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LWT-FOOD SCIENCE AND TECHNOLOGY · 2023 · IF 6

Applying HS-SPME-GC-MS combined with PTR-TOF-MS to analyze the volatile compounds in coffee husks of Coffea arabica with different primary processing treatments in Yunnan

Li Wan,Hong Wang,Xinyuan Mo,Yueping Wang,Lianping Song,Liangyan Liu,Wenjuan Liang

Primary processing treatments are crucial to the flavor profile of coffee beans, which create the flavor precursors basis in coffee husks and diffuse into the beans, with satisfying outcomes. In this study, eleven coffee husks of Coffea arabica with different primary processing treatments (sun exposure, washing and honey treatment) from three latitudes of Yunnan were investigated by the combination of HS-SPME-GC-MS and PTR-TOF-MS. A total of 114 volatile organic compounds (VOCs) and 77 masses were identified. The characteristic compounds octanoic acid ( S1 ) and methyl linoleate ( S11 ) in sun-exposed, phenethyl alcohol ( F4 ), methyl salicylate ( F7 ), 3,5-dimethylbenzaldehyde ( F9 ) and phytone ( T9 ) in washed and n -hexadecanoic acid ( S9 ) of honey-treated husks were recognized by the ions at m/z 33.032, m/z 68.049, m/z 83.049, m/z 67.054, m/z 57.034, m/z 41.030 and m/z 49.010, respectively. This study demonstrated the feasibility and complementarity of HS-SPME-GC-MS and PTR-TOF-MS in the rapid identification of VOCs in coffee husks. Meanwhile, the antioxidant capacities of the 11 husks were evaluated in vitro , and the sun-exposed samples exhibited most promising potency, in which methyl salicylate ( F7 ), methyl linoleate ( S11 ), methyl linolenate ( S13 ), ethyl linoleate ( S14 ), ethyl linolenate ( S16 ), linalool ( T1 ), citronellol ( T2 ) and caffeine ( J3 ) contributed mainly to the antioxidant capacities.

研究领域: 食品科学 · 分析化学 · 农业科学
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FOOD RESEARCH INTERNATIONAL · 2025 · IF 8

Characteristic aroma changes during the sauce-flavoured black pork processing based on HS-SPME-GC-O-MS and aroma recombination/omission experiments of the final product

Jiacheng Li,Cong Li,Xueli Chen,Xianyan Liao,Hui Zhou,Baocai Xu,Li Zhang,Liming Jiang

To understand the characteristic aroma compounds and their changes during the processing of sauce-flavoured black pork (SBP), headspace solid phase microextraction gas chromatography-olfactometry mass spectrometry (HS-SPME-GC-O-MS) was used to determine the volatiles during processing. A total of 63 volatiles were detected during the whole processing, including aldehydes, alcohols, esters, and furans, etc. The aroma characteristics of SBP are meaty, fatty, fruity, and grassy. During the processing, the aroma characteristics gradually shift from grassy and fruity aromas to being dominated by meaty, supplemented by fruity, fatty, and grassy aromas. Further, the impact of 25 characteristic aroma compounds on aroma changes was visualized through co-occurrence network analysis. Specifically, esters showed increasing centrality (network connectivity) in later stages, indicating their dominant role in transitioning aroma from grassy and fruity to meaty dominance. Ten key characteristic aroma compounds of SBP were confirmed based on molecular sensory science methods: isovaleraldehyde, hexanal, phenylacetaldehyde, eucalyptol, linalool, ethyl butyrate, ethyl 2-methylbutyrate, ethyl isovalerate, ethyl hexanoate, and 2-pentylfuran. Esters are the most important contributor to the characteristic aroma of SBP, with significantly higher content (929.34 μg/kg) and aroma character impact (58 %) than aldehydes (662.35 μg/kg, 25 %).

