. Dominant organic acids (lactic acid and acetic acid) and free amino acids (Ser, Glu, and Ala) increased with fermentation time, with lactic acid reaching 7.73 ± 0.05 mg/mL and Ser increasing 56-fold after 7 days. A total of 58 volatile flavor compounds were identified using headspace solid-phase microextraction-gas chromatography–mass spectrometry (HS-SPEM/GC–MS), with esters, alcohols and acids as the main volatile flavor compounds. Fourteen volatile flavor compounds had odor activity value >1. High-throughput sequencing showed Firmicutes and Proteobacteria as the main bacterial phyla, dominated by lactic acid bacteria (Levilactobacillus, Lactiplantibacillus, Weissella). Correlation analysis revealed that five bacterial genera (Levilactobacillus, Lactiplantibacillus, Enterobacter, Pediococcus and Acetobacter) were highly correlated with organic acids, free amino acids, and volatile flavor compounds, indicating their pivotal role in forming the characteristic flavor of fermented asparagus by-products (FAPS). This study provides new insights into the flavor and microbial profile of FAPS, offering a strategy for value-added processing and industrial production.

Changes in volatile flavors during the fermentation of tomato (Solanum lycopersicum L.) juice and its storage stabilization

Flavor is a crucial indicators of the quality of fermented tomato juice; however, there has been limited research in this area. Herein, headspace solid-phase microextraction gas chromatography–mass spectrometry was used to analyze the volatile metabolites at different stages during FTJ fermentation. 131 volatile organic compounds (VOCs) were identified, with alcohols, acids, and esters as the main compounds. The content of superoxide dismutase (SOD) and lycopene (LYC) had a positive correlation with methyl salicylate, ethyl acetate, and linalyl acetate. Subsequently, the storage stability of FTJ was evaluated at temperatures of 4 °C, 25 °C, and 37 °C over a period of 45 d, revealing that the quality of FTJ decreased with increasing storage temperature. The shelf life of FTJ under different storage conditions was determined using SOD activity and LYC content as quality indicators. The final shelf life was 47 d at 37 °C, 69 d at 25 °C, and 123 d at 4 °C.

Chemical profile and in-vitro bioactivities of three types of yellow teas processed from different tenderness of young shoots of Huoshanjinjizhong (Camellia sinensis var. sinensis)

In the present study, bud yellow tea (BYT), small-leaf yellow tea (SYT) and large-leaf yellow tea (LYT) were produced from the same local “population” variety Huoshanjinjizhong (Camellia sinensis var. sinensis), and the effects of raw material tenderness on the chemical profile and bioactivities of these teas were investigated. The results showed that 11 crucial compounds were screened by headspace solid-phase microextraction-gas chromatography–mass spectrometry from 64 volatiles in these yellow teas, among which the heterocyclic compounds showed the greatest variations. In addition, 43 key compounds including organic acids, flavan-3-ols, amino acids, saccharides, glycosides and other compounds were screened by liquid chromatography-mass spectrometry from 1781 non-volatile compounds. BYT showed the best α-glucosidase inhibitory activity and antioxidant capacity among the selected yellow teas, which might be contributed by the higher content of galloylated catechins. These findings provided a better understanding of the chemical profile and bioactivities of yellow teas.

HS-SPME-GC-MS untargeted metabolomics reveals key volatile compound changes during Liupao tea fermentation

This study used headspace solid-phase microextraction-gas chromatography–mass spectrometry and multivariate statistical analysis to comprehensively analyze the volatile components in Liupao tea samples throughout fermentation. In total, 1009 volatile organic compounds were detected and identified, including terpenoids, heterocyclic compounds, esters, ketones, hydrocarbons, alcohols, aromatics, and acids. Principal component and hierarchical cluster analyses, characterize the volatile components of Liupao tea samples were characterized at various fermentation stages. Orthogonal partial least squares discriminant analysis identified 248 differentiating compounds (VIP ≥ 1, P < 0.05, and |Log2FC| ≥ 1.0) during fermentation. K-means clustering analysis showed that 11 metabolites increased significantly throughout the fermentation process, whereas 31 metabolites decreased continuously. Annotation of these differential compounds revealed significant changes in sensory flavor characteristics in “green, sweet, fruity, floral, and woody” flavors. The results demonstrated significant variations in the volatile components of Liupao tea fermentation, along with notable changes in flavor characteristics.

