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  • 1
    Electronic Resource
    Electronic Resource
    Quantitative determination of valproic acid and 14 metabolities in serum and urine by gas chromatography/mass spectrometry (1992)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 6 (1992), S. 24-29 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method for the determination of the antiepileptic drug valproic acid and 14 of its metabolites in serum and urine by gas chromatography/mass spectrometry with selected ion monitoring of the trimethylsilylated derivatives has been developed. Sample preparation, including hydrolysis of VPA-conjugates and removal of urea in urine is carried out at pH 5.0 and is rapid and simple. The samples are extracted with ethyl acetate and the concentrated extracts are trimethylsilylated. Analysis with adequate separation of metabolites is achieved with a DB 1701 fused silica (Megabore) capillary column. The method exhibits high recovery and reproducibility and is sufficiently sensitive and selective for analysis of small sample volumes. Application of the method for screening patient serum and urine samples for unusual metabolite patterns, with possible predictive value for early detection of liver injury, is presented.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130060108
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  • 2
    Electronic Resource
    Electronic Resource
    Polypeptide sequencing by a gas chromatograph mass spectrometer computer system: II - characterization of complex mixtures of oligopeptides as trimethylsilylated polyamino alcoholsA1, A2,… ions corresponding to the N-terminal amino acid, dipeptide… in the peptide derivatives used (polyamino alcohol-OTMS-ethers). Z1, Z2 … ions corresponding to the C-terminal amino acid, dipeptide … in the peptide derivatives used. R … sidechain of amino acids (as derivatized). Δ, contribution of amino acids to the retention index value of a derivatized peptide molecule. (1975)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 2 (1975), S. 326-339 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complex mixtures of O-trimethylsilylated polyamino alcohols, which have been generated by either acid or enzymatic hydrolysis of polypeptides and subsequent derivatization, are completely characterized by a gas chromatograph mass spectrometer computer system. These peptide derivatives possess excellent gas chromatographic properties; a wide range of derivatives from di- to hexapeptides may be separated in a single chromatographic experiment. The identification of these compounds, either manually or with the assistance of the computer, is based on three sets of data which are automatically generated after the g.c.m.s. computer experiment: (1) mass spectra, which exhibit sequence-determining ions of high abundance; (2) selected ion records, which allow efficient location of peptide derivatives in the gas chromatogram as well as resolution of incompletely separated fractions; (3) retention indices, which can be calculated from values which have been assigned to each amino acid residue.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200020608
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  • 3
    Electronic Resource
    Electronic Resource
    Polypeptide sequencing by a gas chromatograph mass spectrometer computer system: I - generation and derivatization of complex mixtures of oligopeptidesDAP I and DAP IV = dipeptidylaminopeptidases I and IV. (1975)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 2 (1975), S. 313-325 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A generally applicable strategy for polypeptide sequencing has been developed which involves cleavage of a large peptide (for example, primary degradation peptides obtained by tryptic or cyanogen bromide cleavage of a protein) to a mixture of small peptides whose individual amino acid sequences are then determined without their prior isolation. This is accomplished by conversion of the peptide mixture into the corresponding mixture of O-trimethylsilylated polyamino alcohols through reduction of the N-acetylated peptide esters with lithium aluminum deuteride, followed by treatment with trimethylsilyldiethylamine. The conditions for the enzymatic or chemical cleavage were optimized to yield mixtures of peptides best suited for this technique and which represented complete overlap. Limited acid hydrolysis combined with a second experimen utilizing either an enzyme with broad specificity, a set of enzymes, or dipeptidyl aminopeptidase I on the original and/or Edman-degraded molecule was found to be the best choice. This sequencing strategy was evaluated using 0.4 to 1.4 μmol of peptides with known structures (ribonuclease S-peptide, glucagon) and then applied to primary degradation peptides of rabbit skeletal muscle actin up to twenty amino acids long (0.4 to 1 μmol per experiment).
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200020607
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  • 4
    Electronic Resource
    Electronic Resource
    Zur Kenntnis der Phasen A2-2xSn5+xCl12 (A = K, In) (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 558 (1988), S. 193-200 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the A2-2xSn5+xCl12 (A = K, In) PhasesThe refinement of the structure of A2-2xSn5+xCl12 compounds (A = K+, In+) with single crystal data is reported. They crystallize with the Th7S12 type arrangement (a = 1192(2) pm, c = 428.9(8) pm (K-compound); a = 1189.8(6) pm, c = 431.2(3) pm (In-compound)) for which we propose the space group P6. The possibility of meroedric twinning is discussed. Due to the composition of these compounds the structure is necessarily disordered and this leads to a wide range of homogeneity which can be influenced by the size and the polarity of the A type cation.
