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51.
52.
Wolf Dietrich Krautgartner Ljubomir Vitkov Matthias Hannig Klaus Pelz Walter Stoiber 《Microscopy and microanalysis》2005,11(1):2-8
To examine new cytochemical aspects of the bacterial adhesion, a strain 41452/01 of the oral commensal Streptococcus sanguis and a wild strain of Staphylococcus aureus were grown with and without sucrose supplementation for 6 days. Osmiumtetraoxyde (OsO4), uranyl acetate (UA), ruthenium red (RR), cupromeronic blue (CB) staining with critical electrolytic concentrations (CECs), and the tannic acid-metal salt technique (TAMST) were applied for electron microscopy. Cytochemically, only RR-positive fimbriae in S. sanguis were visualized. By contrast, some types of fimbriae staining were observed in S. aureus glycocalyx: RR-positive, OsO4-positive, tannophilic and CB-positive with ceasing point at 0.3 M MgCl2. The CB staining with CEC, used for the first time for visualization of glycoproteins of bacterial glycocalyx, also reveals intacellular CB-positive substances-probably the monomeric molecules, that is, subunits forming the fimbriae via extracellular assembly. Thus, glycosylated components of the biofilm matrix can be reliably related to single cells. The visualization of intracellular components by CB with CEC enables clear distinction between S. aureus and other bacteria, which do not produce CB-positive substances. The small quantities of tannophilic substances found in S. aureus makes the use of TAMST for the same purpose difficult. The present work protocol enables, for the first time, a partial cytochemical differentiation of the bacterial glycocalyx. 相似文献
53.
F. Drawert W. Heimann und G. Tsantalis 《Fresenius' Journal of Analytical Chemistry》1967,228(3):170-180
Zusammenfassung Durch Direktinjektion von 5–20 l verschiedener Branntweine wurden auf gaschromatographischen Trennsäulen in Verbindung mit Flammenionisationsdetektoren die Verbindungen Acetaldehyd, Essigsäure-methylester, Essigsäure-äthylester, Methanol, Butanol-2, Propanol-1, 2-Methylpropanol-1, Butanol-1, 2-Methyl-butanol-1, 3-Methyl-butanol-1 und Hexanol-1 aufgetrennt und quantitativ bestimmt. Vergleiche der Analysenzahlen zeigen, daß sich die Branntweingruppen Obstbrände, Weinbrände und Getreidebrände deutlich voneinander abgrenzen und darüber hinaus z.B. zwischen Cognacs und Weinbränden bzw. zwischen schottischen, amerikanischen und kanadischen Whiskies unterschieden werden kann.
Summary By direct injection of 5–20 l of various spirits the following compounds can be separated and determined on gas-chromatographic columns using flame-ionization detectors: acetaldehyde, methyl acetate, ethyl acetate, methanol, butanol-2, propanol-1, 2-methyl-propanol-1, butanol-1, 2-methyl-butanol-1, 3-methyl-butanol-1 and hexanol-1. A comparison of the analytical results reveals distinct differences between spirits from fruit, wine and grain. Moreover, different analytical results are obtained for cognacs and (German) brandies, and for Scotch, American and Canadian whiskies.相似文献
54.
Witke K Götze J Rössler R Dietrich D Marx G 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2004,60(12):2903-2912
Samples of different three-dimensionally preserved fossil plants (Medullosa sp., Dadoxylon sp., Calamodendron striatum, Psaronius sp.) from the Lower Permian petrified forest of Chemnitz were examined with regard to their chemical composition and structural order. Raman spectroscopy and cathodoluminescence microscopy are shown to be powerful tools for such investigations. Silicified wood from Chemnitz-Hilbersdorf generally shows yellow cathodoluminescence (CL) of the cell walls and only weak yellow-brownish CL of the cell lumina. By time-resolved cathodoluminescence spectroscopy, a secondary mineralisation of hydrothermal origin was recognized. The latter is shown by short-lived blue CL at the cell walls extinguishing the yellow signal. Therefore, after the primary silicification step a secondary mineralisation step initiated by hydrothermal processes, seems to have taken place at probably slightly higher temperatures. The resulting silica matrix consists of phanerocrystalline and microcrystalline alpha-quartz as well as microcrystalline moganite, both partially associated with iron oxides. Dadoxylon sp. is a prominent example for parallel permineralisation by alpha-quartz and fluorspar, which is outstanding for the Chemnitz Petrified Forest. CL on this samples shows parallel silicification and fluoritisation, followed by infiltration of iron oxides. Permineralised samples show very low percentage of original organic remains. The seed fern Medullosa, for example, shows dispersed carbon, which is mainly restricted to the centres of the typical star-shaped vascular bundles. Raman spectroscopy revealed that these carbonaceous particles are of an anthracite structure. For experimental confirmation coal samples of different rank, especially anthracite from different geological times and localities, were studied by means of Raman spectroscopy. The remaining pith of the vascular bundles is white-coloured and consists of alpha-quartz and moganite, whereas surrounding tracheides exhibit white and reddish coloured parts. The reddish parts, mainly found in the rays, additionally contain alpha-Fe2O3 and Fe3O4 among the SiO2 polymorphs of alpha-quartz and moganite. Sometimes iron oxides could have dominated permineralisation processes as the peak intensities of distinct parts of the samples suggest. 相似文献
55.
