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Molecular and Isotopic Characteristics of Mature Condensates from the East China Sea Shelf Basin Using gc×gc-tofms and gc-IRMS

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Journal of Earth Science 2019年第2期30卷 376-386页

作者： Chao Shan Jiaren Ye Alan Scarlett Kliti Grice Key Laboratory of Tectonics and Petroleum Resources of Ministry of Education China University of Geosciences WA Organic and Isotope Geochemistry Centre and John de Laeter Centrethe Institute for Geoscience ResearchDepartment of Applied ChemistryCurtin University of Technology

In this study, biomarkers, together with stable carbon(δ13 C) and hydrogen(δD) isotopic compositions of n-alkanes have been examined in a suite of condensates collected from the East China Sea Shelf Basin(ECSSB) in order to delineate their source organic matter input, depositional conditions and evaluate their thermal maturity. Previously, gc-MS analyses have shown that all the condensates are formed in oxidizing environment with terrestrial plants as their main source input. No significant differences were apparent for biomarker parameters, likely due to the low biomarker content and high maturity of these condensates. Conventional gc-MS analysis however, may provides limited information on the sources and thermal maturity of complex mixtures due to insufficient component resolution. In the current study, we used comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry(gc×gc-tofms) to increase the chromatographic resolution. Compounds such as alkyl cyclohexanes, alkyl cyclopentanes and diamondoids, which can be difficult to identify using conventional gc-MS analysis, were successfully identified using gc×gc-tofms. From our analyses we propose two possibly unreported indicators, including one maturity indicator(C5--cyclohexane/C5+-cyclohexane) and one oxidation-reduction environment indicator(alkyl-cyclohexane/alkyl-cyclopentane). Multiple petroleum charging events were proposed as an explanation for the maturity indicators indexes discrepancy between methyl-phenanthrene index(MPI) and methyl-adamantane index(MDI). In addition, the stable isotopic results show that condensates from the Paleogene have significantly higher positive δ13 C values of individual n-alkanes than the Neogene samples. Based on δD values, the samples can be divided into two groups, the differences between which are likely to be attributed to different biosynthetic precursors. Variation within each group can likely be attributed to vaporization.

关键词： condensate biomarker characteristic source information gc×gc-tofms gc-IRMS

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Characterization of terpenoids and norisoprenoids from base and retail Qingke Baijiu by gc×gc-tofms and multivariate statistical analysis

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Food Science and Human Wellness 2023年第1期12卷 192-199页

作者： Xinlei Wang Lin Zhu Xuebo Song Si Jing Fuping Zheng Mingquan Huang Shengbao Feng Luzhong La Beijing Advanced Innovation Center for Food Nutrition and Human Health Beijing Technology and Business UniversityBeijing 100048China Beijing Laboratory of Food Quality and Safety Beijing Technology and Business UniversityBeijing 100048China Key Laboratory of Brewing Molecular Engineering of China Light Industry Beijing Technology and Business UniversityBeijing 100048China Qinghai Huzhu Highland Barley Wine Co. Ltd.Huzhu 810500China

Qingke(highland barley)Baijiu is a special Chinese Baijiu which is mainly produced from Qinghai-Tibet *** the pine board is used as the bottom of the fermentation pit,we deduced that the terpenoids and norisoprenoids in pine board might be introduced into Qingke ***,the terpenoids and norisoprenoids in Qingke Baijiu were investigated by headspace solid phase microextraction(HS-SPME)combined with comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry(gc×gc-tofms).The results showed thatγ-terpinene(0.70-530.72μg/L),α-phellandrene(0.34-256.66μg/L),longicyclene(0-38.55μg/L),α-pinene(1.21-35.54μg/L)and limonene(0.93-23.69μg/L)were the top 5 terpenoids/norisoprenoids in Qingke *** was detected and reported for the first time in Baijiu,and the concentrations in Qingke Baijiu were 0.78μg/L(fresh)and 3.90μg/L(7 years old).According to the principal component analysis(PCA)plot,young,aged,and retail Qingke Baijiu could be differentiated *** change(FC)and t-tests analysis indicated thatβ-pinene,γ-terpinene,andα-selinene were the most different terpenoids/norisoprenoids between young and aged Qingke Baijiu,and longifolene was the most different terpenoids/norisoprenoids between base and retail Qingke *** terpenoids and norisoprenoids,such as(E)-β-ionone,isoborneol andβ-cyclocitral,could be potential markers indicating the ageing process of Qingke Baijiu.

关键词： Terpenoids Norisoprenoids Qingke Baijiu HS-SPME gc×gc-tofms PCA

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Determination of major aroma components in mainstream cigarette smoke using cold trap followed by gc×gc-tofms

Determination of major aroma components in mainstream cigare...