    Notes: Wir berichten über die Strukturverfeinerung von A2-2xSn5+xCl12-Verbindungen (A = K+ bzw. In+) mit Einkristallmethoden. Sie kristallieren im Th7S12-Strukturtyp (a = 1192(2) pm, c = 428,9(8) pm (K-Salz); a = 1189,8(6) pm, c = 431,2(3) pm (In-Salz)), den wir in der Raumgruppe P6 beschreiben. Darüber hinaus diskutieren wir die Möglichkeit einer meroedrischen Verzwillingung. Die Struktur dieser Verbindungen ist aufgrund ihrer Zusammensetzung zwangsläufig ungeordnet, und dies führt zu einer beträchtlichen nichtstöchiometrischen Phasenbreite, die offensichtlich durch die Größe und Polarität des A-Kations beeinflußt werden kann.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885580119
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  • 5
    Electronic Resource
    Electronic Resource
    Zur Kenntnis des quasi-binären Systems InCl—SnCl2 und eine Anmerkung zum System KCl—SnCl2Professor Albrecht Rabenau zum 65. Geburtstage am 17. November 1987 gewidmet (1987)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 554 (1987), S. 43-49 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Quasi-binary System InCl—SnCl2 and a Remark on the System KCl—SnCl2We report the phase diagrams of the quasi-binary systems InCl/SnCl2 and KCl/SnCl2 derived from DTA and X-ray investigations. In both systems we find a nonstoichiometric phase having the formula A2-2xSn5+xC12 (with 0 ≤ x ≤ 0.15 for A = In and 0 ≤ x ≤ 0.14 for A = K), a peritectic ASn2Cl5 compound and a dystectic 1:1 phase. The nonstoichiometric phases are both isotypic with Th7S12. KSn2Cl5 crystallizes with a tetragonal NH4Pb2Br5-type structure (sp. gr. 14/mcm; a = 803.55(3), c = 1387.5(5) pm) and InSn2Cl5 with a monoclinic NH4Pb2Cl5-type arrangement (sp. gr. P21/c; a = 891.7(3), b = 800.2(3), c = 1251.0(4) pm, β = 89.55(5)°). The lattice constants for InSnCl3 (a = 1680(3), b = 799.2(9), c = 845.4(10) pm, β = 90.8(1)°) were derived by indexing the X-ray powder diagram. In addition the InCl—SnCl2 system contains a peritectic In4SnCl6 phase (sp. gr. Pmma; a = 1270(2), b = 2515(3), c = 1456 (1) pm, (single crystal data)) and a dystectic In9SnCl11 compound (tetragonal primitive; a = 864.6(2), c = 1219.3(6) pm (derived from indexed powder data)).
    Notes: Wir berichten über die Phasendiagramme der quasi-binären Systeme InCl—SnCl2 und KCl—SnCl2, die wir aus DTA- und Röntgenuntersuchngen abgeleitet haben. In beiden Systemen existiert eine nichtstöchiometrische Phase der Zusammensetzung A2-2xSn5+xCl12 (wobei 0 ≤ x ≤ 0,15 für A = In bzw. 0 ≤ x ≤ 0.14 für A = K), eine peritektische Verbindung des Typs ASn2Cl5 und eine dystektische 1:1 Verbindung. Die nichtstöchiometrischen Phasen sind beide isotyp zu Th7S12. KSn2Cl5 kristallisiert im tetragonalen NH4Pb2Br5-Typ (R.G. 14/mcm; a = 803,55(3), c = 1387,5(5) pm), InSn2Cl5 im monoklinen NH4Pb2Cl5-Typ (R.G. P21/c; a = 891,7(3) b = 800,2(3), c = 1251,0(4) pm, β = 89,55(5)°). Für InSnCl3 (a = 1680(3), b = 799,2(9), c = 845,4(10) pm, β = 90,8(1)°) wurden die Gitterkonstanten nur aus indizierten Röntgenplverdiagrammen abgeleitet. Im InCl—SnCl2-System gibt es zusätzlich eine peritektische In4SnCl6-Verbindung (R.G. Pmma; a = 1270(2), b = 2515(3), c = 1456(1) pm, (abgeleitet aus Einkristalldaten)) und eine dystektische In9SnCl11-Verbindung (tetragonal primitiv; a = 864,6(2), c = 1219,3(6) pm, (aus der Indizierung des Pulverdiagramms)).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19875541106
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  • 6
    Electronic Resource
    Electronic Resource
    A Study on AB2X5 Compounds (A: K, In, Tl; B: Sr, Sn, Pb; X: Cl, Br, I) (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 536 (1986), S. 35-44 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Über AB2X5-Verbindungen (A:K, In, Tl; B: Sr, Sn, Pb; X: Cl, Br, I)Wir berichten über die Synthese und die Gitterkonstanten von AB2X5-Verbindungen mit A = K, In, B = Sr, Sn, Pb und X = Cl, Br, I. Alle Verbindungen haben entweder die monokline NH4Pb2Cl5- oder die tetragonale NH4Pb2Br5-Struktur. Am Beispiel des KPb2Br5 wird gezeigt, daß die monokline Struktur bei Hochtemperatur- und die tetragonale bei Hochdruckbedingungen ausgebildet wird. Die Existenzbereiche der beiden Strukturtypen lassen sich abgrenzen in einem Strukturfelddiagramm auf der Grundlage der Größenverhältnisse A/X und B/X.
    Notes: The synthesis and the lattice constants of AB2X5 compounds with A = K, In, B = Sr, Sn, Pb and X = Cl, Br, I are reported. All compounds have either the monoclinic NH4Pb2Cl5 or the tetragonal NH4Pb2Br5 structure. For KPb2Br5 the former is shown to be the high temperature form and the latter is obtained under high pressure. It is shown that all known compounds of this family can clearly be separated with respect to their structure in a structure field diagram on the basis of the size relations A/X and B/X.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19865360505
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