GC×GC-TOFMS

GC × GC - TOFMS
  • 文章类型: Journal Article
    加工技术在茶叶香气的形成中起着至关重要的作用。利用先进的分析技术,如GC-E-Nose,精心跟踪了新鲜香味绿茶(FSGT)不同加工阶段的挥发性代谢物的动态变化。GC-MS,和GC×GC-TOFMS。通过GC-MS和GC×GC-TOFMS共鉴定出244种挥发性代谢产物,其中两种方法同时检测到37种挥发性化合物。扩展和固定阶段被认为是形成FSGT中挥发性成分的关键过程。值得注意的是,芳樟醇,庚醛,2-戊基呋喃,非肛门,β-月桂烯,己醛,2-庚酮,戊醛,1-octen-3-ol,通过结合气味活性值评估,强调了1-辛醇是FSGT香气特征的主要贡献者。此外,脂质降解和糖苷水解是FSGT香气形成的主要途径。结果不仅阐明了挥发性代谢物的复杂变化,而且还为增强加工技术以改善绿茶的香气质量提供了有价值的见解。
    Processing technology plays a crucial role in the formation of tea aroma. The dynamic variations in volatile metabolites across different processing stages of fresh scent green tea (FSGT) were meticulously tracked utilizing advanced analytical techniques such as GC-E-Nose, GC-MS, and GC × GC-TOFMS. A total of 244 volatile metabolites were identified by GC-MS and GC × GC-TOFMS, among which 37 volatile compounds were concurrently detected by both methods. Spreading and fixation stages were deemed as pivotal processes for shaping the volatile profiles in FSGT. Notably, linalool, heptanal, 2-pentylfuran, nonanal, β-myrcene, hexanal, 2-heptanone, pentanal, 1-octen-3-ol, and 1-octanol were highlighted as primary contributors to the aroma profiles of FSGT by combining odor activity value assessment. Furthermore, lipid degradation and glycoside hydrolysis were the main pathways for aroma formation of FSGT. The results not only elucidate the intricate variations in volatile metabolites but also offer valuable insights into enhancing the processing techniques for improved aroma quality of green tea.
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  • 文章类型: Journal Article
    为了全面了解不同类型乌苏里山梨的挥发性成分并评估其香气特征。安利,Dongmili,华盖,Janbali,京百里,金乡水,通过顶空固相微萃取(HS-SPME)和二维气相色谱/飞行时间质谱(GC×GC-TOFMS)进行检测。香气成分,总香气含量,不同香气类型的比例和数量,并对各化合物的相对量进行分析和评价。结果表明,在不同品种中检测到174种挥发性香气化合物,主要包括酯类,酒精,醛类,和烯烃:金香水的总香气含量最高,为2825.59ng/g;南果里的香气种类最高,为108种。梨品种的香气成分和含量各不相同,根据主成分分析将梨分为三组。检测到24种香气;其中,水果和脂肪族是主要的香味类型。不同品种的香气种类比例也不同,直观、定量地显示不同品种梨香气成分变化带来的整体香气变化。这项研究有助于进一步研究挥发性化合物的分析,为果实感官品质的提高和育种工作提供了有用的数据。
    To comprehensively understand the volatile compounds and assess the aroma profiles of different types of Pyrus ussuriensis Maxim. Anli, Dongmili, Huagai, Jianbali, Jingbaili, Jinxiangshui, and Nanguoli were detected via headspace solid phase microextraction (HS-SPME) coupled with two-dimensional gas chromatography/time-of-flight mass spectrometry (GC×GC-TOFMS). The aroma composition, total aroma content, proportion and number of different aroma types, and the relative quantities of each compound were analyzed and evaluated. The results showed that 174 volatile aroma compounds were detected in various cultivars, mainly including esters, alcohols, aldehydes, and alkenes: Jinxiangshui had the highest total aroma content at 2825.59 ng/g; and Nanguoli had the highest number of aroma species detected at 108. The aroma composition and content varied among pear varieties, and the pears could be divided into three groups based on principal component analysis. Twenty-four kinds of aroma scents were detected; among them, fruit and aliphatic were the main fragrance types. The proportions of aroma types also varied among different varieties, visually and quantitatively displaying changes of the whole aroma of the different varieties of pears brought by the changes in aroma composition. This study contributes to further research on volatile compound analysis, and provides useful data for the improvement of fruit sensory quality and breeding work.