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中国烟草学会2017年学术年会

作者： XIANG Zhangmin CAI Kai GENG Zhaoliang PAN Wenjie ZHOU Shuping 贵州省烟草科学研究院 Upland Flue-Cured Tobacco Quality & Ecology Key Laboratory of CNTC

A qualitative and quantitative analytical methodwas developed and applied to the analysis of major aroma components present in mainstream tobacco smoke. The smoke samples were cold trapped using liquid nitrogen and then analysed by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry(gc×gc-tofms). Important experimental parameters, such as the type, volume of the extraction solvent, and flow rate of smoking were optimised to improve the analysis outcome. The results indicated that 180 mL of diethyl ether in the cold trap with a 4.0 mL ·min smoke flow rate were the optimal condition. Using this experimental setup, a total of 112 aroma components were identified and quantified using a mass spectral library search. In addition, a comparison of the cold trap method was made to that obtained using Cambridge filter pad method, this indicated that more peak were present in the sample. A higher peak number and better repeatability were obtained using the cold trap method. Finally, the developed analytical method was applied to the classification of different cigarette styles and useful results were achieved.

关键词： Mainstream smoke Aroma components Cold trap gc×gc-tofms

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利用gc×gc-tofms鉴定包包曲中的游离香气成分

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酿酒科技 2021年第11期 17-24,30页

作者：郑佳赵东何张兰张建敏刘志鹏杨康卓乔宗伟宜宾五粮液股份有限公司四川宜宾644000

包包曲是五粮液酿造独具特色的糖化发酵剂,了解包包曲对五粮液酿造中风味的贡献度对提高酒质具有重要实际意义。本研究采用清蒸法获得了五粮液生产用包包曲粉中的游离香气成分,进一步利用固相萃取法结合全二维气相色谱-飞行时间质谱法... 详细信息

包包曲是五粮液酿造独具特色的糖化发酵剂,了解包包曲对五粮液酿造中风味的贡献度对提高酒质具有重要实际意义。本研究采用清蒸法获得了五粮液生产用包包曲粉中的游离香气成分,进一步利用固相萃取法结合全二维气相色谱-飞行时间质谱法系统研究了包包曲中的游离香气成分。结果表明,共鉴定出209种游离香气成分,包括34种醇类,30种芳香类,26种酮类,22种酯类,22种醛类,21种吡嗪类,21种呋喃类,7种硫化物,6种酸类,以及20种其他类成分,其中68种游离挥发性香气成分为首次在包包曲中检出,并且大多数挥发性香气成分对白酒的香气具有重要贡献。

关键词：包包曲 gc×gc-tofms 鉴定游离香气成分

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包包曲风味萃取方式的对比及gc×gc-tofms在其风味化合物鉴定中的应用

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酿酒科技 2023年第6期 71-76页

作者：陈荻杨康卓刘志鹏赵东郑佳宜宾五粮液股份有限公司技术研究中心四川宜宾644000 固态发酵资源利用四川省重点实验室四川宜宾644000 中国轻工业浓香型白酒固态发酵重点实验室四川宜宾644000

包包曲是五粮液酿造独具特色的糖化发酵剂,分析包包曲中的风味成分对生产控制具有重要意义。本研究采用液液萃取(LLE)、溶剂辅助风味蒸发(SAFE)、顶空固相微萃取(HS-SPME)等方法对包包曲中的风味成分进行萃取,并进一步利用全二维气相色... 详细信息

包包曲是五粮液酿造独具特色的糖化发酵剂,分析包包曲中的风味成分对生产控制具有重要意义。本研究采用液液萃取(LLE)、溶剂辅助风味蒸发(SAFE)、顶空固相微萃取(HS-SPME)等方法对包包曲中的风味成分进行萃取,并进一步利用全二维气相色谱-飞行时间质谱(gc×gc-tofms)对化合物进行分析,以建立最有效的包包曲风味分析方法。结果表明,LLE法共提取化合物316种,在总峰面积、化合物数量及低含量化合物的检出方面具有优势;干法HS-SPME萃取效果优于湿法HS-SPME,两者对醛类表现出良好的吸附性;半定量结果显示,包包曲中数量最多、含量最高的是醇类,2,3-丁二醇、苯乙醇、丙二醇、醋酸、己酸、丁内酯等化合物在包包曲中相对含量较高。本研究可为包包曲乃至酒曲的风味研究提供有效参考。

关键词：包包曲 gc×gc-tofms 萃取风味化合物

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剑南春酒中萜烯类生理活性物质的gc×gc-tofms研究

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酿酒科技 2009年第9期 48-49页

作者：徐占成陈勇莫凯周泽华剑南春集团有限责任公司四川绵竹618200

采用全二维-飞行气质联用检测仪(gc×gc-tofms)全面分析剑南春酒体中各种风味成分。结果表明,剑南春中含有近百种萜烯类化合物,其中又以金合欢烯、古芸烯、香橙烯、香柠檬烯、雪松烯、蛇床烯、罗汉柏烯、榄香烯、杜松烯等倍半萜居多,这... 详细信息