Comparison and identification of aroma components in 21 kinds of frankincense with variety and region based on the odor intensity characteristic spectrum constructed by HS–SPME–GC–MS combined with E-nose

Frankincense is an important seasoning and spice known for its distinctive and intricate flavor profile. Considering the considerable variation in the aromatic quality of frankincense due to geographical origin, species diversity and cultivation conditions, frankincense from major global origins was characterized holistically for the first time. The electronic nose (E-nose) with headspace solid-phase microextraction gas chromatography–mass spectrometry (HS–SPME–GC–MS) and sensory evaluation were implemented to characterize the aroma components of 21 commercial varieties of frankincense from around the world. The results showed that a total of 149 volatile organic compounds (VOCs) of 10 categories were identified in frankincense, among which the numbers of alcohols, terpenes and esters compounds accounted for 22.15 %, 18.79 % and 15.44 % of the total VOCs of frankincense, respectively. The PLS-DA model effectively distinguished frankincense from Oman/Somalia and other origins. Furthermore, the study identified two differential VOCs with VIP > 1 in three Asian countries and five in six African countries. The total VOCs content and sensory characteristic score of “Lemon/Citrus” in Oman frankincense is significantly higher than other regions. The OAV results showed that 61 substances (e.g., Diacety, alpha-Pinene, Camphene, Myrcene) as key aroma compounds and OICS model indicated that p-Cymenol was found to contribute significantly to the citrus aroma in frankincense. This study identified the fundamental components of frankincense flavor and revealed different flavor descriptors of frankincense, which are crucial for reconstructing frankincense flavor and improving flavor quality.

An Evaluation of Pig Type Regarding the Quality of Xuanwei Ham

To determine the influence of pig type (Landrace, Wujin, or Tibetan fragrant) on the quality of Xuanwei ham, we measured the ham pH, color, fat content, and moisture content; used an E-nose (a device intended to detect odors or flavors); and analyzed flavoring substances using headspace solid-phase microextraction–gas chromatography, free amino acids using high-performance liquid chromatography, and microbial diversity using high-throughput sequencing. The ham types differed from each other in these attributes. The moisture and fat contents of Landrace pig ham were significantly lower than those of the other pig types, the brightness values of the Tibetan fragrant pig ham were significantly lower than those of the other pig types, and the redness values of the Landrace and Wujin pig hams were significantly higher than those of the Tibetan fragrant pig ham. The essential amino acid contents, e-wind odor response values, and volatile flavor substances of Wujin pig hams were significantly higher than those of the Tibetan fragrant pig ham, and the relative aldehyde contents of Wujin pig ham were significantly higher than those of the other pig types. The dominant microbial phyla in each ham type were assessed based on the species commonness, composition, and diversity and included taxa such as Actinobacteria and Ascomycetes and thick-walled bacteria such as Orphanomyces, Grass Spirochaetes, and Pseudoalteromonas. The microbial diversity and richness were the greatest in the Wujin pig ham. Of the three pigs, we conclude that the Wujin pig produces the best Xuanwei ham.

Effect of gamma irradiation on sensory and aroma compounds of soaked bayberry jiu

Soaked bayberry jiu is a homely fruit alcoholic beverage that produced by soaking bayberry in Baijiu, a traditional Chinese distilled spirit. To investigate the changes in the sensory and aroma compounds of soaked bayberry jiu following gamma irradiation, the sensory evaluation, electron nose, electron tongue, and headspace solid-phase microextraction gas chromatography mass spectrometry (HS-SPME-GC-MS) were conducted. The results showed that the different irradiation doses of samples could be well separated. The taste and smell of 6 kGy irradiated soaked bayberry jiu were significantly improved, but the color of irradiated samples was deteriorated. Moreover, a total of 53 differential products (21 decreased and 32 increased products) were detected compared 6 kGy irradiated soaked bayberry jiu to unirradiated sample, including some important aroma compounds of Baijiu, indicating that the active free radicals produced by gamma irradiation promote the oxidation-reduction reaction in soaked bayberry jiu and lead to the mutual transformation and equilibrium among the compounds. These findings suggest that gamma irradiation can improve the quality of soaked bayberry jiu.