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  • 文章类型: Journal Article
    威士忌,白兰地,朗姆酒,中国白酒是全球流行的蒸馏酒,挥发性成分在这些蒸馏酒的香气中起着至关重要的作用。威士忌中的挥发性化合物,白兰地,朗姆酒,和中国白酒的三种主要香气类型(浓烈,光,和酱汁)使用全面的二维气相色谱-飞行时间质谱(GC×GC-TOFMS)进行了研究。两种重要的变量检测方法,投影中的变量重要性(VIP)和非参数检验(Mann-WhitneyU检验),进行了比较,以确定这些样品中的挥发性标志物。发现VIP模型在筛选显著变体方面比U检验更有效。通过VIP和U测试方法共选择了117个具有潜在香气贡献的常见标记。酯和酸是白酒的主要香气标记,二乙酯是白兰地的主要香气标记,其中吡嗪,内酯,呋喃是威士忌的主要香气标志。根据选择的标记,在模型验证中成功分类了不同的未知蒸馏液.该研究为基于GC×GC-TOFMS获得的挥发性成分的烈酒样品推测提供了可行的方法。
    Whisky, brandy, rum, and Chinese baijiu are popular distilled spirits globally, and the volatile components play an essential role in the aroma of these distilled liquors. Volatile compounds in whisky, brandy, rum, and three main aroma types of Chinese baijiu (strong, light, and sauce) were investigated using comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS). Two significant variable detection approaches, the variable importance in the projection (VIP) and nonparametric test (Mann-Whitney U test), were compared to determine the volatile markers among these samples. It was found that the VIP model was more efficient in screening significant variants than the U test. A total of 117 common markers were selected by both the VIP and U test methods with potential aroma contributions. Esters and acids were the main aroma markers for baijiu, diethyl esters were the main aroma markers for brandy, whereras pyrazines, lactones, and furans were the main aroma markers for whisky. Based on the chosen markers, different unknown distilled liquors were successfully classified in the model validation. This study provided a feasible methodology for spirit sample speculation based on volatile composition obtained by GC×GC-TOFMS.
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  • 文章类型: Journal Article
    加工是绿茶香气品质的关键因素。在这项研究中,利用气相色谱电子鼻(GC-E-Nose)研究了栗香绿茶整个生产过程中香气的动态变化,气相色谱-离子迁移谱(GC-IMS),和全面的二维气相色谱耦合飞行时间质谱(GC×GC-TOFMS)。GC-IMS鉴定出33种挥发性化合物,而GC×GC-TOFMS鉴定出211种挥发性成分。干燥对栗香绿茶的挥发性成分影响最大,并促进了在焙烧阶段通常通过美拉德反应产生的杂环化合物和硫化合物的产生。大量的杂环化合物,如1-甲基-1H-吡咯,吡咯,甲基吡嗪,糠醛,2-乙基-5-甲基吡嗪,1-乙基-1H-吡咯-2-甲醛,和3-乙酰吡咯在干燥过程中新形成。这项研究还验证了GC-E-Nose与GC-IMS和GC×GC-TOFMS结合用于跟踪整个制造过程中绿茶挥发性成分变化的适用性。
    Processing is the crucial factor for green tea aroma quality. In this study, the aroma dynamic changes throughout the manufacturing process of chestnut-like aroma green tea were investigated with gas chromatography electronic nose (GC-E-Nose), gas chromatography-ion mobility spectrometry (GC-IMS), and comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOFMS). GC-IMS identified 33 volatile compounds while GC × GC-TOFMS identified 211 volatile components. Drying exerted the greatest influence on the volatile components of chestnut-like aroma green tea, and promoted the generation of heterocyclic compounds and sulfur compounds which were commonly generated via the Maillard reaction during the roasting stage. A large number of heterocyclic compounds such as 1-methyl-1H-pyrrole, pyrrole, methylpyrazine, furfural, 2-ethyl-5-methylpyrazine, 1-ethyl-1H-pyrrole-2-carboxaldehyde, and 3-acetylpyrrole were newly formed during the drying process. This study also validated the suitability of GC-E-Nose combined with GC-IMS and GC × GC-TOFMS for tracking the changes in volatile components of green tea throughout the manufacturing process.
