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HS-SPME
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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JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE · 2023 ·Vol. 103 ·期 15 ·7631-7642 · IF 4.1

Simultaneous qualitative and quantitative analyses of volatile components in Chinese honey of six botanical origins using headspace solid-phase microextraction and gas chromatography–mass spectrometry

Dongshuang Liang,Haosong Wen,Yaxuan Zhou,Taohong Wang,Guangqun Jia,Zongyan Cui,Adan Li

Background Honey aroma is one of its most important properties and it depends on the qualitative and quantitative composition of the volatile compounds. The volatile profile of honey could reveal its botanical origin to avoid a false characterization. Thus, it is of great significance to honey authentication. This study developed and validated a headspace solid-phase microextraction and gas chromatography–mass spectrometry (HS-SPME-GC–MS) method for simultaneous qualitative and quantitative analyses of 34 volatile components in honey. The developed method was applied to 86 honey samples from six different botanical origins, including linden honey, rape honey, jujube honey, vitex honey, lavender honey and acacia honey. Results The volatile fingerprints and quantitative results were simultaneously obtained by using the full scan and selected ion monitoring (SCAN+SIM) MS scanning mode. The limits of quantification (LOQs) and limits of detection (LODs) of 34 volatile compounds were in the ranges of 1–10 ng/g and 0.3–3 ng/g, respectively. And the spiked recoveries ranged between 70.6% and 126.2%, with the relative standard deviations (RSDs) not higher than 45.4%. A total of 98 volatile compounds were found with relative contents determined, and the 34 volatile compounds were determined with absolute concentrations. Based on the volatile fingerprints and the contents of volatile compounds, honey samples from six botanical origins were well classified by principal component analysis and orthogonal partial least-squares discrimination analysis. Conclusions The HS-SPME-GC–MS method was successfully applied to achieve the volatile fingerprints of six types of honey and to quantitatively analyze 34 volatile compounds with satisfying sensitivity and accuracy. Chemometrics analysis showed significant correlations between honey types and volatiles. These results reveal the characteristics of volatile compounds in six types of unifloral honey and provide some supports for honey authentication. © 2023 Society of Chemical Industry.

研究领域: 食品科学 · 分析化学
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Food Analytical Methods · 2020 ·Vol. 14 ·期 3 ·616-630 · IF 2.667

Gas Chromatography-Mass Spectrometry Analysis as a Tool to Reveal Differences Between the Volatile Compound Profile of Royal Jelly Produced from Tea and Pagoda Trees

Qi Dandan,Ma Chengying,Wang Wenwen,Zhang Licui,Li Jianke

Royal jelly produced by nurse bees from tea tree (tea royal jelly) is a special bee product in China and it is popular with consumers owing to its multiple healthcare functions. However, the volatile compound profile of tea royal jelly has not been investigated. To obtain a comprehensive understanding of volatile compound profile of tea royal jelly, a method based on headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME/GC-MS) and chemometric analysis was applied. Moreover, two royal jelly samples produced from pagoda tree were also investigated to reveal the difference in volatile compounds between royal jelly produced from tea tree and other plants. A total of 66 volatile compounds were identified in tea royal jelly, including 16 alkanes, 14 aldehydes, 9 alcohols, 9 ketones, 8 esters and lactones, 5 phenols, 2 organic acids, and 3 other compounds, and most of them were discovered in royal jelly for the first time. Notably, α -ionone, an important aroma compound in tea, was first identified in tea royal jelly. Moreover, the result of chemometric analysis indicates a significant difference on volatile compound profile between royal jelly produced from tea and pagoda trees. To sum up, 35 differential compounds were identified and they could well distinguish royal jelly samples. Our data offers the first characterization of volatile compound profile of tea royal jelly and significantly expands the knowledge of volatile compounds in royal jelly. It is potentially useful as a new approach to distinguish royal jelly produced from different botanical origins. Graphical abstract

CAS / MDL: 100-51-6 100-52-7
研究领域: 食品科学 · 化学分析 · 蜂产品研究
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Plants-Basel · 2023 ·Vol. 12 ·期 2 ·308 · IF 4.5

Volatile Metabolome and Aroma Differences of Six Cultivars of Prunus mume Blossoms

