共查询到20条相似文献,搜索用时 15 毫秒
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Pozzar F Sassi A Pace G Lora S D'Archivio AA Jeràbek K Grassi A Corain B 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,11(24):7395-7404
Six gel-type functional resins, that is, three poly-DMAA-co-TMPTP (DMAA = N,N-dimethylacrylamide, TMPTP = trimethylolpropyltrimethacrylate) samples with different degrees of cross-linking (0.6, 1.2, 1.7 % mol) and three poly-DMAA-co-MA-co-TMPTP (MA = methacrylic acid, ca. 5.5 % mol) samples with 1.7, 3.5, and 7 % mol cross-linking were investigated with ISEC (inverse steric exclusion chromatography), and ESR and CP-MAS (cross polarization magic angle spinning) 13C NMR spectroscopy after swelling in water and other solvents. This unprecedented combination of conceptually independent physicochemical techniques provides a thorough overall consistent picture of the morphology of the resins on the nanometer scale and of the molecular accessibility of the swollen polymer framework to the paramagnetic probe TEMPONE (2,2,6,6-tetramethyl-4-oxo-1-oxypiperidine) and to selected solvents. 相似文献
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M. L. Scheepers P. J. Adriaensens J. M. Gelan R. A. Carleer D. J. Vanderzande N. K. De Vries P. M. Brandts 《Journal of polymer science. Part A, Polymer chemistry》1995,33(6):915-920
1H and 13C NMR have been used for the quantitative determination of methylene-ether bridges in melamine-formaldehyde (MF) resins. The amount of methylene-ether bridges was determined by 13C NMR from the number of monomethylolated amino groups consumed in the condensation reactions and is in agreement with that calculated from the condensation water contents. This latter method, which involves a combination of 1H and 13C NMR, is based on the amount of condensation water released during the formation of both methylene and methylene-ether bridges. © 1995 John Wiley & Sons, Inc. 相似文献
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Flavio A. Franchina Delphine Zanella Lena M. Dubois Jean‐Franois Focant 《Journal of separation science》2021,44(1):188-210
In this review, we consider and discuss the affinity and complementarity between a generic sample preparation technique and the comprehensive two‐dimensional gas chromatography process. From the initial technical development focus (e.g., on the GC×GC and solid‐phase microextraction techniques), the trend is inevitably shifting toward more applied challenges, and therefore, the preparation of the sample should be carefully considered in any GC×GC separation for an overreaching research. We highlight recent biomedical, food, and plant applications (2016–July 2020), and specifically those in which the combination of tailored sample preparation methods and GC×GC–MS has proven to be beneficial in the challenging aspects of non‐targeted analysis. Specifically on the sample preparation, we report on gas‐phase, solid‐phase, and liquid‐phase extractions, and derivatization procedures that have been used to extract and prepare volatile and semi‐volatile metabolites for the successive GC×GC analysis. Moreover, we also present a milestone section reporting the early works that pioneered the combination of sample preparation techniques with GC×GC for non‐targeted analysis. 相似文献
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麝鼠香化学成分的色谱—质谱分析 总被引:2,自引:0,他引:2
用常规化学分析法测得麝鼠香含脂肪93.0%,含水分6.8%,GC/MS联机分析麝鼠香醚提物,共鉴定出19种化学成分,主要是大环酮类和脂肪酸类化合物,其中环十七烷酮,环十七烯酮,环十五烷酮和环十五烯酮的含量较高,色谱峰面积分别占13.50%,6.32%,7.21%和4.15%7种大环酮的EI电离质谱图有相似的谱态和一些相同的碎片离子,烯丙基离子(m/z41)和烯羰基离子(m/z55)是基峰。 相似文献