Uwe Klingebiel Dietrich Fischer Prof. Dr. Anton Meller 《Monatshefte für Chemie / Chemical Monthly》1975,106(2):459-471
The reaction of aminofluorsilanes of the type (R=H,F) (Me 3Si)2N?SiF2R with two moles of ammonia, or of a mono- or dialkylamine, yields the corresponding amino-compounds, e.g. (Me 3Si)2N?Si(F)R?NH2, (Me 3Si)2N?Si(F)R?NHR′ and (Me 3Si)2N?Si(F)R?NR2′ (R′=Me, Et). Analogous products are obtained by reaction of the aminofluorosilanes with lithium salts of amines with bulky organic substituents in a 1 : 1 molar ratio. Alkoxy- and aryloxyaminofluorosilanes are prepared by the reaction of sodium alcoholates and sodium phenolate with (Me 3Si)2N?Si(F2)R (R=H, C2H3, C2H5, C6H5). The i.r.-, mass-,1H- and19F-NMR spectra of the above compounds are reported. 相似文献
56.
Zusammenfassung Es wird ein einfaches Verfahren zur Dünnschichtchromatographie von Phenol sowie isomeren Kresolen und Xylenolen auf formamidimprägnierten Kieselgel-G-Platten beschrieben. Die Methode läßt sich direkt auf die Analyse solcher Weichmacher anwenden, bei deren Verseifung Phenole entstehen.
Summary The separation and identification of phenol and the isomeric cresols and xylenols by thin-layer chromatography on silica gel plates impregnated with formamide is described. The method is applicable to the direct analysis of phenols from saponificated plasticizers.相似文献
57.
Keil O LeRiche T Deppe H Volmer DA 《Rapid communications in mass spectrometry : RCM》2002,16(8):814-820
This paper focuses on the technical aspects of chemical screening from 384-well plate nano-scale single-bead combinatorial libraries. The analytical technique utilized is a combination of capillary liquid chromatography with ultraviolet detection and matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. The HPLC/MALDI-MS hyphenation is achieved by means of a micro-fraction collector with a peak detection system that automatically collects the peaks onto the MALDI targets for subsequent characterization. Several experimental parameters such as type of 384-well plate, well-plate sealing foils, and a column-switching procedure were investigated using a small test library of nine components. Additionally, the influence of different MALDI matrices, different MALDI targets and sample-spotting techniques on the MALDI detection sensitivity as well as the ruggedness and sample throughput capacity of this technique were studied. Optimum results for the analytes investigated were obtained with 2,5-dihydroxybenzoic acid using on-line mixing of HPLC effluent and matrix solution. To demonstrate the potential of this capillary HPLC/MALDI-TOFMS method, its application to several single-bead libraries was investigated. The instrumental method allowed for the rapid identification and purity assessment of combinatorial libraries with detection limits down to the higher femtomole level using both UV detection and MALDI mass spectrometry. 相似文献
58.
59.
Zoltan Bajko Dietrich Gudat Falk Lissner Martin Nieger Thomas Schleid 《无机化学与普通化学杂志》2004,630(12):1969-1976
Phosphonio‐benzo[c]phospholides with an additional phosphonium ylide substituent in 3‐position were synthesized by deprotonation of appropriately substituted 1, 3‐bis‐phosphonio benzophospholide cations and characterized by spectroscopic and analytical data. The ability of these molecules to act as bidentate P, C‐chelating ligands to transition metal atoms was demonstrated in the reactions with [W(CO)4(norbornadiene)] and [MCl2(cyclooctadiene)] (M = Pd, Pt). The PdII and PtII complexes are distinguished by a strong inclination towards addition of H2O to the 10π‐electron system of the ligand. The molecular structures of a W0 complex with a P, C‐chelating ylidyl‐phosphonio‐benzophospholide ligand and of the product resulting from H2O‐addition to a corresponding PtII complex were determined. The structural parameters of the W0 complex provide evidence for the presence of substantial steric strain around the metal atom. 相似文献
60.
Hatsis P Brombacher S Corr J Kovarik P Volmer DA 《Rapid communications in mass spectrometry : RCM》2003,17(20):2303-2309
In this work, a high repetition rate laser matrix-assisted laser desorption/ionization (MALDI) source is studied on a quadrupole-time-of-flight (QqTOF) and a triple quadrupole (QqQ) mass spectrometer for rapid quantification of small pharmaceutical drugs. The high repetition rate laser allows an up to 100-fold higher pulse frequency as compared with regular MALDI lasers, resulting in much larger sample throughput and number of accumulated spectra. This increases the reproducibility of signal intensities considerably, with average values being around 5% relative standard deviation after taking into account the area ratio of the analyte to an internal standard. Experiments were conducted in MS/MS mode to circumvent the large chemical background due to MALDI matrix ions in the low mass range. The dynamic range of calibration curves on the QqTOF mass spectrometer extended over at least two orders of magnitude, whereas on the QqQ it extended over at least three orders of magnitude. Detection limits ranged from 60-400 pg/microL on the QqTOF and from 6-70 pg/microL on the QqQ for a series of benzodiazepines. The benzodiazepine content of commercial pill formulations was quantified, and less than 5% error was obtained between the present method and the manufacturer's certified values. Furthermore, a high sample throughput was achieved with this method, so that a single MALDI spot could be quantitatively scanned in as little as 15 s, and an entire 96-well MALDI plate in 24 min. 相似文献