研究领域: 食品科学 · 风味化学 · 分析化学 · 食品加工 · 感官科学
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JOURNAL OF MOLECULAR LIQUIDS · 2024 · IF 5.3

Investigating the interactions between selected heterocyclic flavor compounds and beef myofibrillar proteins using SPME-GC–MS, spectroscopic, and molecular docking approaches

Meng Wei,Xiaochang Liu,Peng Xie,Aiyun Han,Yuanhua Lei,Xiaodong Yang,Yinchu Liu,Songshan Zhang,Baozhong Sun

In this study, the interactions between myofibrillar proteins (MPs) and key heterocyclic flavor compounds, 2-ethyl-6-methylpyrazine, 2-acetylpyrrole, 2-acetyl-thiazole, and 2-acetyl-2-thiazoline, in beef, were investigated using solid phase microextraction (SPME) combined with gas chromatography-mass spectrometry (GC–MS), spectroscopic, and followed by molecular docking. The GC–MS results revealed that the molecular structures of the flavor compounds strongly influenced their binding affinity with MPs. 2-Ethyl-6-methylpyrazine and 2-acetylpyrrole exhibited salting-out effects from the MPs solution, and 2-acetyl-2-thiazoline displayed a higher binding affinity with MPs compared to 2-acetyl-thiazole, indicated by the Hill binding models. Fluorescence static quenching experiments also demonstrated that 2-acetyl-2-thiazoline had a higher Stern–Volmer constant with MPs than 2-acetyl-thiazole. Circular dichroism analysis revealed that increased concentrations of flavor compounds transformed ordered structures in MPs into random coils. This suggests that high molar concentrations of 2-acetyl-thiazole and 2-acetyl-2-thiazoline induced conformational changes in MPs. In accordance with the molecular docking model, hydrogen bonds, van der Waals forces, and hydrophobic interactions were identified as the primary noncovalent interactions between MPs and 2-acetyl-thiazole and 2-acetyl-2-thiazoline. This study provides valuable insights for controlling flavor profiles of beef products.

CAS / MDL: 29926-41-8 24295-03-2
研究领域: 食品科学 · 分析化学 · 分子生物学 · 蛋白质化学
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FOOD RESEARCH INTERNATIONAL · 2020 · IF 4.972

Screening of key flavonoids and monoterpenoids for xanthine oxidase inhibitory activity-oriented quality control of Chrysanthemum morifolium Ramat. ‘Boju’ based on spectrum-effect relationship coupled with UPLC-TOF-MS and HS-SPME-GC/MS

An Peng,Lianzhu Lin,Mouming Zhao

This study aimed at obtaining precise quality control standards to efficiently screen Chrysanthemum morifolium Ramat. ‘ Boju ’ with strong xanthine oxidase (XO) inhibitory activity for developing C. morifolium ‘ Boju ’ extract based-hypouricemic functional food. The results indicated significant differences in volatile and phenolic profiles and XO inhibitory (XOI) activities of 31 batches of C. morifolium ‘ Boju ’ collected in herb/tea market. The minority of C. morifolium ‘ Boju ’ having abundant characteristic monoterpenoids and flavonoid aglycones showed strong XOI activities, while the majority of C. morifolium ‘ Boju ’ possessing few corresponding monoterpenoids and flavonoid aglycones exhibited moderate XOI activities. Seven XOI activity-directly related phenolics and ten XOI activity-indirectly related volatiles were identified by UPLC-ESI-QTOF/MS-based and HS-SPME-GC/MS-based spectrum-effect relationships, respectively. Three flavonoids (luteolin, apigenin and acacetin) identified as key XO inhibitors and four monoterpenoids (filifolone, α-terpineol, thymol and piperitenone) closely related to key XO inhibitors were screened for XOI activity-oriented quality control of C. morifolium ‘ Boju ’.

CAS / MDL: 64-18-6
研究领域: 药理学 · 分析化学 · 植物科学
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2022 · IF 5.895

Accurate Determination of 12 Lactones and 11 Volatile Phenols in Nongrape Wines through Headspace-Solid-Phase Microextraction (HS-SPME) Combined with High-Resolution Gas Chromatography-Orbitrap Mass Spectrometry (GC-Orbitrap-MS)

Yaran Liu,Xu Qian,Jiangtao Xing,Na Li,Junlong Li,Qingyu Su,Yixin Chen,Bolin Zhang,Baoqing Zhu