Ting Li,Xi Zhao,Xueli Cao

Prunus mumeis a traditional Chinese plant with high ornamental and application values due to its very early blooming and unique fragrance. Long-term breeding and cultivation have resulted in a variety ofP. mumeblossoms and have made their exploitation more possible. Existing studies on the volatile metabolome and aroma ofP. mumeblossoms are limited. In this study, six extensively planted cultivars ofP. mumeblossoms, including Gulihong (GLH), Yudie (YD), LvE (LE), Dongfang Zhusha (DFZS), Jiangmei (JM), and Gongfen (GF), were investigated for their differences in terms of volatile metabolome, as well as their aroma characteristics based on the strategies and methods of metabolomics. The volatile metabolites were analyzed using HS-SPME-GC-MS technique. A total of eighty-nine compounds were detected and sixty-five of them were tentatively identified, including thirty-seven phenylpropanoids/benzenes, seventeen fatty acid derivatives, ten terpenoids, and one other compound. YD contains the most volatile metabolites in terms of number and amounts, which impart more abundant aromas to this cultivar. Fifteen differential compounds were screened through the untargeted metabolic analysis of twenty-nine samples by principal component analysis (PCA) and partial least squares-discriminant analysis (PLS-DA), while nine compounds were screened based on the odor activity value (OAV) analysis of the sixty-five identified compounds. GLH and GF, JM and LE were found to be more similar to each other based on chemometrics analysis of both volatile contents and OAVs, while YD and DFZS were markedly different from other cultivars. Six main metabolites, including benzaldehyde, methyl benzoate, benzyl acetate, eugenol, (E)-cinnamic alcohol, and 4-allylphenol, together with 2-nonenal, 3,4-dimethoxytoluene, and trans-β-Ionone were screened as differential compounds, owing to their higher contents and/or lower olfactory threshold, which endow an almond, cherry, phenolic, wintergreen, cananga odorata, floral, jasmine, hyacinth, cinnamon, clove, woody, medicinal, and violet fragrance to each variety, and greatly contribute to the aroma differences of six cultivars ofP. mumeblossom.Keywords:aroma;HS-SPME-GC-MS;Prunus mumeblossom;untargeted metabolomics;volatile metabolome

研究领域: 植物学 · 代谢组学 · 农学
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2018 · IF 3.129

Effects of hot and cold-pressed processes on volatile compounds of peanut oil and corresponding analysis of characteristic flavor components

Qian Dun,Lei Yao,Zeyuan Deng,Hongyan Li,Jing Li,Yawei Fan,Bing Zhang

The volatile compounds were concentrated from hot-pressed and cold-pressed peanut oils by HS-SPME and were analyzed by GC-MS-O. In the present study, 101 volatiles were identified in the hot-pressed peanut oil samples, mainly including pyrazines, aldehydes, furans, alcohols and pyrroles, of which characteristic flavor compounds present fresh, fatty, nutty and baking flavor. Sixty-four volatiles were obtained from the cold-pressed peanut oil samples, mainly consisting of aldehydes, alcohols, hydrocarbons, furans and ketones, of which characteristic flavor compounds show fresh and nutty flavor. Our results indicated that hot-pressed peanut oil has an advantage over cold-pressed peanut oil in the retention of flavor components. Hence, the process method has a significant effect on the flavor components of peanut oil, and the present study may be helpful in evaluating peanut oil quality, as well as discrimination of hot-pressed and cold-pressed peanut oil.

研究领域: 食品科学 · 分析化学
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Food Science and Technology · 2020 ·Vol. 40 ·期 4 ·786-793 · IF 1.443

Optimization of a headspace solid-phase microextraction method for the gas chromatography-mass spectrometry analysis aroma compounds of Litsea mollis Hemsl. immature fruit

YANG Yi-Ni,LIANG Miao,YANG Yan,ZHENG Fu-Ping,WANG Xing-Ping,YU Ai-Nong

This study optimized using a headspace solid-phase microextraction (HS-SPME) method for extracting volatile aroma compounds, terpenoids in particular, from Litsea mollis Hemsl. immature fruit (LMIF). Gas chromatography-mass spectrometry was used to separate and identify volatile terpenoids in LMIF. The types of SPME fiber coating, salt addition, and desorption time were optimized by single factor-experiments to determine the range of extraction temperature. Built on insights from the single factor-experiments, the response surface methodology was further used to optimize the extraction temperature, extraction time, and equilibrium time of HS-SPME. The results showed that the optimal HS-SPME conditions for extracting volatile terpenoids from LMIF were: 50/30 μm of DVB/CAR/PDMS SPME fiber, 2.0 g of added sodium chloride, desorption at a temperature of 250 °C for 3 min, extraction and equilibrium temperature of 46 °C, extraction time of 36 min, and equilibrium time of 20 min. Under the above conditions, the predicted value of extraction was 66.92, while the experimental value was 65.78. The prediction value matched well with the experimental value with good repeatability. The designed model was proven to be valid, which can be applied for future extraction of aroma compounds from IMIF.

