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  • 04. Solid Earth::04.08. Volcanology::04.08.06. Volcano monitoring  (31)
  • BIOSCIENCES  (23)
  • GEOPHYSICS  (17)
  • Analytical Chemistry and Spectroscopy  (14)
  • 1
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 918-926 
    ISSN: 0887-6134
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A negative ion chemical ionization (NICI) gas chromatographic/mass spectrometric method is described for the identification of 15 valproic acid (VPA) metabolites as their pentafluorobenzyl derivatives. Samples analyzed were serum, urine and saliva taken from a volunteer on VPA at steady state and also given selected doses of (2H6)VPA. Metabolite peaks were identified by comparison to synthetic standards. All the metabolites, like the parent drug, produced abundant [M - 181]- ions, except 3-keto VPA, which gave an [M - 181 - CO2]- ion. Using the NICI method, two new VPA metabolites were identified. One of these metabolites was characterized as 4′-keto-2-ene VPA by synthesis, while the second one appeared to be a positional isomer of 4′-keto-2-ene VPA. The sensitivity of the method was also sufficient to detect metabolites of VPA in saliva. The ratio of the levels of (Z)-2-ene VPA to (E)-2-ene VPA was much greater in saliva than in serum, suggesting stereoselective plasma protein binding or transport of these two metabolites. The lower limit of detection for the quantification of VPA in serum or saliva was 2 ng ml-1.
    Zusätzliches Material: 11 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 2
    Digitale Medien
    Digitale Medien
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 6 (1994), S. 5-10 
    ISSN: 1040-7685
    Schlagwort(e): caffeine ; coffee ; micellar electrokinetic capillary chromatography (MECC) ; reproducibility ; HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Samples of regular and decaffeinated varieties of green coffee beans, instant coffee, and “roast & grind” coffee have been examined by micellar electrokinetic capillary chromatography (MECC). The separation conditions affecting the reproducibility of the determination of caffeine in these samples are presented. Sodium dodecyl sulfate (SDS) and cetyltrimethylammonium chloride (CTAC) Were employed to demonstrate the role of the surfactant system in reproducibility. The use of NaOH and HCl was explored for column rinsing to enhance the stability of the electroosmotic flow. The levels of caffeine ranged from 3.95% (by weight) for regular coffee to 0.07% for decaffeinated coffee. The relative standard deviation (RSD) for the migration time of the peak corresponding to caffeine in coffee samples was 0.74%. The RSDs for the peak areas and heights were 1.04 and 2.07%, respectively. The results of the quantitation of caffeine by MECC are compared to levels determined by high-performance liquid chromatography (HPLC).
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 3
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 12 (1985), S. 405-408 
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The electron impact induced fragmentations observed in the mass spectra of eight 1,4-diene-3-ketopregnane steroids are described. The effect of hydroxyl substituents in positions 11β, 17α and 21, on the typical fragmentation pattern is analysed; in particular the ‘long range’ effect of the 17α-hydroxy group on the relative abundance of the ions m/z 121 and 122 is confirmed using specific deuterium labelling.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 4
    ISSN: 1076-5174
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: The production and detection of doubly charged organic cations were studied using a previously unreported approach - electrospray ionization coupled with Fourier transform ion cyclotron resonance mass spectrometry. Owing to its ultra-high mass resolution, accurate and stable mass calibration, multiple stages of collisionally activated dissociation (CAD) allowing tandem mass spectrometry and extremely long ion storage times (〉 1 min), this technique has proven to be a powerful method for the detection and study of doubly charged organic compounds. CAD studies were used for the identification of ion-molecule reactions and for the investigation of the propensity towards gas-phase SN1 and SN2 reaction pathways. To date exclusively SN1-type reactions in the gas phase have been detected. Three doubly charged pyridinium salts were chosen as model compounds for this study.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 5
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 523-528 
    ISSN: 0935-6304
    Schlagwort(e): Nonaqueous solvents ; Capillary electrophoresis ; Capillary electrochromatography ; Current measurement ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The solvents acetonitrile, methanol, N, N-dimethylformamide, dimethyl sulfoxide, formamide, and deionized water were investigated for their ability to support current flow without added electrolyte. Using open tubular capillary electrophoresis, currents were measured to be in the nanoampere (10-9 A) range for all solvents but formamide (10-6 A). Comparisons with flow data showed no clear relationship between current and electroosmotic flow. Packed capillary columns (3-μm ODS) were used for separations using both pure solvent and hydrophobic dyes showed mild retention in pure ACN. A 16 polynuclear aromatic hydrocarbon (PAH) standard soluton was separated in 80/20 ACN/H2O with reduced plate heights (h) between 2.8 and 3.1 for retained species. A separation of nine androstenediones was achieved using a 70/30 MeOH/H2O mobile phase.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 6
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 22 (1984), S. 586-591 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The 13C NMR spectra of sixteen 4-ene-3-keto- and 1,4-diene-3-keto corticosteroids are described. Substituent shifts and the effect of added methanol-d4 are reported, and conformational distortions and intramolecular hydrogen bonding are analysed based on these data.