This paper clarifies the contribution of lactones and volatile phenols to the aroma of nongrape wine. A target method for the simultaneous determination of these two kinds of volatiles in nongrape wines was developed using headspace-solid-phase microextraction (HS-SPME) combined with high-resolution gas chromatography-Orbitrap mass spectrometry (GC-Orbitrap-MS). A high-resolution mass spectrometry database including 12 lactones and 11 volatile phenols was established for qualitative accuracy. Different matrix-matched calibration standards should be prepared for specific samples due to the matrix effects. The method was successfully validated and applied in three nongrape wines. Hawthorn wine contained more lactones (δ/γ-hexalactone, δ/γ-nonalactone, δ/γ-decalactone, γ-undecalactone, δ/γ-dodecalactone, C10 massoia lactone, and whiskey lactone), while blueberry wine contained more volatile phenols (especially 4-vinylguaiacol and 4-ethylguiaiacol). Goji berry wines contained certain concentrations of δ-nonalactone, γ-nonalactone, δ-hexalactone, and 3-ethyl phenol. This study demonstrated that HS-SPME-GC-Orbitrap-MS can be applied for the accurate quantification of trace aroma compounds such as lactones and volatile phenols in fruit wines.

研究领域: 食品科学 · 分析化学 · 农学
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FOOD RESEARCH INTERNATIONAL · 2024 · IF 7

Revealing the characteristic aroma and boundary compositions of five pig breeds based on HS-SPME/GC-O-MS, aroma recombination and omission experiments

Xueli Chen,Haoyue Liu,Cong Li,Yujuan Xu,Baocai Xu

To clarify the characteristic aroma compounds and flavor discrepancies of five Chinese typical pig species, headspace-solid phase microextraction gas chromatography–olfactometry-mass spectrometry (HS-SPME/GC-O-MS), electronic nose (E-nose), aroma recombination and omission experiments were used to analyze the characteristic aroma and boundary of five boiled pork. A total of 38 volatile compounds were identified, of which 14 were identified as important odorants with odor-activity values (OAVs) greater than 1. Aroma recombination and omission experiments revealed 8 key characteristic aroma compounds, which significantly contributed to the overall aroma. Sensory evaluation of the recombination model with the 8 aroma compounds scored 3.0 to 4.0 out of 5 points. 12 potential markers were identified to distinguish by principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA), including (E)-2-octenal, 3-ethyl-2-methyl-1,3-hexadiene, (E)-2-heptenal, 2-pentylfuran, cyclooctanol, 1-heptanol, sec -butylamine, D-limonene, N-vinylformamide, 2,3-octanedione, 2-ethylfuran and 3-pentanamine. Alongside benzaldehyde and pentanal, the combinations and fluctuations of these 14 aroma markers were proposed to constitute the aroma boundaries of different pork breeds. The aroma-active substances were able to effectively differentiate different breeds.

研究领域: 食品科学 · 分析化学 · 农学 · 感官科学
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International Journal of Food Engineering · 2024 · IF 1.6

Qualitative and quantitative analysis for monitoring the fishy odor of anchovy oil

Kaiwen Zheng,Xianqing Luo,Shijun Song,Ruijuan Dong,Pinmei Wang,Bubin Xu,Jinzhong Xu

The fishy odor of fish oil, a popular nutritional supplement, affects its quality as well as consumer acceptance and eating experience. An objective or scientific method for analyzing fish oil’s olfactory characteristics is still lacking. This study examined anchovy oil to develop qualitative and quantitative approaches for identifying fishy odor components. Multiple fish oil refining samples were analyzed using gas chromatography-ion mobility spectrometry (GC-IMS). Due to their significant alterations during fish oil refining, low threshold values, and distinct olfactory properties, the unsaturated aldehydes ( E )-2-pentenal and ( E , E )-2,4-heptadienal and the unsaturated ketone 1-penten-3-one may contribute to the fishy odor. Among the chemicals, ( E , E )-2,4-heptadienal was chosen as the marker for developing a method to quantify fishy odor and analyze deodorization samples using headspace solid-phase micro-extraction gas chromatography-mass spectrometry (HS-SPME-GC-MS). The quantitative study of fishy odor in fish oil is a pioneering approach that can help improve quality assurance and refining process.