CAS / MDL: 64-17-5
研究领域: 植物化学 · 分析化学
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2025 · IF 6.6

Aroma profiling by HS-SPME/GC-MS of black tea produced from different leaf grades

Yang-bo Xiao,Rongji Tian,Ying-ying Shen,Han Tang,Jian-an Huang,Wenliang Wu,Shu-guang Zhang,Xia Yin

Leaf grade is a critical factor influencing black tea aroma formation, yet the precise relationship between leaf grade and aroma characteristics, along with their key volatile compounds, remains unclear. This study employed sensory evaluation combined with headspace solid phase microextraction/gas chromatography-Mass spectrometry (HS-SPME/GC-MS), odor activity values (OAV), partial least squares (PLS) regression, and correlation analysis to investigate the association between leaf grades and aroma attributes, as well as their key volatile compounds. Sensory evaluation and quantitative analysis revealed that as fresh tea leaf grade decreased, the sweet aroma attribute gradually declined, while the floral aroma initially decreased before increasing. GC-MS and OAV analyses identified 22 and 23 differential aroma-active compounds in ‘Jinguanyin’ (JGY) and ‘Jinmudan’ (JMD) black teas of different grades, respectively. Furthermore, PLS modeling and correlation analysis determined that β-damascenone, β-myrcene, geraniol, linalool, and trans -β-ocimene were key compounds responsible for sweet aroma variations across leaf grades, whereas methyl jasmonate, β-ionone, and jasmine lactone were identified as critical compounds influencing floral aroma differences. This study deciphered the chemical basis of how leaf grades affect black tea aroma quality, providing theoretical guidance for precision processing of black tea.

研究领域: 食品科学 · 分析化学 · 感官分析 · 植物生物化学
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Food Chemistry-X · 2024 · IF 6.5

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

Jianfeng Liang,Hailin Wu,Mingfei Lu,Ya Li

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 |Log 2 FC| ≥ 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.

研究领域: 食品科学 · 分析化学 · 植物代谢
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FOOD CHEMISTRY · 2024 · IF 8.5

Temporal analysis of non-targeted flavor component variation in green tea storage and rapid prediction of storage duration

Zhen Wang,Waqas Ahmad,Songguang Zhao,Afang Zhu,Shuhao Huo,Quansheng Chen

The precise changes in the flavor quality of green tea before and after the optimal consumption period remain elusive. This study used HS-SPME-GC–MS to carefully examine the volatile compounds of green tea samples from multiple storage periods and simultaneously detected changes in taste and color during tea infusion. Notably, 16 compounds with VIP > 1.5 were identified, highlighting their significance in the overall analysis profile. Among these components, nonanoic acid, octanoic acid and hexanal were identified as potential contributors to off-flavors and rancid oil flavors in tea after storage. The color of the tea broth becomes darker. Bitter flavor is associated with increased amino acid content. The PSO-SVM model showed excellent accuracy for predicting the storage duration of green tea. These findings provide critical theoretical understandings of green tea manufacturing and quality control.

CAS / MDL: 110-38-3
研究领域: 食品科学 · 茶叶研究 · 分析化学
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FOOD CHEMISTRY · 2023 · IF 8.8

Unravelling dynamic changes in non-volatile and volatile metabolites of pulses during soaking: An integrated metabolomics approach

Lei He,Qian Hu,Liyang Wei,Xuliyang Ge,Ning Yu,Ying Chen

An integrated metabolomics approach based on UPLC-QTOF-MS and HS-SPME-GC-orbitrap-MS was performed to investigate the dynamic changes of metabolite profiling in chickpeas, red speckled kidney beans, and mung beans during soaking. There were 23, 23, 16 non-volatile metabolites, and 18, 21, 22 volatile metabolites were identified as differential metabolites in chickpeas, red speckled kidney beans, and mung beans during soaking, respectively. These metabolites mainly included flavonoids, lysophosphatidylcholines (LPCs), lysophosphatidylethanolamines (LPEs), fatty acids, alcohols, aldehydes, and esters. The key time points responsible for the significant changes in metabolites and quality of the three pulses were 4, 8, and 24 h of soaking. Results revealed that the variations of some metabolites could attribute to oxidation and hydrolysis reactions. These results contribute to a better understanding of how soaking affects pulses quality, and provide useful information for determining soaking time according to nutritional and sensory requirements of their final products or dishes.