采用全二维-飞行气质联用检测仪(gc×gc-tofms)全面分析剑南春酒体中各种风味成分。结果表明,剑南春中含有近百种萜烯类化合物,其中又以金合欢烯、古芸烯、香橙烯、香柠檬烯、雪松烯、蛇床烯、罗汉柏烯、榄香烯、杜松烯等倍半萜居多,这类化合物普遍存在于植物体中,是具有较强香气和特殊功效的生理活性物质。

关键词：分析检测剑南春酒 gc×gc-tofms 萜烯

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Distribution and geochemical significance of alkylbenzenes for crude oil with different depositional environments and thermal maturities

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Petroleum Science 2024年第2期21卷 777-790页

作者： Bing-Kun Meng Dao-Fu Song Yuan Chen Sheng-Bao Shi School of Petroleum Engineering and Environmental Engineering Yan'an UniversityYan'an716000ShaanxiChina State Key Laboratory of Petroleum Resources and Prospecting College of GeosciencesChina University of PetroleumBeijing102249China

A total of 45 alkylbenzenes were detected and identified in crude oils with different depositional environments and thermal maturities from the Tarim Basin,Beibuwan Basin,and Songliao Basin using comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry(gc×gctofms).By analyzing the distribution characteristics of C0-C5alkylbenzenes,it is found that the content of some alkylbenzenes varies greatly in crude *** on the distribution characteristics of 1,2,4,5-tetramethylbenzene(Te MB)and 1,2,3,4-Te MB,the ratio of 1,2,4,5-Te MB to 1,2,3,4-Te MB is proposed to indicate the organic matter origin and depositional environment of ancient *** samples originated mainly from lower hydrobiont,algae,bacteria and source rocks deposited under reducing/anoxic conditions have low 1,2,4,5-/1,2,3,4-Te MB values(less than 0.6),while oil samples originated mainly from terrestrial higher plants and source rocks deposited under oxic/sub-oxic conditions have higher 1,2,4,5-/1,2,3,4-Te MB values(greater than 1.0).The significant difference of 1,2,4,5-/1,2,3,4-Te MB values is controlled by 1,2,4,5-Te MB content.1,2,4,5-Te MB content in oils derived from source rocks deposited in oxidized sedimentary environment(greater than 1.0 mg/g whole oil)is higher than that in oils from source rocks deposited in reduced sedimentary environment(less than 1.0 mg/g whole oil).1,2,4,5-/1,2,3,4-Te MB ratio might not or slightly be affected by evaporative fractionation,biodegradation and thermal maturity.1,2,4,5-/1,2,3,4-Te MB ratio and 1,2,4,5-Te MB content can be used as supplementary parameter for the identification of sedimentary environment and organic matter *** should be noted that compared to the identification of organic matter sources,the 1,2,4,5-/1,2,3,4-Te MB parameter is more effective in identifying sedimentary environments.

关键词： 1 2 4 5-Tetramethylbenzene gc×gc-tofms Organic matter origin Depositional environment

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基于多维色谱技术的Lager啤酒特征香气成分解析

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食品与发酵工业 2024年

作者：郭琪王玉海陈明江伟王德良孙志伟葛佳伟郝建秦中国食品发酵工业研究院国家酒类品质与安全国际联合研究中心广州珠江啤酒股份有限公司新疆农业大学食品科学与药学学院

该研究采用人工感官评价、顶空气相色谱火焰离子化检测器法（headspace gas chromatography with flame ionization detection，HS-gc-FID）、顶空固相微萃取气相色谱-质谱联用技术（headspace solid phase microextraction gas chromatography-mass spectrometry，HS-SPME-gc-MS）及顶空固相微萃取-全二维气相色谱-飞行时间质谱（headspace solid phase microextraction-comprehensive two-dimensional gas chromatograph-time of flight mass spectrometer，HS-SPME-gc×gc-tofms）技术对国内6种品牌的Lager啤酒的特征香气成分进行了分析。通过HS-SPME-gc×gc-tofms技术对6种啤酒中的香气化合物进行了全面检测及半定量分析，分别测出520、520、519、522、518、513种物质，并首次在Lager啤酒中测出罗勒烯、白铃兰醇、桃醛等化合物。通过HS-gc-FID及HS-SPME-gc-MS共定量了61种香气成分，其中酯类24种、醇类14种、醛类10种、酸类6种、酮类3种、酚类2种、含S及含O杂环化合物各1种。结合多元变量统计分析的方法，通过一维色谱发现主要差异物质为异戊醇、苯乙醇、乙酸乙酯等，通过HS-SPME-gc×gc-tofms的相对定量结果进一步表明，差异物质还体现在2，3-丁二醇硝酸酯等含N化合物及（E）-β-金合欢烯、罗勒烯等其他共计100种化合物之间。此外，通过多元统计学、气味活性值结合皮尔森相关性分析发现，啤酒麦芽香高低与菠萝酮的含量高低相关，酒花香与芳樟醇、乙酸芳樟酯的含量相关，花香、酯香高低与乙酸乙酯、辛酸乙酯、乙酸苯乙酯等的含量高低相关，醇香高低与异丁醇的含量高低相关，异香高低与柠檬醛、壬醛的含量高低相关。通过二维结合正交偏最小二乘-判别分析还发现，麦芽香还与2，3-丁二醇硝酸酯，1，2-丙二醇硝酸酯等含N化合物相关。

