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JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS · 2019 · IF 3.47

Diverse impact of α-Fe2O3 with nano/micro-sized shapes on the catalytic fast pyrolysis of pinewood: Py-GC/MS study

Adel Baimoldina,Konstantinos Papadikis,Elena Yu. Konysheva

The feasibility of α-Fe 2 O 3 catalyst addition in the in-situ catalytic fast pyrolysis of Pinewood was considered with the focus on the variation in its shape: nano-sized non-ideal spheres, nanotubes, hollow nano/microtubes, and octadecahedral crystals. Nano-sized spheres strongly promoted the formation of acetaldehyde, something that was also observed for the octadecahedral crystals. The formation of acids was primarily facilitated through the addition of nanotube catalysts and octadecahedral crystals. Newly formed alicyclic ketonic compounds were promoted through the addition of nano-sized spheres, hollow nano/microtubes, and octadecahedral crystals. The latter two catalysts also showed a moderate selectivity in the formation of furfural. All applied catalysts showed loss of activity, though at different degrees, on the formation of lignin derived phenolic compounds, which can be primarily attributed to favoring the formation of char with simultaneous release of CO 2 . All used α-Fe 2 O 3 catalysts with different shapes maintained their original morphology after the rapid heating with the rate of 20 K/ms followed by catalytic fast pyrolysis at 500 °C, indicating that nanomaterials with targeted dimensions can be applied as catalysts in the catalytic fast pyrolysis of biomass to enhance conversion of undesired oxygenated compounds to higher quality bio-oil and valuable chemicals.

CAS / MDL: 1309-37-1 7681-49-4
研究领域: 催化 · 生物质能源 · 分析化学 · 材料科学
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INDUSTRIAL CROPS AND PRODUCTS · 2024 · IF 5.6

Unraveling the flavor variation mechanism of wheat bran insoluble dietary fibers during different dynamic solid-state fermentation patterns: identification via E-nose, GC-MS, and GC-IMS combination with fingerprinting

Wei Liang,Qian Lin,Wenqing Zhao,Xinyue Liu,Rong Ma,Teng Zhang,Jie Zeng,Haiyan Gao,Wenhao Li

To investigate the influence of microbes on flavor attributes during solid-state fermentation of wheat bran insoluble dietary fiber (IDF), this study constructed CK (unfermented IDF), NF (native fermented IDF), YF (yeast fermented IDF), LF ( Lactobacillus plantarum fermented IDF) and MF (mixed fermented IDF) systems and studied their flavor profiles change during dynamic processes (12–48 h). The E-nose results indicated that the sensor response values of flavor compounds in the samples were increased as fermentation progressed (especially in the YF and MF groups). Also, the GC-MS findings verified that co-fermentation promoted flavor release and enhanced compound species. Cluster analysis validated E-nose results, while O2PLS-DA selected 8 flavor compounds with prominent VIP scores. Moreover, GC-IMS verified the differences in flavor formation in IDF, confirming a more balanced fermentation hypothesis in MF. Also, the fingerprints were compared and differentiated in the distribution of the 75 flavor compounds featured in different fermentation groups. This flavor formation and conversion pattern may be attributed to synthesizing and releasing flavor compounds during co-fermentation by degrading bran and utilizing its products. The production of this complex flavor is related to its components' interactions. Obtained results are expected to enhance whole grain flavored food development and high-value utilization of IDF.

研究领域: 食品科学 · 微生物学
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ANALYTICAL LETTERS · 2025 · IF 1.8

Determination of Trace Ethephon in Fruit by Catalytic Methylation with (Trimethylsilyl) Diazomethane (TMSD) and Gas Chromatography-Mass Spectrometry (GC-MS)