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Regis D. Gougeon Dr. Marianna Lucio Arnaud De Boel Moritz Frommberger Dr. Norbert Hertkorn Dr. Dominique Peyron Dr. David Chassagne Dr. François Feuillat Dr. Philippe Cayot Prof. Andrée Voilley Prof. Istvan Gebefügi Dr. Philippe Schmitt‐Kopplin Priv.‐Doz. Dr. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2009,15(3):600-611
A non‐targeted, ultra‐high‐resolution mass spectrometric, direct analysis of oak‐wood extracts from two species (Quercus robur L. and Quercus petraea Liebl.) from three French forests, and of a wine aged in barrels derived therefrom has been performed to identify families of metabolites that could discriminate both the species and the geographical origin of woods. From 12 T ultra‐high‐resolution Fourier transform ion cyclotron resonance mass spectra of wood extracts, hundreds of mass signals were identified as possible significant biomarkers of the two species, with phenolic and carbohydrate moieties leading the differentiation between Q. robur and Q. petraea, respectively, as corroborated by both FTMS and NMR data. For the first time, it is shown that oak woods can also be discriminated on the basis of hundreds of forest‐related compounds, and particular emphasis is put on sessile oaks from the Tronçais forest, for which sugars are significantly discriminant. Despite the higher complexity and diversity of wine metabolites, forest‐related compounds can also be detected in wines aged in related barrels. It is only by using these non‐targeted analyses that such innovative results, which reveal specific chemodiversities of natural materials, can be obtained. 相似文献
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茶叶香味扫描和挥发性化学成分分析 总被引:11,自引:0,他引:11
为区分不同茶叶的香味,利用电子扫描仪对铁观音、兰贵人、玉针、碧螺春和云雾茶等5种茶叶进行了香味扫描,确定了电子鼻在茶叶香味辨别中的作用。采用固相微萃取.气相色谱/质谱联用法对这5种茶叶样品中的挥发性化学成分进行了定性和定量分析,分别鉴定出40、40、35、16和13种化合物。在鉴定出的化学成分中,乙酸、大茴香醚、十六烷、咖啡因、十六酸和双酚A是5种茶叶样品中所共有的化学成分,每种茶叶样品中又都含有一些特有的化学成分。最后对香味扫描结果和挥发性化学成分分析结果进行了分析,研究了挥发性化学成分组成和含量上的差别,对茶叶样品数据点在香味分析三维图中位置的影响。 相似文献
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追风伞挥发油的化学成分研究 总被引:7,自引:0,他引:7
研究了贵州产追风伞 (LysimachiatrientaloidesHemsl.)挥发油的化学成分。采用水蒸汽蒸馏法提取追风伞挥发性成分 ,用气相 质谱进行分离测定 ,结合计算机质谱图库检索技术对分离的化合物进行结构鉴定 ,从中鉴定出 4 0种化学成分 ;应用峰面积归一化法测定各成分的相对含量。水蒸汽蒸馏提取物的提取率是 0 11%。研究结果表明 ,贵州产追风伞挥发油的主要成分为萜烯类及其含氧衍生物等 ,主要有广藿香醇 (2 2 5 4 % )、乙酸龙脑酯(16 17% )、γ 古芸烯 (3 2 7% )、δ 愈创烯 (2 6 2 % )、橙花叔醇 (2 0 2 % )、芳樟醇 (1 99% )和棕榈酸 (1 96 % )。 相似文献
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Scalarone D van der Horst J Boon JJ Chiantore O 《Journal of mass spectrometry : JMS》2003,38(6):607-617
Electron impact (EI) ionization and ammonia chemical ionization (NH(3)/CI) direct-temperature mass spectrometry (DTMS) was used to characterize five natural terpenoid resins: dammar, mastic, colophony, Manila copal and sandarac. Compositional differences were highlighted by the identification of low molecular mass compounds, ranging from di- to triterpenoids, and polymeric components, based on polycadinene and polycommunic acid. Photo-ageing processes occurring under accelerated indoor and outdoor exposure conditions were also investigated. NH(3)/CI and tetramethylammonium hydroxide EI were applied to increase the sensitivity towards highly oxidized molecules. Oxidation and cross-linking reactions were found to affect mostly triterpenoid resins and diterpenoid abietane and pimarane molecules. Oxidation proceeds through a radical mechanism, generally starting from conjugated double bonds. Oxygen atoms are incorporated in the terpenoid structures in the form of alcohols, ketones and carboxylic acids. Oxidized cadinene oligomers released by pyrolytic degradation of the polycadinene fraction of dammar were detected even in unaged samples. Evidence is given indicating the occurrence of cleavages in the cross-linked polycommunic structure of aged sandarac and Manila copal. Bond scissions produce oligomeric fragments based on the communic acid structure and sufficiently volatile to be desorbed at low temperature in DTMS measurements. 相似文献