关键词：啤酒香气成分 gc-FID gc-MS gc×gc-tofms 多变量统计学分析

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Origin,Distribution and Geochemical Significance of Isopropyltoluene Isomers in Crude Oil

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Journal of Earth Science 2022年第1期33卷 215-228页

作者： Bingkun Meng Daofu Song Yuan Chen Shengbao Shi Shixin Zhou Northwest Institute of Eco-Environment and Resources Chinese Academy of SciencesLanzhou 730000China University of Chinese Academy of Sciences Beijing 100049China State Key Laboratory of Petroleum Resources and Prospecting College of GeosciencesChina University of PetroleumBeijing 102249China

With comprehensive two-dimensional gas chromatography linked to time-of-flight mass spectrometry(gc × gc-tofms),ten light hydrocarbon(LH) compounds were qualitatively and quantitatively studied in light hydrocarbons(LHs) components of crude *** significant differences in the concentrations of 3-isoproyltoluene(3-iPT),4-isoproyltoluene(4-iPT) and 2-isoproyltoluene(2-iPT) in crude oils,and the 2-iPT probably derived mainly from similar skeleton monocyclic terpenoids via dehydrogenation and aromatization,the ratios of(3+4)-/2-iPT(iPTr),3-/2-iPT(iPTr1) and 4-/2-iPT(iPTr2) are proposed to distinguish the organic matter origin of crude *** higher iPTr(>8.0),iPTr1(>7.0) and iPTr2(>4.0) values indicate that crude oils are sourced from the co-contribution of lower aquatic organisms,bacteria,algae,and terrestrial higher plants,whereas lower iPTr(<5.0),iPTr1(<3.0),iPTr2(<2.0) values suggest that crude oils originated from terrestrial higher *** iPTr,iPTr1,and iPTr2 values show notable distinction which is mainly controlled by 2-iPT concentrations,while the concentrations of 3-iPT and 4-iPT have similar distribution range in all studied *** 2-iPT depleted in marine oils from the Tarim Basin and lacustrine oils from the Beibuwan Basin is less than 0.30 mg/g LHs,whereas 2-iPT enriched in swamp oils from the Tarim Basin is greater than 0.50 mg/g *** iPTr,iPTr1,and iPTr2 ratios and 2-iPT concentrations can be used to distinguish the organic matter origin of crude oils,especially for light oils and condensates with low concentrations of biomarkers.

关键词： organic carbon gc×gc-tofms light oils and condensates organic matter origin

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Non-target Screening and Quantitation of Organic Chlorides in Oilfield Chemicals with Comprehensive Two Dimensional Gas Chromatography Coupled with Time of Flight Mass Spectrometry

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China Petroleum Processing & Petrochemical Technology 2017年第4期19卷 65-71页

作者： Zheng Kewen Guo Rui Ren Guofa Xia Lingyan Xiong Wei Zhang Jin Chu Xiaodong Yu Zhiqiang Institute of Environmental Pollution and Health School of Environmental and Chemical Engineering Shanghai University Shanghai 200072 SINOPEC Shengli Oilfield Branch Dongying 257000

Advanced analytical methodology based on comprehensive two-dimensional gas chromatography-time of flight mass spectrometry(gc×gc-tofms) is proposed for investigation of organic chlorides in different oilfield *** target screening was initially carried out on 8 suspected organic chlorides by evaluating the capability of the enhanced separation and reliable identification at a trace concentration. gc×gc-tofms allowed for the fast and automated analysis of organic chlorides at a level of 200 μg/L. This method was subsequently applied for non-target screening of organic chlorides in different oilfield chemicals at various locations across China. 22 organic chlorides were identified and verified by comparison with pure standards in the mixed sample. Finally, this method was used to determine the content of the organic chlorides in individual samples. The result showed that the organic chloride levels in 19 of the 39 tested oilfield chemicals were above the threshold limit of 1.0 mg/L.

关键词： gc×gc-tofms non-target screening oilfield chemicals organic chlorides quantitation

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