Sur la composition de l'arǒme de the noir V

Methyl anthranilate, geranylacetone and five lactones: γ-valerolactone, γ-heptalactone, γ-décalactone, δ-décalactone, 5-hydroxy dec-7-enoic acid-lactone have recently been identified in black tea aroma by means of GC./MS. and by sniffing the effluent from a gas chromatograph. Their intrinsic character, rather fruity and flowery, gives a certain freshness and an agreable note to the aroma.     

Sur la composition de l'arôme de thé

A gas-chromatographic investigation of black tea aroma has revealed, besides 19 known components, the presence of 4 new substances: 1-penten-3-ol, trans-2-hexen-1-ol, α-terpineol and β-ionone. The fragmentation pattern of 1-penten-3-ol has been determined by means of high resolution mass spectrography.     

黑胡椒根萜类化合物的分析

报道了用蒸馏 萃取法提取黑胡椒根中挥发性物质,测得黑胡椒根挥发油的质量分数为3.1%,用GC/MS法从黑胡椒根挥发油中分离并确定出28种化学成分。其中主要成分为萜类化合物,占总检出量的82.48%。     

Sur la composition de l'arôme de thé noir II

Trans-2-penten-1-ol, 1-ethyl-2-formyl-pyrrole, 2-trans, 4-cis-heptadienal, phenyl-acetonitrile, methyl benzoate, 2-phenyl-but-2-enal and the lactone of 2,6,6-trimethyl-2-hydroxy-cyclohexylidene acetic acid have been separated from black tea aroma by gas-liquid chromatography, and identified by infra-red and mass spectrometry.     

薄荷卷烟中香味成分的全二维气相色谱/飞行时间质谱分析

采用全二维气相色谱/飞行时间质谱法(GC×GC/TOFMS),以较长的非极性柱DB-5MS(30m×0.25mm×0.25μm)作为第一维柱,较短的中等极性柱DB-17MS(2m×0.1mm×0.1μm)作为第二维柱,利用固相微萃取法作为香味成分的萃取方法,对薄荷型ESSE卷烟的核心香味成分进行了定性分析,TOFMS谱图库检索结合全二维特有的包含结构信息的二维谱图,通过族分离和结构谱图鉴定,共鉴定了187种挥发性成分,其中对香气有贡献的成分118种.     

Screening of key odorants and anthocyanin compounds of cv. Okuzgozu (Vitis vinifera L.) red wines with a free run and pressed pomace using GC‐MS‐Olfactometry and LC‐MS‐MS

The principal purpose of the present work is to characterize the aroma, aroma‐active, and anthocyanin profiles of Okuzgozu wines and to observe the effect of the pomace pressing technique on these parameters. A total of 58 and 59 volatile compounds were identified and quantified in free‐run juice wine (FRW) and pressed pomace wine (PW). Alcohols were found as the most dominant group among aroma compounds followed by esters and acids. However, among all these compounds, only 11 and 13 of them could be considered as key odorants in aromatic extracts of FRW and PW, respectively. According to GC‐MS‐O analysis, ethyl octanoate (fruity), phenyl ethyl acetate (fruity), and 2‐phenyl ethanol (flowery) were found as the main contributors to the overall scent of both wines. Beyond the aroma profiles, anthocyanin contents of both types of wines were also investigated, and total 14 and 15 anthocyanins were identified and quantified in FRW and PW. Malvidin‐3‐glycoside and its acetyl and coumaroyl forms were identified as the dominant anthocyanins in both wines. It is worth noting the pressing application (2.0 atm) led to an increase of some unpleasant notes in the aroma providing chemical, pharmacy, and fermented aromas in wine. On the other hand, the wines produced with pressed pomace presented higher amounts of anthocyanins.     

Sur la composition de l'arôme de cacao

A gas-chromatographic separation of cocoa aroma, followed by infra-red and mass-spectrometric identification, has yielded, besides 22 of the 91 previously described constituents, 35 new substances (8 aliphatic, 1 alicyclic, 7 aromatic, 9 o-heterocyclic, 4 pyrrolic, and 6 pyrazinic).     