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Bio‐oils, produced by biomass pyrolysis, have become promising candidates for feedstocks of high value‐added chemicals and alternative sources for transportation fuels. Bio‐oil is such a complicated mixture that contains nonpolar hydrocarbons and polar components which cover almost all kinds of organic oxygenated compounds such as carboxylic acids, alcohols, aldehydes, ketones, esters, furfurals, phenolic compounds, sugar‐like material, and lignin‐derived compounds. Comprehensive characterization of bio‐oil and its subfractions could provide insight into the conversion process of biomass processing, as well as its further utilization as transportation fuels or chemical raw materials. This review focuses on advanced analytical strategies on in‐depth characterization of bio‐oil, which is concerned with gas chromatography, high‐resolution mass spectrometry, FTIR spectroscopy and NMR spectroscopy, offering complementary information for previous reviews. 相似文献
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I. D. Wilson E. D. Morgan R. Lafont J. P. Shockcor J. C. Lindon J. K. Nicholson B. Wright 《Chromatographia》1999,49(7-8):374-378
Summary HPLC coupled in parallel to nuclear magnetic resonance (NMR) and mass spectrometry (MS) has been used to obtain1H NMR and mass spectra of a number of ecdysteroids present in an extract of the plantSilene otites. Reversed phase gradient chromatography was performed using a D20-acetonitrile-based solvent system. NMR and mass spectra were obtained for integristerone A, 20-hydroxyecdysone, 2-deoxy-20-hydroxyecdysone
and 2-deoxyecdysone to provide structural confirmation using continuous and stopped flow HPLC-NMR. The combined HPLC-NMR-MS
system described here provided a more comprehensive analysis of the ecdysteroids present in the extract than HPLC-NMR alone. 相似文献
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Two different analytical approaches, direct exposure electron ionization mass spectrometry (DE-MS) and gas chromatography/mass spectrometry (GC/MS), were compared in a study of archaeological resinous materials. DE-MS was found to be an efficient fingerprinting tool for the fast screening of organic archaeological samples and for providing information on the major components. GC/MS appeared to be more efficient in unravelling the sample composition at a molecular level, despite the long analysis time and the need for a wet chemical pretreatment. Both procedures were applied to characterize the organic material present as coatings in Roman and Egyptian amphorae. DE-MS successfully identified abietanic compounds, hence a diterpenic resinous material could be identified and its degree of oxidation assessed. GC/MS enabled us to identify dehydroabietic acid, 7-oxodehydroabietic acid, 15-hydroxy-7-oxodehydroabietic acid, 15-hydroxydehydroabietic acid, retene, tetrahydroretene, norabietatriene, norabietatetraene and methyl dehydroabietate. These oxidized and aromatized abietanes provided evidence that the amphorae examined were waterproofed with a pitch produced from resinous wood of plants from the Pinaceae family. The chemometric evaluation of the GC/MS data highlighted significant chemical differences between the pitches found in the two archaeological sites, basically related to differences in the production techniques of the materials and in their degradation pathways. 相似文献
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食品中胆固醇色谱/质谱/质谱的测定 总被引:3,自引:0,他引:3
确立了用色谱/质谱/质谱测定食品中胆固醇的一种新方法,试样经乙酸乙酯提取后,GC/MS/MS测定分析,以胆固醇分子离子为母离了,以其子离子为定量分析的碎片离子。线性好,回收率高,方法可靠。 相似文献