CAS / MDL: 4313-03-5
研究领域: 食品科学 · 分析化学 · 营养学
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Vegetable Research · 2024 ·Vol. 4 ·期 1 · IF 0

Detection and analysis of VOCs in chili pepper based on HS-SPME-GC × GC-TOFMS and HS-SPME-GC-MS techniques

Chenxi Ji,Sihui Guan,Chenxu Liu,Chao Yu,Zhuping Yao,Hongjian Wan,Qingjing Ye,Guozhi Zhou,Huasen Wang,Yuan Cheng

Chili pepper (Capsicum annuum L.) is highly preferred by consumers owing to its distinctive flavor. Volatile organic compounds (VOCs) significantly influences the aromatic characteristics of chili peppers, thereby impacting their overall fruit quality. The study of chili pepper aroma remains at a nascent stage, with a notable gap in the literature regarding the composition and metabolic regulation of volatile flavor compounds in fresh chili peppers. This study focuses on the pepper cultivar var 'Qujiao 5' with rich fruit aroma, using headspace solid-phase microextraction full two-dimensional gas chromatography time of flight mass spectrometry (HS-SPME-GC × GC-TOFMS) and headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS) detection technology platforms to analyze the VOCs present in green ripe pepper. A total of 1,558 VOCs were successfully identified. Utilizing the HS-SPME-GC × GC-TOFMS method pinpointed 933 substances, whereas the HS-SPME-GC-MS approach detected 773 compounds. Moreover, the two methods together identified 150 substances. Through the meticulous analysis of relative odor activity values (ROAV), it was conclusively determined that Pyrazine, 2-methoxy-3-(2-methylpropyl)- and 2-Nonenal, (E)- serve as pivotal volatile flavor compounds in chili fruit. Through the analysis of sensory flavor characteristics of chili peppers, it was found that fresh chili peppers have the main aroma characteristics of fatty, green bell pepper, and green, while also possessing modified odors such as floral and sweet. This research undertook a thorough comparative analysis of two different detection methods. It also meticulously examined the compositional and sensory attributes of the pepper VOCs, providing an essential reference for subsequent studies on the development of pepper fruit flavor quality.

研究领域: 植物学 · 食品科学 · 分析化学
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Foods · 2023 ·Vol. 13 ·期 1 ·42 · IF 5.2

Effect of Leaf Grade on Taste and Aroma of Shaken Hunan Black Tea

Kuofei Wang,Yangbo Xiao,Nianci Xie,Hao Xu,Saijun Li,Changwei Liu,Jianan Huang,Shuguang Zhang,Zhonghua Liu,Xia Yin

Shaken Hunan black tea is an innovative Hunan black tea processed by adding shaking to the traditional Hunan black tea. The quality of shaken black tea is influenced by leaf grades of different maturity. In this study, the taste and aroma quality of shaken Hunan black tea processed with different grades were analyzed by sensory evaluation (SP, HPLC, and HS-SPME/GC-MS). The results showed that shaken Hunan black tea processed with one bud and two leaves has the best quality, which has a sweet, mellow, and slightly floral taste, as well as a floral, honey, and sweet aroma. Moreover, caffeine and EGCG were identified as the most important bitter and astringent substances in shaken Hunan black. Combined with the analysis of GC-MS and OAV analysis, geraniol, jasmone, β-myrcene, citral, and trans-β-ocimene might be the most important components that affect the sweet aroma, while methyl jasmonate, indole, and nerolidol were the key components that affect the floral aroma of shaken Hunan black tea. This study lays a foundation for this study of the taste and aroma characteristics of shaken Hunan black tea and guides enterprises to improve shaken black tea processing technology.Keywords:shaken Hunan black tea;leaves grade;taste;aroma;HS-SPME/GC-MS

CAS / MDL: 110-38-3
研究领域: 食品科学 · 茶叶研究
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ACS Omega · 2025 · IF 4.3

Flavor Characteristics of Different Varieties of Flue-Cured Tobacco Based on Headspace Gas Chromatography–Ion Mobility Spectrometry and Headspace Solid-Phase Microextraction–Gas Chromatography–Mass Spectrometry

Xiaoyu Chen,Cong Chen,Yutong Liu,Kun Tang,Mengqi Chen,Jianhua Qiu,Lin Yuan,Hongtao Shen,Zhiyong Wu

In order to investigate characterization and the differences of volatile substances in different types of flue-cured tobacco, the volatile components (VOCs) and relative contents of six varieties of flue-cured tobacco were analyzed by headspace gas chromatography–ion mobility spectrometry (HS-GC-IMS) and headspace solid-phase microextraction–gas chromatography–mass spectrometry (HS-SPME-GC-MS). Combined with the relative odor activity value (ROAV), important flavor substances were determined and different aroma components were screened by multivariate statistical analysis. The results showed that 93 and 80 kinds of compounds, such as esters, alcohols, and aldehydes, were detected by GC-IMS and HS-SPME-GC-MS in six flue-cured tobacco varieties, respectively. A total of 19 volatile flavor compounds, such as benzaldehyde, acetic acid, valeraldehyde, and methyl acetate, were selected as compounds to distinguish the aroma of different toasted tobaccos by orthogonal partial least-squares discrimination analysis (OPLS-DA). In this study, more comprehensive information about volatile flavor components of six flavor types of flue-cured tobacco has been obtained by the synergistic analysis of two distinct analytical instruments. Meanwhile, this study clarified the composition and differences of aroma components of six types of flue-cured tobacco, which lays a foundation for the flavor control of different types of flue-cured tobacco.