Characterization of the volatile flavor profiles of black garlic using nanomaterial-based colorimetric sensor array, HS-SPME-GC/MS coupled with chemometrics strategies

This work investigated the feasibility of applying headspace solid phase microextraction-gas chromatography–mass spectrometry (HS-SPME-GC/MS) combining olfactory visualization for flavor characterization of black garlic. Volatile organic compounds (VOCs) analysis was performed to select important differential VOCs during black garlic processing. A multi-channels nanocomposite CSA assembled with two porous metal-organic frameworks was then developed to characterize flavor profiles changes during black garlic processing, and garlic samples during processing could be divided into five clusters, consistent with VOCs analysis. Artificial neural network (ANN) model outperformed other pattern recognition methods in discriminating processing stages. Furthermore, SVR model for odor sensory scores with the correlation coefficient for prediction set of 0.8919 exhibited a better performance than PLS model, indicating a preferable prediction ability for odor quality. This work demonstrated that the nanocomposite CSA combining appropriate chemometrics can offer an effective tool for objectively and rapidly characterizing flavor quality of black garlic or other food matrixes.

Dynamic changes in the aroma profiles and volatiles of Enshi Yulu tea throughout its industrial processing

Although Enshi Yulu tea (ESYL) possesses a distinctive fragrance, there is a scarcity of studies focusing on its primary volatiles or aroma genesis. This study aims to elucidate the dynamics in the profiles of aromas and volatiles through aroma profiling analysis and headspace solid–phase microextraction/gas chromatography–mass spectrometry. A total of 10 aroma attributes and 128 volatiles were identified in ESYL, with geraniol and linalool exhibiting the highest levels, and alcohols constituting the predominant proportion. Besides, a relative odor activity value (ROAV) based molecular aroma wheel was constructed, revealing 12 key odorants with ROAVs >1, wherein linalool, β-ionone, and nonanal ranked highest. Notably, steaming and final drying emerged as critical steps for ESYL aroma development, while the non-enzymatic degradation of fatty acids likely contributed to the formation of its fresh aroma. These findings significantly enhance our comprehension of ESYL aroma formation.

Sensory and chemical characterization of chestnuts processed in different methods using instrumental analyses and the Check-all-that-apply method

Chestnuts are known for their unique sensory characteristics and nutritional value. However, the changes in their sensory attributes after processing remain unclear. This study used instrumental analysis and sensory evaluation combined with multivariate statistical analysis to investigate the effect of packaging and thermal sterilization procedures on the sensory characteristics of chestnuts. The results showed that the significant variations (p < 0.05) between the different processing methods for chestnuts were revealed via the texture analysis, headspace solid-phase microextraction gas chromatography × gas chromatography-time of flight-mass spectrometry (HS-SPME-GC×GC-TOF-MS), and check-all-that-apply (CATA) sensory evaluation. The packaging had a more significant influence on the sensory quality of the chestnuts than thermal sterilization procedures. The HS-SPME-GC×GC-TOF-MS identified 116 volatile compounds, and the partial least squares-discriminant analysis (PLS-DA) identified the 28 volatile compounds responsible for the similarities and differences among different processing methods of chestnuts. Principal component analysis (PCA) combined with texture analysis and the fingerprint of HS-SPME-GC×GC-TOF-MS, as well as the correspondence analysis (CA) analysis of CATA, could discriminate samples from different packaging of chestnuts. This study provides chestnuts processing recommendations for satisfying consumer preferences and predicting possible related quality changes.

Screening and tentatively identifying of volatile hazards of desiccant and deoxidizer in food package

Food desiccant and deoxidizer are becoming more prevalent in food preservation, where they keep food in good quality for longer periods of time by absorbing moisture and oxygen. In such a way that they are in direct contact with the food inside the food package. However, their safety is still unclear and they must be fully screened and identified. In this study, the volatiles in five representative desiccants and two deoxidizers in the market were screened and tentatively identified by headspace solid-phase microextraction gas chromatography coupled with mass spectrometry (HS-SPME-GC-MS), compared with NIST spectral libraries, and combined with manual analysis. Specific migration limits are provided in accordance with EU NO 10/2011. Risk classes are predicted for substances lacking toxicological data through toxtree software. More than half of the substances were initially screened with toxicological data, seven with specific migration limits, three Cramer III substances, the remainder being Cramer I substances and substances with no risk level. The high-risk substances were further analyzed and traced back to their potential sources. However, there are a few substances for which the potential sources are still unclear and require further research. Despite this, this study has established the safety of desiccant and deoxidizer for use in food to a large extent, providing a solid basis for the future development of the industry.