研究领域: 食品科学 · 代谢组学 · 植物学
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Journal of Food Measurement and Characterization · 2026 · IF 3.6

Differentiation and characterization of volatile organic compounds from different parts of saffron based on HS-SPME-GC-MS

Zhao Xiaohan,Wang Liling,Yin Xianggang,Wu Linlin,Zheng Ying,Shao Qingsong,Zhou Yifeng,Huang Jun

Saffron ( Crocus sativus L. ) is a valuable perennial bulbous medicinal herb, often referred to as the “golden spice”. Although previous studies have investigated the non-volatile components and bioactive constituents in various parts of saffron, comprehensive profiles of its volatile organic compounds (VOCs) remained limited. This study employed headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) combined with cluster heatmaps, principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA) to analyze and compare the VOCs in seven parts of Zhejiang-cultivated saffron, namely stigma (SS), petal (SP), pollen (SPO), filaments (SF), corms (SC), buds (SB), and leaves (SL). A total of 72 VOCs of saffron were identified, comprising 10 alcohols, 7 esters, 19 ketones, 7 aldehydes, 17 alkenes, and 12 other compounds. Among these, fatty acid methyl esters were the predominant VOC components in SC, whereas safranal or isophorone exhibited relatively higher abundances in the other six parts, which were also enriched in trimethylcyclohexane or cyclohexene derivatives. Cluster heatmaps and PCA grouped the seven saffron parts into three major clusters: SS, SPO and the remaining five parts. Furthermore, 15 significantly differential compounds were screened using the scatter loading plot (S-plot) of the OPLS-DA model combined with variable importance in the projection (VIP) values. Isophorone, 2,2,6-trimethylcyclohexane-1,4-dione (DOIP), and 2,6,6-trimethyl-1,3-cyclohexadiene-1-carbaldehyde (safranal) were identified as common key discriminant compounds across all comparisons, and while SS, SP, SF, SB and SL each contain unique marker compounds. These findings provide a scientific foundation for the authentication, quality assessment and comprehensive utilization of saffron resources.

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LWT-FOOD SCIENCE AND TECHNOLOGY · 2019 · IF 3.714

Chemical composition and biological activities of essential oil isolated by HS-SPME and UAHD from fruits of bergamot

Chen Xing,Chunqing Qin,Xueqing Li,Fuming Zhang,Robert J. Linhardt,Peilong Sun,Anqiang Zhang

Bergamot essential oil (BEO), which is extracted from bergamot fruit peel, has many health benefits such as improving blood circulation and anticancer activity. In this paper, volatile components were obtained by headspace solid phase microextraction (HS-SPME) and ultrasound-assisted hydrodistillation (UAHD) from the fruits of bergamot ( Citrus medica L. var. sarcodactylis (Noot.) Swingle). The oil yield of BEO from UAHD extraction was 0.48%, which is 118% higher than that of hydrodistillation (HD). The chemical compositions of the volatile components were analyzed using GC-MS. A total of 46 volatile compounds belonging to distinct chemical families were identified. The major components were identified as d -limonene (60.44%), γ-terpinene (20.28%). The biological activities, including antimicrobial activities and antioxidant activities of BEO were detected. The BEO exhibited activities against bacteria and fungi with minimal inhibitory concentration (MIC) values in the range of 0.78–3.13 μL/mL and minimum bactericidal or fungicidal concentration (MBC/MFC) values in the range of 1.56–6.25 μL/mL. BEO showed strong activity against E. coli (MIC = 0.78 μL/mL, MBC = 1.56 μL/mL). BEO also showed substantial antioxidant activity based on ferric reducing antioxidant power (FRAP) assay for reducing power, 2,2′-azino-bis(3-ethyl benzothiazoline-6-sulfonic acid) (ABTS) assay for radical scavenging activity, and superoxide anion radical scavenging activity.

CAS / MDL: 1397-89-3 64-75-5
研究领域: 植物学 · 药理学 · 分析化学
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