Yunna Li,Fan Qi,Jinsong Liu,Yunfei Zhao,Jiale Fang,Xueliang Li,Kezhi Jiang

Ethephon (ETH) is a widely used plant growth regulator in fruit production. Due to its harm to people’s health, its content is an important indicator for fruit quality control. However, due to the extremely high polarity and acidity, as well as the absence of chromophores, efficient and simple detection of ETH remains challenging. In this work, a convenient method for determining trace ETH in fruit was developed that involved a combination of catalytic methylation and gas chromatography-mass spectrometry (GC-MS) analysis. ETH in fruit was extracted with acetonitrile and derivatized with (trimethylsilyl) diazomethane (TMSD) by the catalysis of trimethylchlorosilane to generate methylated ETH (ETH-M) which was determined by GC-MS. The instrumental linear range of ETH was 10–1000 µg/L with a coefficient of determination (R2) > 0.999. The limit of detection (LOD) of the method was 1.0 µg/kg. The ETH content in 12 types of fruits was determined with a reasonable recovery rate ranging from 83.20 ± 0.05% to 118.21 ± 0.01%. The ETH content in the unwashed fruits was in the range of undetectable (ND) to 111 µg/g and below the LOD in their flesh. After washing, the content was significantly reduced and even undetectable. The established method showed good efficiency, selectivity, and reproducibility, and can be used for the determination of ETH in various fruits.

CAS / MDL: 75-77-4 34819-78-8
研究领域: 分析化学 · 食品安全 · 植物生长调节剂 · 环境与农业化学
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Polymers · 2025 ·Vol. 17 ·期 17 ·2421 · IF 4.9

Determination of Odor Compounds in Lignocellulose-Based Panels Using DHS-GC/MS Combined with Odor Activity Value Analysis

Lina Tang,Qian Chen,Liming Zhu,Xiaorui Liu,Xianwu Zou,Yuejin Fu,Bo Liu

Wood, as the oldest natural polymer composite material on Earth, holds significant importance in the era of carbon neutrality and serves as an irreplaceable core material in the furniture and construction industries. As a primary raw material for furniture, wood-based lignocellulosic boards have drawn increasing consumer attention due to their odor characteristics. In order to achieve the determination of odor compounds in lignocellulose-based panels, this study established a method combining dynamic headspace sampling (DHS), gas chromatography–mass spectrometry (GC–MS), and odor activity value (OAV) analysis. To address the wide concentration range of odor compounds in lignocellulose-based panels, a three-level standard curve was established to meet the detection of odor substances in common lignocellulose-based panels. The favorable conditions for each factor were as follows: sheet-shaped samples, TENAX-TA adsorbent, 20 mL headspace vials, and a split ratio of 25:1. The method demonstrated good linearity within the range of 0.002–15 mg/m3, with recovery rates ranging from 94.74% to 103.44%. The method was applied to analyze commercially available particleboard, fiberboard, and plywood. A total of 33 odor components were detected. The results indicated that aldehyde contributed significantly to the odor of particleboard, acids were the main contributors to the odor of fiberboard, and terpenes dominated the odor of plywood. The established method is suitable for the qualitative and quantitative analysis of odor compounds in lignocellulose-based panels and provides reliable technical support for tracing, identifying, and controlling odors in these materials.

CAS / MDL: 67-56-1
研究领域: 木材科学与技术 · 分析化学 · 室内空气质量 · 材料气味分析 · 可持续材料
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FOOD CHEMISTRY · 2023 · IF 8.8

GC–MS and LC-MS/MS metabolomics revealed dynamic changes of volatile and non-volatile compounds during withering process of black tea

Xin Fang,Yanan Liu,Jingyi Xiao,Cunqiang Ma,Youyi Huang

High-performance liquid chromatography (HPLC), headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC–MS) and ultra-high performance liquid chromatography–Q-Exactive HF-X mass spectrometer (UHPLC–Q-Exactive HF/MS) were carried out to reveal dynamic changes of volatile and non-volatile compounds during the withering process of black tea. A total of 118 volatile organic compounds (VOCs) and 648 metabolites were identified in fresh and withered tea-leaves, respectively. Among them, 47 VOCs (OAV > 1.0) for the aroma formation, and 46 characteristic metabolites (VIP > 1.50, p  < 0.01) selected through orthonormal partial least squares-discriminant analysis, indicated the withering contribution during black tea processing. Overall, the withering promoted alcohols, aldehydes, phenols, heterocyclic oxygen, hydrocarbons and halogenated hydrocarbons through relevant hydrolyzation, decomposition, terpene synthesis, and O -methylation. The hydrolyzation, O -methylation, condensation and N -acylation of kaempferol glycosides, quercetin glycosides, ester catechins, and gallic acid generated the accumulation of methoxyl flavonoids and flavonoid glucosides, dihydrokaempferol, syringic acid, theaflavins, and N -acylated amino acids, respectively.