Identification of Free and Glycosidically Bound Volatiles and Glycosides by Capillary GC and Capillary GC‐MS in “Lulo del Chocó” (Solanum topiro)

The volatile constituents of lulo del Chocó (Solanum topiro) fruit pulp obtained by liquid‐liquid extraction were analyzed by capillary GC and capillary GC‐MS. In total, 30 components were identified with methyl salicylate, hexadecanoic acid, hexanal, guaiacol, ethyl butanoate, and ethyl acetate being the major components. Chirospecific MDGC analysis revealed the predominance of (R)‐ethyl‐3‐hydroxybutanoate (ee 40%) and the presence of racemic mixtures both of δ‐octalactone and of δ‐decalactone. For γ‐hexalactone, γ‐octalactone, and γ‐decalactone enantiomeric distributions of 22.4 : 77.6, 22.9 : 77.1, and 20.0 : 80.0, (R) : (S), respectively, were determined. Glycosidically bound aroma compounds were identified by capillary GC and capillary GC‐MS after isolation of the glycosidic fraction obtained by Amberlite XAD‐2 adsorption and methanol elution followed by hydrolysis with a commercial pectinase enzyme. In total 13 bound aroma compounds (aglycones) were identified. These aglycones mainly consisted of compounds exhibiting aromatic structures. Additionally, with the aid of capillary GC and capillary GC‐MS (EI and NCI) of trifluoroacetylated derivatives we identified eight glucosides: the novel 3,6‐epoxy‐7‐megastigmen‐5,9‐diol β‐D‐glucopyranoside and the hexyl, benzyl, linalyl oxide (furanic), 2‐phenylethyl, vomifolyl (isomer 1), (6S,9R)‐vomifolyl, and scopoletin β‐D‐glucopyranosides.     

中国苦水玫瑰油香气成分的研究

 选择OV1701交联毛细管柱作为中国苦水玫瑰油的分离柱,并采用现代气相/质谱(GC/MS)、气相/红外光谱(GC/IR)技术手段,结合标准品对照,对玫瑰油中分离出的130余种化合物进行鉴别,初步鉴定出了101种化合物。研究表明,不同品种的玫瑰油形成各自不同的香味,这与栽培品种和土壤、温度、降雨量等综合栽培环境差异有关。中国苦水玫瑰油以其特有的浓郁玫瑰香气,应成为世界玫瑰油中一个重要品种。     

Headspace Solid-Phase Microextraction GC–MS for Rapid Rice Aroma Analysis Using Optimization Tools

A key feature of rice acceptance by consumers is closely related to its aroma. A few decades of research on rice aroma indicated associated difficulties which arise from its complicated volatile composition. Our investigation seeks to resolve this highly complicated aroma profile using an experimental design for headspace solid-phase microextraction GC–MS. The Plackett–Burman methodology was used as a factor screening method for the headspace solid-phase microextraction procedure and GC–MS analysis, and a central composite design was implemented as an optimization methodology for both steps. Optimization of the extraction procedure and GC–MS analysis leads to a highly resolved rice aroma profile resulting in 66 new constituents. A total of 123 constituents were identified by implementing the procedure on Champa rice from the south of Iran.     

GC‐MS of amaryllidaceous galanthamine‐type alkaloids

Galanthamine‐type alkaloids produced by plants of the Amaryllidaceae family are potent acetylcholinesterase inhibitors. One of them, galanthamine, has been marketed as a hydrobromide salt for the treatment of Alzheimer's disease. In the present work, gas chromatography with electron impact mass spectrometry (GC‐EIMS) fragmentation of 12 reference compounds isolated from various amaryllidaceous plants and identified by spectroscopic methods (1D and 2D nuclear magnetic resonance, circular dichroism, high‐resolution MS (HRMS) and EIMS) was studied by tandem mass spectrometry (GC‐MS/MS) and accurate mass measurements (GC‐HRMS). The studied compounds showed good peak shape and efficient GC separation with a GC‐MS fragmentation pattern similar to that obtained by direct insertion probe. With the exception of galanthamine‐N‐oxide and N‐formylnorgalanthamine, the galanthamine‐type compounds showed abundant [M]^+. and [M‐H]⁺ ions. A typical fragmentation pattern was also observed, depending on the substituents of the skeleton. Based on the fragmentation pathways of reference compounds, three other galanthamine‐type alkaloids, including 3‐O‐(2′‐butenoyl)sanguinine, which possesses a previously unelucidated structure, were identified in Leucojum aestivum ssp. pulchelum, a species endemic to the Balearic islands. GC‐MS can be successfully applied to Amaryllidaceae plant samples in the routine screening for potentially new or known bioactive molecules, chemotaxonomy, biodiversity and identification of impurities in pharmaceutical substances. Copyright © 2012 John Wiley & Sons, Ltd.     

吸附热脱附-气质联用技术分析烟丝中挥发及半挥发性成分

卷烟致香成分是卷烟质量的重要指标,利用吸附热脱附-气相色谱-质谱技术分析了烟丝中挥发及半挥发性成分79种,其中酸性物质17种,碱性物质5种,中性物质57种,为烟草化学研究提供了简单快速的分析方法.     

