Coating of carbon fibers with adhesion-promoting thin poly(acrylic acid) and poly(hydroxyethylmethacrylate) layers using electrospray ionization

Thin coatings of poly(acrylic acid) (PAA) and poly(hydroxyethylmethacrylate) (PHEMA) were deposited onto carbon fibers by means of the electrospray ionization (ESI) technique in ambient air. These high-molecular weight polymer layers were used as adhesion promoters in carbon fiber–epoxy resin composites. Within the ESI process, the carbon fibers were completely enwrapped with polymer in the upper 10 plies of a carbon fiber roving. As identified with scanning electron microscopy also shadowed fibers in a bundle as well as backsides of fiber rovings were pinhole-free coated with polymers (‘electrophoretic effect’). Under the conditions used, the layers have a granular structure. Residual solvent was absent in the deposit. PAA and PHEMA films did not show any changes in composition and structure in comparison with the original polymers as analyzed by X-ray photo-electron spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Single-fiber pullout tests of coated fibers embedded in epoxy resin showed significantly increased interfacial shear strength. It is assumed that chemical bonds between carbon fiber poly(acrylic acid) and epoxy resin contribute significantly to the improved interactions.     

高效液相色谱-电喷雾质谱联用法检测大豆异黄酮和皂苷

应用高效液相色谱 电喷雾质谱联用法 ,直接对大豆胚芽的 70 %乙醇室温提取液进行检测 .根据各色谱峰的质谱特征 ,在室温提取液中鉴定出 9种异黄酮 ,7种A组皂苷 ,4种B组皂苷和2种E组皂苷 .结果证明对于复杂天然产物的定性定量分析 ,高效液相色谱 电喷雾质谱 (HPLC/ESI MS)联用分析法是一种方便快捷有效的方法 .     

Limited contribution of isoflavones to hepatocellular phase II enzyme-inducing activity of soybean (Glycine max) extracts

Soy flour was successively extracted with ethyl acetate, ethanol, and water and tested for quinone reductase (QR) induction in the Hepa 1c1c7 cell line. The ethanol extract was found to be the most potent, with a CD value (concentration required to double QR specific activity) of 460 μg/ml. Phase separation of the ethanol extract and a phospholipid removal procedure yielded a fraction that doubled QR at 80 μg/ml. Reverse phase medium pressure chromatography of the purified ethanol extract yielded 13 fractions. Constituents of selected fractions were identified using mass spectrometry and NMR analysis. Fractions 2, 8, and 10 contained 47% of the recovered mass and were the least active of the isolates. These three fractions contained isoflavone glycosides. The latest eluting fractions 11–13 were found to be the most potent, and contained the majority of recovered inducing units (IUs), a measure of potency.     

FDE:一种有效的动态网页传送方法

在作者的片段自动探测算法基础上,提出了一种基于网页片段的Delta编码方法FDE,它能够重用片段和相似片段内容,并且也能透明地部署在现有的万维网基础设施上.实验结果显示,与传统方法相比,FDE方法能够有效地提高带宽利用率,同时可进一步减少页面传送的延迟.     

Investigation of chemical transformations of thiophenylglycoside of muramyl dipeptide on the fumed silica surface using TPD-MS,FTIR spectroscopy and ES IT MS

In this study, chemical transformations of benzyl ester of О-(phenyl-2-acetamido-2,3-dideoxy-1-thio-β-d-glucopyranoside-3-yl)-d-lactoyl-l-alanyl-d-isoglutamine (SPhMDPOBn) on the fumed silica surface were examined, and the surface complex structure was characterized by temperature-programmed desorption mass spectrometry (TPD-MS), infrared spectroscopy (FTIR) and electrospray ion trap mass spectrometry (ES IT MS). Stages of pyrolysis of SPhMDPOBn in pristine state and on the silica surface have been determined. Probably, hydrogen-bonded complex forms between silanol surface groups and the C = O group of the acetamide moiety NH-(CH₃)-C = O…H-O-Si≡. The thermal transformations of such hydrogen-bonded complex result in pyrolysis of SPhMDPOBn immobilized on the silica surface under TPD-MS conditions. The shifts ∆ν of amide I band (measured from 1,626 to 1,639 cm^−l for SPhMDPOBn in pristine state) of 33 and 35 cm^−l which occurred when SPhMDPOBn was immobilized on the silica surface may be caused by a weakening of the intramolecular hydrogen bonding of the SPhMDPOBn because the interaction with the silica surface as hydrogen bond with silanol groups is weaker than that in associates.     

Electron spectroscopic imaging of the morphology of in situ polyethylene ‘shish kebabs’

The simultaneous imaging of the crystalline and rigid amorphous areas of semi-crystalline polyethylene is made possible by electron spectroscopic imaging (ESI) in an energy-filtering transmission electron microscope (EFTEM). Conventional bright-and dark-field imaging modes mainly provide information about the non-crystalline areas which react chemically with classical staining agents such as ruthenium tetroxide. The ability of ESI to image structures which are inaccessible to the staining agent is shown in TEM micrographs of nascent polyethylene ‘shish kebabs’ embedded in a Lowicryl HM20 matrix.     