研究领域: 食品科学 · 农学 · 化学 · 代谢组学 · 茶叶加工
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2022 · IF 6.056

Identification of volatile and odor-active compounds in Hunan black tea by SPME/GC-MS and multivariate analysis

Xia Yin,Jian'an Huang,Jing Huang,Wenliang Wu,Tong Tong,Shujuan Liu,Lingyun Zhou,Zhonghua Liu,Shuguang Zhang

Hunan black tea is well-known for its floral-honey aroma, but the volatile components responsible for the fragrance have not been elucidated yet. In this study, the volatile compounds in Hunan black tea were identified and quantified by the headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME-GC-MS). The results showed that 88 compounds were extracted and determined in Hunan black tea, including the dominant components Geraniol, phenethyl alcohol, phenylacetaldehyde, linalool, nonanal and other 5 aromatic compounds. Furthermore, the aroma-active compounds were identified by odor activity value (OAV). It was found that 24 aroma compounds, including geraniol with an OAV≥1 were regarded as the primary active aromatic compounds in Hunan black tea. Finally, partial least squares (PLS) regression analysis was employed and results revealed that Nonanal, trans -nerolidol, benzyl alcohol, and phenylethanol exhibit a positive correlation with the intensity of floral and sweet honey aromas. Overall, this study identified the volatile compounds responsible for the dominant floral-honey aroma in Hunan black tea.

研究领域: 食品科学 · 分析化学 · 农学
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Foods · 2023 ·Vol. 12 ·期 14 ·2656 · IF 5.2

Difference in Volatile Aroma Components of Stropharia rugosoannulata under Two Cultivated Environments Investigated by SPME-GC-MS

Yanbin Wang,Dan Wu,Yingqi Wu,Xiaoqing Tong,Yuchuan Qin,Liling Wang

In order to study the effect of both greenhouse and forest cultivating environments onStropharia rugosoannulata, its volatile aroma compounds were measured by a headspace solid phase micro extractions—gas chromatograph—mass spectrometer (SPME–GC–MS). The optimal adsorption temperature was 75 °C and the optimal adsorption time was 40 min. A total of 36 volatile aroma compounds were identified by GC–MS, including 8 aldehydes, 2 ketones, 4 alcohols, 15 alkenes, and 4 alkanes. Hexanal, 3-Octanone, 2-Undecanone, (E)-Nerolidol, and (Z)-β-Farnesene made great aromatic contributions. Among them, Hexanal, 3-Octanone, 2-Undecanone were the key aroma compounds for which odor activity values (OAVs) were more than 1. (E)-Nerolidol showed odor modification in the forest samples and showed a key aroma effect in greenhouse samples. (Z)-β-Farnesene showed odor modification in greenhouse samples. 3-Octanone was the largest contributing compound for which the OAV was more than 60. The total content of volatile aroma compounds first increased and then decreased with growth time; it reached the highest level at 48 h: 2203.7 ± 115.2 μg/kg for the forest environment and 4516.6 ± 228.5 μg/kg for the greenhouse environment. The aroma was the most abundant at this time. All samples opened their umbrella at 84 h and become inedible. Principal component analysis (PCA), hierarchical cluster analysis (HCA), and orthogonal partial least squares discriminant analysis (OPLS–DA) were combined to analyze the aroma difference ofS. rugosoannulataunder two cultivation modes. PCA and HCA could effectively distinguish the aroma difference in different growth stages. Under different culturing methods, the aroma substances and their changes were different. The samples were divided into two groups for forest cultivation, while the samples were divided into three groups for greenhouse cultivation. At the end of growth, the aroma ofS. rugosoannulatawith the two cultivation modes was very similar. OPLS–DA clearly distinguished the differences between the two cultivation methods; 17 key aroma difference factors with variable importance projection (VIP) > 1 were obtained from SPLS–DA analysis.Keywords:Stropharia rugosoannulata;cultivation mode;volatile aroma compounds;mushroom;gas chromatography—mass spectrometry

研究领域: 食品科学 · 分析化学 · 真菌学
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FOOD CHEMISTRY · 2024 · IF 8.5

Identification and selection of volatile compounds derived from lipid oxidation as indicators for quality deterioration of frozen white meat and red meat using HS-SPME-GC–MS combined with OPLS-DA