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  • 文章类型: Journal Article
    “余味”对白酒的质量和消费者偏好至关重要。开发了一种口腔固相微萃取(SPME)结合全面的二维气相色谱-飞行时间质谱(GC×GC-TOFMS)的方法,用于白酒的口腔香气物质监测。提取时间,sip体积和冲洗时间为120秒,5mL,10秒,分别。该方法在浓度为1.56μg/L-1500mg/L的白酒中对不同香气化合物表现出良好的性能(大多数R2>0.9)。此外,优化的程序检测到85种具有不同化学结构的芳香化合物,并提供了良好的光表现,坚强,酱油和混合香气型白酒的口腔香气概况。主成分分析(PCA)累积解释率为72.42%。该程序的可接受性能可以与动态感官评价相结合,以提高白酒香气的质量。
    The \'\'after-odor\" is essential to the quality and consumer preference of Baijiu. An intra-oral solid-phase microextraction (SPME) combined with comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-TOFMS) was developed for oral aroma compounds monitoring of Baijiu. The extraction time, sip volume and rinse time were 120 s, 5 mL, and 10 s, respectively. The procedure showed good performances at concentrations of 1.56 μg/L-1500 mg/L for different aroma compounds of Baijiu (most R2 > 0.9). Furthermore, the optimized procedure detected 85 aroma compounds with different chemical structures and provided good representations of the light, strong, soy sauce and mix aroma type Baijiu\'s oral aroma profiles. Principal component analysis\'s (PCA) cumulative interpretation rate was 72.42%. The acceptable performance of this procedure can be combined with dynamic sensory evaluation to improve the quality of the Baijiu aroma.
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  • 文章类型: Journal Article
    五粮液白酒是中国最著名的白酒之一,具有受保护的地理标志。这项研究使用基于LiChrolut®EN的固相萃取(SPE)和分馏结合全面的二维色谱-飞行时间质谱(GC×GC-TOFMS)来揭示其挥发性成分。用基于LiChrolut®EN的SPE和传统的液-液萃取(LLE)分离挥发物。将来自LLE和SPE的中性/碱性级分在LiChrolut®ENSPE柱上分馏,并通过综合GC×GC-TOFMS进行分析。与LLE相比,在基于SPE的萃取中检测到更多的酯和醇。SPE分馏和GC×GC-TOFMS分析在五粮液白酒的3000多个峰中鉴定出大约500种挥发性化合物。该方法将复杂的白酒成分简化为基于官能团的馏分,以进行可靠的鉴定和分析。本研究提供了一种基于SPE分馏GC×GC-TOFMS的中国白酒挥发性成分置信度鉴定方法。
    Wuliangye baijiu is one of the most famous Chinese liquors with a protected geographical indication. This study used LiChrolut® EN-based solid-phase extraction (SPE) and fractionation combined with comprehensive two-dimensional chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) to unveil its volatile composition. The volatiles were isolated with LiChrolut® EN-based SPE and traditional liquid-liquid extraction (LLE). The neutral/basic fractions from LLE and the SPE were fractionated on a LiChrolut® EN SPE column and analyzed by comprehensive GC×GC-TOFMS. Compared with LLE, more esters and alcohols were detected in the SPE-based extraction. The SPE fractionation and GC×GC-TOFMS analysis resulted in the identification of about 500 volatile compounds in more than 3000 peaks of the Wuliangye baijiu. The approach simplifies the complex baijiu composition into functional group-based fractions for reliable identification and analysis. This study provided a confidence volatile identification approach for Chinese baijiu based on the SPE fractionation GC×GC-TOFMS.
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  • 文章类型: Journal Article
    工业应用中使用的数千种有机物质最终会进入土壤,并可能对人类健康产生负面影响。由于分析限制,通常在环境介质中监测有限数量的目标污染物。在这项研究中,开发了一种通过二维气相色谱高分辨率飞行时间质谱法快速分析污染区(化工园区)的多个土壤样品的非目标筛选方法。通过数据简化和视觉评估,初步分析了土壤样品中存在的化合物类型。选取化工园区样品中检测频率≥40%的有机化合物81种进行鉴定,包括38种PAHs,26含氧有机化合物,八种含N化合物,和其他九种化合物。研究了工业园区中有机化合物的潜在来源。土壤中的一些药物和有机合成中间体受到附近化工厂的影响。在评估相对丰度和检测频率后,初步确定了36种可能对环境构成潜在风险的污染物。研究结果有助于评估洋口工业园区周围的环境风险,对评估其他污染区域的风险也有帮助。
    Thousands of organic substances that are used in industrial applications ultimately enter the soil and may negatively affect human health. Limited numbers of target pollutants are usually monitored in environmental media because of analytical limitations. In this study, a non-target screening method for quickly analyzing multiple soil samples from a contaminated area (a chemical industry park) by two-dimensional gas chromatography high-resolution time-of-flight mass spectrometry was developed. The types of compounds present in the soil samples were preliminarily analyzed through data simplification and visual assessment. A total of 81 organic compounds with detection frequencies ≥40% in the samples from the chemical industry park were selected for identification, including 38 PAHs, 26 oxygenated organic compounds, eight N-containing compounds, and nine other compounds. Potential sources of the organic compounds in the industrial park were investigated. Some pharmaceutical and organic synthetic intermediates in the soil were affected by nearby chemical plants. After assessing the relative abundances and detection frequencies, 36 pollutants that may pose potential risks to the environment were preliminarily identified. The results of the study were helpful for assessing environmental risks around Yangkou industrial park and they will be helpful when assessing risks in other contaminated areas.