A method for the determination of acrylamide in bakery products using ion trap LC-ESI-MS/MS

Acrylamide levels of bakery products, e. g., bread and bread rolls, are usually below 100 microg/kg , often even below 50 microg/kg. Therefore, usual analytical methods which have an LOQ greater, not dbl equals 25 microg/kg are not sensitive enough for detailed investigations on acrylamide formation within these commodities. An improved method for trace level determination of acrylamide in bakery products was developed using ion trap LC-ESI-MS/MS. Samples were divided into crumbs and crusts to achieve an initial concentration by removing the crumbs since these are devoid of acrylamide. After sample extraction and clean-up using multimode SPE cartridges, further analyte enrichment was accomplished by solid-phase-supported liquid-liquid extraction with ethyl acetate prior to LC-MS/MS analysis. The method was evaluated using bread, bread rolls, alkali-baked bread rolls, and toast. LOQ was calculated from the confidence interval of the calibration curve and found to be 1.7 ng/mL, corresponding to 17 microg/kg of product. When crumbs and crusts were separated, an LOQ of 10.2 microg/kg of bakery product could be obtained. As demonstrated in preliminary comparative analyses, accuracy of the method met the requirements for determination of trace level acrylamide formation in bakery products. Mean recovery was 102.4% (CV 4.5%), intermediate reproducibility revealed a CV of 2.1%, and a repeatability of CV 6.0%.     

一种用于ESI离子源的可控高压直流电源的研究

介绍了一种用于电喷雾离子源的可控高压直流电源。分析了它的电场控制原理,讨论了它的硬件组成,具体给出了它的功能原理电路及其电路功能的实现。     

Assessment of phenolic profile of Turkish honeys

In this study, phenolic profile and antioxidant activity of 60 Turkish honey samples of nineteen different floral origins were evaluated by ultra-performance liquid chromatography with electrospray ionization coupled to tandem mass spectrometry, providing the identification of 32 phenolic compounds. Thyme (1051.58 mg/kg), pine (994.18 mg/kg), carob (935.03 mg/kg), eucalyptus (814.46 mg/kg), rhododendron (680.71 mg/kg), heather (562.59 mg/kg), cedar (561.83 mg/kg), and euphorbia (501.64 mg/kg) present significantly high phenolic content. Moreover ferulic, homogentisic, gentisic, syringic, 3,4-dihydroxybenzoic, caffeic, vanillic, p-coumaric, 4-hydroxy benzoic, and trans-2-hydroxy cinnamic acids were the most abundant of the determined compounds. The antioxidant activities of the honeys were evaluated by β-carotene-linoleic acid inhibition, DPPH free radical scavenging activity and ABTS⁺ cation radical scavenging activity which were measured as IC₅₀: 10.87 – 48.23 µg/mL, SC₅₀: 54.33 – 99.40 µg/mL and SC₅₀: 10.33 – 41.20 µg/mL, respectively. Phenolic compounds are considered antioxidant constituents, and they could be stated as components that account for antioxidant activity in Turkish honeys.     

Non‐galloylated and galloylated proanthocyanidin oligomers in grape seeds from Vitus vinifera L. cv. Graciano,Tempranillo and Cabernet Sauvignon

Non‐galloylated and galloylated flavan‐3‐ol composition in seeds from Vitis vinifera L. var. Graciano, Tempranillo and Cabernet Sauvignon grapes harvested in 2000, 2001 and 2002 at the same geographical area were determined using normal‐phase HPLC coupled with electrospray ionization mass spectrometry (LC/ESI‐MS) detection. Non‐galloylated and monogalloylated flavan‐3‐ols up to octamers, and di‐, and trigalloylated flavan‐3‐ols up to heptamers were identified in all grape seeds. Comparisons of the flavan‐3‐ol composition in three grape varieties harvested in three different years indicate that levels of non‐galloylated flavan‐3‐ols decrease as the degree of polymerization increased, whereas the monogalloylated dimers were present in the highest levels in all varieties and vintages. The levels of other monogalloylated flavan‐3‐ols varied in different vintages. Tempranillo contained the lowest levels of non‐galloylated and monogalloylated flavan‐3‐ols, whereas Graciano contained the highest levels, with the exception of non‐galloylated flavan‐3‐ols in vintage 2001, and non‐galloylated monomers in vintages 2000 and 2002. Grape seeds from vintage 2000 contained the highest levels of both non‐galloylated and galloylated structures. Statistical analyses indicate that the distribution of the flavan‐3‐ols is primarily determined by genetic factors and is also strongly influenced by climate conditions. Copyright © 2006 Society of Chemical Industry