Correlation between physicochemical properties, flavor characteristics and microbial community structure in Dushan shrimp sour paste

Dushan shrimp sour paste (DSSP), a traditional Guizhou condiment, and its unique flavor is determined by the fermentation microbiota. However, the relationship between the microbiota structure and its flavor remains unclear. This study identified 116 volatile flavor compounds using electronic nose and headspace solid-phase microextraction-gas chromatography mass spectrometry (HS-SPME-GC–MS) techniques, of which 19 were considered as key flavor compounds, mainly consisting of 13 esters and 1 alcohol. High-throughput sequencing technique, the bacterial community structure of nine groups of DSSPs was determined. Further analysis revealed Vagococcus, Lactococcus, and Tepidimicrobium as key bacteria involved in flavor formation. This study contributes to our understanding of the relationship between bacterial communities and the flavor formation, and provides guidance for screening starter culture that enhance the flavor of DSSP in industrial production.

Volatile flavor behavior characterization of Hericium erinaceus during postharvest storage using E-nose, HS-GC-IMS, and HS-SPME-GC–MS after treated with electron-beam generated X-ray irradiation

Flavor alteration is a crucial factor affecting the quality of mushrooms during preservation. The dynamic variations of volatile profiles of fresh Hericium erinaceus with electron-beam generated X-ray irradiation were investigated by combining E-nose, headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS), and headspace solid-phase microextraction gas chromatography–mass spectrometry (HS-SPME-GC–MS). E-nose analysis achieved rapid discrimination in all treatments over storage time. 65 and 73 volatile organic compounds (VOCs) were identified by HS-GC-IMS and HS-SPME-GC–MS, respectively. Thereinto, 1-octen-3-ol, 1-octen-3-one, and 2-octanone were screened out as the characteristic VOCs, which contents declined during storage. While the contents of (E)-2-octenal, (E)-2-nonenal, and 1-octanol increased. The flavor profile changes from distinct mushroom and floral odor to an intense alcohol and fatty odor. Notably, one-kGy irradiation remained more volatiles and denser mushroom odor after storage. Multivariate analysis further confirmed that 1.0 kGy irradiation contributed to the overall aroma retention during postharvest storage of H. erinaceus.

Influence of germination and roasting on the characteristic volatile organic compounds of quinoa using sensory evaluation, E-nose, HS-GC-IMS, and HS-SPME-GC-MS

This study aimed to investigate the effects of germination and roasting on the flavor of quinoa. Firstly, the aroma of quinoa and germinated quinoa roasted under different conditions was analyzed using sensory evaluation and electronic nose (E-nose). Results showed that the best favorable aroma of quinoa and germinated quinoa was obtained when roasted at 160 °C for 15 min. Then, a total of 34 and 80 volatile organic compounds (VOCs) of quinoa and germinated quinoa roasted at 160 °C for 15 min were determined using headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS) and headspace solid-phase microextraction gas chromatography–mass spectrometry (HS-SPME-GC–MS), respectively. Germination and roasting effectively reduced the contents of VOCs that produced undesirable flavor. Moreover, germination improved the floral aromas, while roasting mainly produced caramel, cocoa, and roasted nut aromas of quinoa. This study indicated that germination and roasting treatments might serve as promising processing methods to improve the flavor of quinoa.

Characterization of Key Aroma Compounds and Main Contributing Amino Acids in Hot-Pressed Oil Prepared from Various Peanut Varieties.

The production of peanut oil in the industrial sector necessitates the utilization of diverse raw materials to generate consistent batches with stable flavor profiles, thereby leading to an increased focus on understanding the correlation between raw materials and flavor characteristics. In this study, sensory evaluations, headspace solid-phase micro-extraction gas chromatography mass spectrometry (HS-SPME-GC-MS), odor activity value (OAV) calculations, and correlation analysis were employed to investigate the flavors and main contributing amino acids of hot-pressed oils derived from different peanut varieties. The results confirmed that the levels of alcohols, aldehydes, and heterocyclic compounds in peanut oil varied among nine different peanut varieties under identical processing conditions. The OAVs of 25 key aroma compounds, such as methylthiol, 3-ethyl-2,5-dimethylpyrazine, and 2,3-glutarone, exceeded a value of 1. The sensory evaluations and flavor content analysis demonstrated that pyrazines significantly influenced the flavor profile of the peanut oil. The concentrations of 11 amino acids showed a strong correlation with the levels of pyrazines. Notably, phenylalanine, lysine, glutamic acid, arginine, and isoleucine demonstrated significant associations with both pyrazine and nut flavors. These findings will provide valuable insights for enhancing the sensory attributes of peanut oil and selecting optimal raw peanuts for its production.