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  • 文章类型: Journal Article
    The detection of trace aroma compounds in samples with complex matrices such as Chinese liquor (Baijiu) requires a combination of several methods, which makes the analysis process very complicated. Therefore, a headspace solid-phase microextraction (HS-SPME) method coupled with two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS) was developed for the quantitation of a large number of trace compounds in Baijiu. Optimization of extraction conditions via a series of experiments revealed that dilution of the alcohol content of 8 mL of Baijiu to 5%, followed by the addition of 3.0 g of NaCl and subsequent SPME extraction with DVB/CAR/PDMS fiber coating over 45 min at 45 °C was the most suitable. To check the matrix effects, various model Baijiu matrices were investigated in detail. The quantitative method was established through an optimized model synthetic solution, which can identify 119 aroma compounds (esters, alcohols, fatty acids, aldehydes and ketones, furans, pyrazines, sulfur compounds, phenols, terpenes, and lactones) in the Baijiu sample. The developed procedure provided high recovery (86.79-117.94%), good repeatability (relative standard deviation < 9.93%), high linearity (R2 > 0.99), and lower detection limits than reported methods. The method was successfully applied to study the composition of volatile compounds in different types of Baijiu. This research indicated that the optimized HS-SPME-GC×GC-TOFMS method was a valid and accurate procedure for the simultaneous determination of different types of trace compounds in Baijiu. This developed method will allow an improved analysis of other samples with complex matrices.
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  • 文章类型: Journal Article
    Sorghum is the major raw material for the production of Chinese Baijiu (Chinese liquor) and has a great effect on the flavor of Baijiu. Volatiles in cooked glutinous and non-glutinous sorghum samples were extracted using solid-phase microextraction (SPME) and analyzed via comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) and gas chromatography-olfactometry/mass spectrometry (GC-O/MS). A total of 145 volatile compounds and 52 potent odorant compounds were identified from both sorghum types according to the retention index, MS, aroma, and standards. Based on their aroma features, the compounds were grouped into eight general categories, and the intensities of each aroma group were summed. Moreover, most of the compounds detected in the cooked sorghums were also detected in commercial Chinese Baijiu, indicating that the aroma compounds produced during the sorghum cooking process have a direct and significant influence on the final flavor quality of Baijiu.
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  • 文章类型: Journal Article
    In this study, the detailed volatile compositions of Chinese herbaceous aroma-type Baijiu (HAB) were characterized by comprehensive two-dimensional gas chromatography-time of flight mass spectrometry (GC×GC-TOFMS). A total of 606 compounds were tentatively identified by similarity, mass spectral data, and retention indices, among which 247 compounds were positively verified by authentic standards. Esters were present in higher numbers (179), followed by aldehydes and ketones (111), and alcohols (81). In addition, there were also many terpenes (82), sulfides (37), furans (29), nitrogenous compounds (29), lactones (17), and so on. Meanwhile, the extraction effects of volatile components from different sample pretreatment methods (headspace solid-phase microextraction (HS-SPME), solid phase extraction (SPE), and stir bar sorptive extraction (SBSE)) for HAB were also revealed. The results indicated that HS-SPME has a better extraction effect on easily volatile compounds, such as alcohols and sulfides, especially for terpenes. SPE was particularly beneficial for the analysis of nitrogen-containing compounds; SBSE showed medium extraction ability for most types of compounds and was more suitable for the target analysis of trace content substances.
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