Headspace solid-phase microextraction gas chromatography/mass spectrometry in the analysis of the aroma constituents of 'Cannonau of Jerzu' wine

"Cannonau of Jerzu" wine is a typical Sardinian product, obtained from only one particular grape variety. Its aroma profile is highly characteristic from the organoleptic point of view but, until now, no analytical investigation of the aroma components has been reported. This aspect has been studied by headspace solid-phase microextraction coupled with gas chromatography/mass spectrometry (GC/MS). Using this approach, 76 abundant aroma components were identified. The results thus obtained show on one hand that the terpene profile is, as expected, dependent on the quality of the grapes (in terms of selection before vintage), and, on the other, that some components are strongly dependent on the production and ageing method.     

固相微萃取-气相色谱-质谱联用结合嗅觉检测法鉴定血橙汁中的香气活性化合物

采用固相微萃取-气相色谱-质谱法(SPME-GC-MS)和嗅觉检测法对血橙汁中的挥发性物质进行分析,确定了血橙汁中的香气活性化合物。采用二乙烯基苯/碳分子筛/聚二甲基硅氧烷共聚物(DVB/CAR/PDMS)萃取头在40 ℃条件下顶空萃取40 min。通过气相色谱-质谱联用结合保留指数,在所萃取的血橙汁的挥发性化合物中共鉴定出46种化合物。通过嗅觉检测法检测出34种具有气味的化合物,其中23种被定性。结果表明,对血橙汁香气起主要贡献的化合物是丁酸乙酯、辛醛、γ-松油烯、芳樟醇、4-乙酰基-1-甲基环己烯、癸醛、(-)-香芹酮、乙酸香叶酯、巴伦西亚桔烯以及保留指数分别为1020,1143,1169和小于800的4个未知化合物,这些香气强度较高的化合物的总相对含量为7.22%。     

黑蚂蚁的脂肪酸及抗氧化性能的分析

对黑蚂蚁中脂肪酸的组成和含量进行测定。采用索氏提取法提取其脂肪酸,再进行甲酯化处理,以气相色谱-质谱联用仪进行了分离和鉴定。由黑蚂蚁中分离鉴定出11种脂肪酸,占脂肪酸总量的99.78%,不饱和脂肪酸占脂肪酸总量的80.65%,饱和脂肪酸占脂肪酸总量的19.13。通过流动注射化学发光法分析了黑蚂蚁的抗氧化性能,结果表明,黑蚂蚁具有较强的抗氧化性能。     

Determination of Aroma Compounds from Alcoholic Beverages in Spiked Blood Samples by Means of Dynamic Headspace GC–MS

Some aroma compounds found in alcoholic beverages are characteristic of a certain beverage (i.e. 2,4-decadienoic acid ethyl ester is characteristic of pear spirit and 5-butyltetrahydro-4-methylfuran-2-on “whiskey lactone” is characteristic of aged spirits like whiskey). These substances were detectable in beverages but not in blood samples. The aim of this investigation was to find a sensitive sampling technique for aroma compounds in whole blood samples. This technique may be used in forensic toxicology for examination of drinking claims. The method comprises dynamic headspace sampling using a purge and trap concentrator, followed by quantitative gas chromatography–mass spectrometry (dynamic HS–GC–MS). The influence of sample preparation, trap adsorbents and sample temperature as well as desorption time and purge time on the quality of the analytical results were investigated. The following optimal parameters were determined: stirred and diluted whole blood sample without salt addition, use of Carbotrap C as trap material, sample temperature at 80 °C, desorption time 20 min and purge time 30 min. These optimal parameters were used for the determination of detection limits (LOD). The LOD of aroma compounds by means of dynamic headspace sampling were compared with the results of conventional sampling: the static headspace technique. Limits of detection for the aroma compounds with conventional static headspace GC are in the range 400–10,000 μg L⁻¹. Dynamic headspace–GC was found to be a more sensitive sampling technique for most of the aroma compounds investigated (e.g. C₄–C₈ ethyl esters, benzoic acid ethyl ester, linalool oxide and 4-ethylguaiacol) with detection limits between 1 and 50 μg L⁻¹, but there were also limits to the sampling of substances with lower volatility like decanoic acid ethyl ester, 2,4-decadienoic acid ethyl ester, eugenol and whiskey lactone with detection limits of about 1,000 μg L⁻¹.