Ligang Yu,Ying Pang,Guang Shen,Baoqing Bai,Yukun Yang,Maomao Zeng

This work aimed to investigate the effects of frozen storage on volatile compounds of white meats (chicken and duck) and red meats (pork, beef, and mutton). The samples were stored at −18 °C for 0, 2, 4, 10, 18 weeks, and volatile compounds were analyzed by headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry. Results indicated that the total amounts of volatile compounds increased with frozen storage duration of meats. The correlations were observed between frozen storage duration and levels of 2-ethyl-1-hexanol, tetradecane, nonanal, decanal, octanal, tridecanal, benzaldehyde, pentadecane, propanoic acid,2-methyl-,3-hydroxy-2,2,4-trimethylpentyl ester, heptadecane, and hexanal ( r  = 0.7456–0.9873). Levels of octanal and propanoic acid,2-methyl-,3-hydroxy-2,2,4-trimethylpentyl ester in white meat and benzaldehyde in red meat versus frozen storage duration fitted very well with zero-order reactions. Therefore, it was concluded that changes in volatile compounds derived from lipid oxidation may be used as indicators of quality deterioration during frozen storage of meat.

CAS / MDL: 13019-20-0
研究领域: 食品科学 · 分析化学
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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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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2022 · IF 3.571

A sensitive and accurate GC–MS method for analyzing microbial metabolites short chain fatty acids and their hydroxylated derivatives in newborn fecal samples

Fangbo Xia,Lishan Guo,Peng Cui,Qian Xu,Junda Huang,Hongwei Zhou,Wei Shen

Short chain fatty acids (SCFAs), crucial intestinal bacterial metabolites , have been widely accepted as potential diagnostic markers in neonatal medicine. Nevertheless, it is still a great challenge to accurately quantify SCFAs in newborn fecal samples due to the huge variation of water content, limited commercial isotope-labeled internal standards and poor sensitivity. In this study, Na 2 CO 3 solution (50 μg/mL) was applied to convert the free SCFAs to SCFA sodium salts, which could prevent the loss of violate SCFAs during lyophilization process. Furthermore, N-methylbenzylamine- d 0 / d 3 was applied as the chemical derivatization regent to enhance the sensitivity and accuracy. Based on this method, the SCFA contents in meconium and neonatal fecal samples were analyzed to illustrate the change of SCFAs during the gut microbiome development. Chemical derivatization based on N-methylbenzylamine- d 0 / d 3 could not only significantly promote the sensitivity (323–1280 folds compared to free SCFAs) by promoting the ionization efficiency, but also provide one-to-one isotope internal standards. Moreover, 7 SCFAs, including acetic acid ( 2 ), n-butyric acid ( 4 ), isobutyric acid ( 5 ), 2-hydroxybutyric acid ( 11 ), 2-hydroxy-3-methylbutyric acid ( 13 ), 3-hydroxybutyric acid ( 14 ), 2-hydroxy-2-methylbutyric acid ( 17 ) were found to be significantly increased in neonatal fecal samples compared to the meconium fecal samples. All these results proved that this method could be applied for SCFA analysis in newborn fecal samples with perfect accuracy and sensitivity.

CAS / MDL: 148893-10-1 121-44-8
研究领域: 分析化学 · 微生物学 · 新生儿学 · 代谢组学
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Analytical Methods · 2016 ·Vol. 8 ·期 23 ·4727-4735 · IF 1.915

Characterization of the aromatic profile in “zijuan” and “pu-erh” green teas by headspace solid-phase microextraction coupled with GC-O and GC-MS

Chaojun He,Xiangmeng Guo,Yumin Yang,Yanfu Xie,Fengyang Ju,Wenbo Guo

Aroma volatiles from zijuan and pu-erh green teas were extracted by headspace solid-phase microextraction (HS-SPME). They were then characterized and identified using gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS). The conditions of HS-SPME, including fiber selection and optimization of sampling conditions, have been previously investigated. Under optimal conditions, 51 and 42 aroma-active compounds were detected and characterized in zijuan and pu-erh green tea samples, respectively. Alcohols, ketones, and hydrocarbons were qualitatively the most dominant aroma-active compounds in zijuan and pu-erh green teas. The aroma-active compounds with similar sensory descriptors were grouped into the same category, and the sum of individual aroma intensity values within each category showed that the “floral” aroma, “woody” aroma, and “fruity” aroma in both zijuan and pu-erh green teas were the major aroma categories. These aroma notes were closely related to the characteristics of green tea aroma and its sensory perception.

研究领域: 食品科学 · 分析化学 · 茶叶科学
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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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