CAS / MDL: 13019-20-0
研究领域: 烟草科学 · 分析化学
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JOURNAL OF SEPARATION SCIENCE · 2010 ·Vol. 33 ·期 12 ·1806-1815 · IF 2.551

The use of liquid phase deposition prepared phosphonate grafted silica nanoparticle-deposited capillaries in the enrichment of phosphopeptides

Jian-Hong Wu,Yong Zhao,Ting Li,Cong Xu,Kuang Xiao,Yu-Qi Feng,Lin Guo

In our current work, we describe how open tubular-immobilized metal-ion affinity chromatography (OT-IMAC) capillary columns connected to a solid phase microextraction (in-tube SPME) device can be used for the enrichment of phosphopeptides. A phosphonate modified silica nanoparticle (NP)-deposited capillary was prepared by liquid phase deposition (LPD), and used for the immobilization of Fe 3+ , Zr 4+ or Ti 4+ . The enrichment capacities of three different OT-IMAC capillary columns were compared by using tryptically digested α-casein as sample. The improved extraction efficiency in our technique was demonstrated by comparing to a directly modified capillary, and a comparison of phosphopeptide extraction from simple and complex samples was tested for both modes. Our results show that the NP-IMAC-Zr 4+ capillary column can be used to selectively isolate phosphopeptides from real samples, and can enrich for β-casein phosphopeptides from concentrations as low as 1.7×10 −9 M.

CAS / MDL: 108-75-8 10025-87-3
研究领域: 分析化学 · 蛋白质组学
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MOLECULES · 2022 ·Vol. 27 ·期 9 ·2865 · IF 4.927

Effect of Natural Antioxidants from Marigolds (Tagetes erecta L.) on the Oxidative Stability of Soybean Oil

Xiuqiong Huang,Wei Gao,Xuan Yun,Zhixing Qing,Jianguo Zeng

In recent years, synthetic antioxidants that are widely used in foods have been shown to cause detrimental health effects, and there has been growing interest in antioxidants realised from natural plant extracts. In this study, we investigate the potential effects of natural antioxidant components extracted from the forage plant marigold on the oxidative stability of soybean oil. First, HPLC-Q-TOF-MS/MS was used with 1,1-diphenyl-2-picrylhydrazyl (DPPH) to screen and identify potential antioxidant components in marigold. Four main antioxidant components were identified, including quercetagetin-7-O-glucoside (1), quercetagetin (2), quercetin (3) and patuletin (4). Among them, quercetagetin (QG) exhibited the highest content and the strongest DPPH radical scavenging activity and effectively inhibited the production of oxidation products in soybean oil during accelerated oxidation, as indicated by reductions in the peroxide value (PV) and acid value (AV). Then, the fatty acids and volatile compounds of soybean oil were determined with gas chromatography–mass spectrometry (GC-MS) and headspace solid-phase microextraction–gas chromatography–mass spectrometry (HS-SPME-GC-MS). A total of 108 volatile components, including 16 alcohols, 23 aldehydes, 25 ketones, 4 acids, 15 esters, 18 hydrocarbons, and 7 other compounds, were identified. QG significantly reduced the content and number of aldehydes and ketones, whereas the formation of acids and hydrocarbons was completely prevented. In addition, the fatty acid analysis demonstrated that QG significantly inhibited oxidation of unsaturated fatty acids. Consequently, QG was identified as a potential, new natural antioxidant that is believed to be safe, effective and economical, and it may have potential for use in plant extracts feed additives.Keywords:Tagetes erectaL.;quercetagetin;DPPH-HPLC-Q-TOF/MS;HS-SPME-GC-MS;oxidative stability

研究领域: 植物学 · 食品科学 · 分析化学
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