     

Determination of Aroma Compounds from Alcoholic Beverages in Spiked Blood Samples by Means of Dynamic Headspace GC–MS

Some aroma compounds found in alcoholic beverages are characteristic of a certain beverage (i.e. 2,4-decadienoic acid ethyl ester is characteristic of pear spirit and 5-butyltetrahydro-4-methylfuran-2-on “whiskey lactone” is characteristic of aged spirits like whiskey). These substances were detectable in beverages but not in blood samples. The aim of this investigation was to find a sensitive sampling technique for aroma compounds in whole blood samples. This technique may be used in forensic toxicology for examination of drinking claims. The method comprises dynamic headspace sampling using a purge and trap concentrator, followed by quantitative gas chromatography–mass spectrometry (dynamic HS–GC–MS). The influence of sample preparation, trap adsorbents and sample temperature as well as desorption time and purge time on the quality of the analytical results were investigated. The following optimal parameters were determined: stirred and diluted whole blood sample without salt addition, use of Carbotrap C as trap material, sample temperature at 80 °C, desorption time 20 min and purge time 30 min. These optimal parameters were used for the determination of detection limits (LOD). The LOD of aroma compounds by means of dynamic headspace sampling were compared with the results of conventional sampling: the static headspace technique. Limits of detection for the aroma compounds with conventional static headspace GC are in the range 400–10,000 μg L^?1. Dynamic headspace–GC was found to be a more sensitive sampling technique for most of the aroma compounds investigated (e.g. C₄–C₈ ethyl esters, benzoic acid ethyl ester, linalool oxide and 4-ethylguaiacol) with detection limits between 1 and 50 μg L^?1, but there were also limits to the sampling of substances with lower volatility like decanoic acid ethyl ester, 2,4-decadienoic acid ethyl ester, eugenol and whiskey lactone with detection limits of about 1,000 μg L^?1.     

Preparation of novel solid-phase microextraction fibers by sol-gel technology for headspace solid-phase microextraction-gas chromatographic analysis of aroma compounds in beer

3-(Trimethoxysilyl)propyl methacrylate (TMSPMA) was first used as precursor as well as selective stationary phase to prepare the sol-gel-derived TMSPMA-hydroxyl-terminated silicone oil (TMSPMA-OH-TSO) solid-phase mircroextraction (SPME) fibers for the analysis of aroma compounds in beer. TMSPMA-OH-TSO was a medium polarity coating, and was found to be very effective in carrying out simultaneous extraction of both polar alcohols and fatty acids and nonpolar esters in beer. The extraction temperature, extraction time, and ionic strength of the sample matrix were modified to allow for maximium sorption of the analytes onto the fiber. Desorption temperature and time were optimized to avoid the carryover effects. To check the matrix effects, several different matrices, including distilled water, 4% ethanol/water (v/v) solution, a concentrated synthetic beer, a "volatile-free" beer and a real beer were investigated. Matrix effects were compensated for by using 4-methyl-2-pentanol as internal standard and selecting the "volatile-free" beer as working standard. The method proposed in this study showed satisfactory linearity, precision and detection limits and accuracy. The established headspace SPME-gas chromatography (GC) method was then used for determination of volatile compounds in four beer varieties. The recoveries obtained ranged from 92.8 to 105.8%. The relative standard deviations (RSD, n = 5) for all analytes were below 10%. The major aroma contributing substances of each variety were identified via aroma indexes.     

Characterization of Ayran Aroma Active Compounds by Solvent-Assisted Flavor Evaporation (SAFE) with Gas Chromatography–Mass Spectrometry–Olfactometry (GC–MS–O) and Aroma Extract Dilution Analysis (AEDA)

The aroma compounds of ayran were isolated using solvent-assisted flavor evaporation (SAFE) resulting in a more representative extract of ayran odor compared to liquid–liquid extraction (LLE), solid-phase extraction (SPE), and simultaneous distillation–extraction (SDE). The aromatic extract was subjected to sensory analysis and identified and quantified by gas chromatography–mass spectrometry (GC–MS). A total of 19 volatile compounds were detected that included alcohols, aldehyde, acids, esters, ketones, and terpenes. However, the compounds present at the highest concentrations were ethyl lactate, ethanol, 2,3-butanediol, acetoin, and acetic acid. The key odorants for the ayran drinks were detected using aroma extract dilution analysis (AEDA) and GC–MS–olfactometry (GC–MS–O). A total of 14 aroma-active compounds were determined for the first time. The flavor dilution (FD) factors ranged between 4 and 512 while their odor activity values (OAVs) were from 1.35 to 1126.99. Ethyl lactate (FD of 512 whey/creamy), 2-methylbutanal (FD of 512, fruity), acetoin (FD of 256, buttery creamy), and butanoic acid (FD of 256, cheesy-sweet) were the strongest aroma-active components of the Ayran drink.     

中国车前草挥发性化学成分分析

用同时蒸馏 萃取装置(SDE)提取中国车前草的挥发性物质,测得车前草挥发油质量分数为2.79%,用GC MS法从车前草的挥发油中分离确认出20种化学成分,占挥发油总量的95.08%。用峰面积归一化法通过化学工作站数据处理系统得出各化学成分在挥发油中的质量分数。