    Zusätzliches Material: 4 Tab.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 7
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: The empirical correlation method δ = is discussed in general terms for a large number of halogenated compounds and new diamagnetic anisotropy corrections are determined. The significance of these corrections is critically examined. Careful analysis of the data permitted the establishment of the limitation of this method.
    Notizen: La corrélation empirique δ = est étendue à un grand nombre de composés halogénés et de nouvelles corrections d'anisotropie diamagnétique sont déterminées. La signification de ces corrections est discutée et une analyse soignée des données permet de fixer les limites de la méthode.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 8
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 11 (1978), S. 275-280 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The 19F NMR chemical shifts and geminal FCP and FCH coupling constants are reported for a number of fluorinated quaternary phosphonium salts of the type \documentclass{article}\pagestyle{empty}\begin{document}$ [{\rm R}_3 \mathop {\rm P}\limits^ \oplus {\rm CFXY}]{\rm Z}^ \ominus $\end{document}, where generally R = alkyl or aryl; X, Y = hydrogen or halogen and Z = halogen. Spectral parameters remain relatively unaffected upon variance of R, Z-, and/or solvent, except when R is a bulky alkyl group. Linear relationships accurately describe the correlation between the summation of the electronegativities of X and Y, or simply of Y if X = F, and the 19F NMR chemical shift and geminal FCP coupling constant; geminal FCH coupling constants show no such dependence. These relationships are of demonstrated analytical value, particularly for the purpose of spectral prediction.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 9
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 24 (1986), S. 829-831 
    ISSN: 0749-1581
    Schlagwort(e): Indole ; indole derivatives ; 13C NMR spectra ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: 13C chemical shifts for indole and ten indoles substituted at positions 1, 3 and/or 6 are reported. Previous assignments have been revised using specific deuterium labelling and selective proton decoupling.
    Zusätzliches Material: 2 Tab.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 10
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 33 (1995), S. 201-211 
    ISSN: 0749-1581
    Schlagwort(e): superspin ; BIRD pulses ; spin dynamics ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The BIRD pulse sequence is widely used to distinguish between protons that are directly bonded to a 13C nucleus and those that are not. It consists of a proton 90° pulse, a delay of 1/(21JCH), simultaneous carbon and proton 180° pulses, a further delay of 1/2J and a final proton 90° pulse. For two spins at equilibrium, the effect of this sequence can be easily understood, but for complex systems the behaviour can be counter-intuitive. This paper explains the general behaviour of the BIRD sequence using theoretical equations and numerical simulations, and discusses some practical applications of the BIRD pulse train. The theoretical equations are derived using tables of general behaviour for the spin systems AX, AX2 and AX3. The tables allow the exact calculation of the effect of any pulse sequence on these spin systems, including all multiple quantum effects. The simulations show that the sequence is usually robust with respect to pulse imperfections and non-ideal spin systems. In other cases, particularly when signals should be suppressed, small errors can have dramatic consequences. The results derived here are for a BIRD sequence inserted into an INEPT experiment, but many of the conclusions can be applied to all of the more standard applications of the BIRD.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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