Identification of key off-flavor compounds during storage of fried pepper (Zanthoxylum bungeanum Maxim.) oils by sensory-directed flavor analysis and partial least squares regression (PLSR)

Fried pepper oil (FPO) is a widely used flavoring oil in China, but it suffers from complex chemical reactions that give an unpleasant odor. The aim of this paper is to study the main causes of off-flavor in FPO, as well as identify key off-flavor compounds in FPO. Fifty-eight volatiles were identified using HS-SPME–GC–MS (headspace solid-phase microextraction–gas chromatography–mass spectrometry) during storage. Fifteen off-flavor compounds were initially targeted by odor activity values (OAVs) calculations and partial least squares regression (PLSR) analysis. Eventually, five key off-flavor compounds were identified by recombination experiments and omission test, which were hexanal, (E)-2-octenal, terpinyl acetate, α-terpineol, and hexanoic acid. The off-flavors could derive from the oxidative degradation of long-chain fatty acids and the acid-catalyzed rearrangement of terpenes. The results of the study provide a theoretical basis for the regulation of off-flavor in FPO and a practical guide for the industrial production of FPO.

Analysis of Three Dimethyl Sulfides in Freshwater Lakes Using Headspace Solid-Phase Microextraction-Gas Chromatography with Flame Photometric Detection

Dimethyl sulfides are ubiquitous odorous substances in eutrophic freshwater bodies. In this study, a simple headspace solid-phase microextraction-gas chromatography-flame photometric detection method was developed to detect three representative algal-derived dimethyl sulfides in freshwater lake water samples: dimethyl monosulfide (DMS), dimethyl disulfide (DMDS), and dimethyl trisulfide (DMTS). The effects of extraction fiber, temperature, pH, ionic strength, and sample volume were investigated orthogonally, and the optimized method was applied to analyze surface water samples from Lake Ulansuhai in Inner Mongolia, China. Optimal extraction was obtained with a 50/30 µm DVB/CAR/PDMS extraction fiber, 20% ion concentration, 87 min extraction time, and 50 °C extraction temperature. The correlation coefficients of the standardized working curves for DMS, DMDS, and DMTS were 0.9967, 0.9907, and 0.9994, respectively, indicating good linear relationships. Limits of detection were in the nanogram range, and the recoveries of the spiked standards for DMS, DMDS, and DMTS were 97.22~99.07%, 93.39~99.34%, and 91.17~99.25%, with relative standard deviations of 5.18~5.94%, 3.08~6.25%, and 2.56~5.47%, respectively. This method is stable and reliable, and can be used for the determination of volatile sulfides in freshwater lake water.

Improvement mechanism of volatile flavor in fermented tilapia surimi by cooperative fermentation of Pediococcus acidilactici and Latilactobacillus sakei: Quantization of microbial contribution through influence of genus

Single starter can hardly improve the volatile flavor of fermented fish surimi. In this study, the changes of volatile compounds (VCs) and microbial composition during cooperative fermentation of Latilactobacillus sakei and Pediococcus acidilactici were studied by headspace solid-phase microextraction gas chromatography–mass spectrometry and 16S rRNA gene high-throughput sequencing. During cooperative fermentation, most VCs and the abundance of Latilactobacillus and Lactococcus significantly increased, while Pediococcus, Acinetobacter, and Macrococcus obviously decreased. After evaluation of correlation and abundance of each genus, Latilactobacillus and Lactococcus possessed the highest influence on the formation of volatile flavor during cooperative fermentation. Compared with the natural fermentation, cooperative fermentation with starters significantly enhanced most of pleasant core VCs (odor activity value≥1), but inhibited the production of trimethylamine and methanethiol, mainly resulting from the absolutely highest influence of Latilactobacillus. Cooperative fermentation of starters is an effective method to improve the volatile flavor in the fermented tilapia surimi.