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  • 1
    Electronic Resource
    Electronic Resource
    Field desorption and fast atom bombardment mass spectrometry of pyridine nucleotides and nucleoside triphosphates (1985)
    Springer
    Fresenius' Zeitschrift für analytische Chemie 321 (1985), S. 531-537 
    Details
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The complete mass spectra of nicotinamide mononucleotide (free acid), β-nicotinamide adenine dinucleotide (free acid and lithium salt), dihydronicotinamide adenine dinucleotide (disodium salt), nicotinamide adenine dinucleotide phosphate (disodium salt) and adenosine-5′- triphosphate (disodium salt) are introduced. The first comparison of field desorption and fast atom bombardment mass spectrometry of these biologically active phosphates is reported. A critical evaluation of the merits and pitfalls of both soft ionization methods for the investigations of pyridine nucleotides and nucleoside triphosphates is given. In particular, the experimental difficulties for ionic desorption of organic phosphates in FD-MS and the basic problems of chemical noise as well as matrix/substance-interaction in FAB-MS are discussed.
    Notes: Zusammenfassung Erstmals werden die kompletten Massenspektren von Nicotinamid-Mononucleotid (freie Säure), β-Nicotinamid-Adenin-Dinucleotid (freie Säure und Lithiumsalz), Dihydronicotinamid-Adenine-Dinucleotid (Dinatriumsalz), Nicotinamid-Adenin-Dinucleotidphosphat (Dinatriumsalz) und Adenosin-5′-triphosphat (Dinatriumsalz) vorgestellt. Über einen ersten Vergleich der Felddesorptions- und Fast Atom Bombardment-Massenspektrometrie von diesen biologisch aktiven Phosphaten wird berichtet. Eine kritische Wertung der Vor- und Nachteile der beiden schonenden Ionisierungsverfahren für die Untersuchungen von Pyridin-Nucleotiden und Nucleosid-Triphosphaten wird gegeben. Insbesondere werden die experimentellen Schwierigkeiten der ionischen Desorption von organischen Phosphaten bei der FD-MS und die grundsätzlichen Probleme des chemischen Untergrundes sowie der Matrix/Substanz-Wechselwirkung bei FAB-MS angesprochen.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00464359
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  • 2
    Electronic Resource
    Electronic Resource
    Spiro-Verbindungen, VI. Stereoisomere Acorenone. PFT-13C-NMR-Spektren und massenspektroskopische Untersuchungen (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 1615-1622 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Spiro Compounds. VI. Stereoisomeric Acorenones. PFT 13C NMR Spectra and Mass Spectroscopic InvestigationsThe 13C NMR spectra of the four stereoisomeric acorenones 1-4 (1-isopropyl-4.8-dimethylspiro[4.5]dec-8-en-7-ones) allow the assignment of these spiranes to the 1,4-trans (1/2) or 1,4-cis (3/4) series, respectively; in case of the cis-isomers 3 and 4 the relative configuration at the spirochirality center C-5 can be determined.  -  Comparison of different intensities of corresponding ion pairs in the mass spectra of 1-4 allows the unequivocal discrimination of the four stereoisomers.
    Notes: Die 13C-NMR-Spektren der vier stereoisomeren Acorenone 1-4 (1-Isopropyl-4,8-dimethylspiro[4.5]dec-8-en-7-one) erlauben eine Zuordnung dieser Spirane zur 1,4-trans-(1/2) bzw. 1.4-cis-Reihe (3/4) und bei den cis-Isomeren 3 und 4 auch die relative Konfigurationsbestimmung am Spirochiralitätszentrum C-5.  -  Die Massenspektren von 1-4 ermöglichen an der unterschiedlichen Intensität entsprechender Ionenpaare die eindeutige Differenzierung aller vier Stereoisomeren.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771100504
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  • 3
    Electronic Resource
    Electronic Resource
    Beiträge zur Kenntnis des chromophoren Systems der Corrine, IV. Über die partielle, reversible Ringöffnung am Dicyano-cobyrin-säure-heptamethylester mit intermediärer reversibler Entfernung des Cobalts (1979)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1979 (1979), S. 811-825 
    Details
    ISSN: 0170-2041
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Contributions to the Knowledge of the Corrin Chromophore, IV. - Partial, Reversible Ring Cleavage of Dicyano-cobyrinic Heptamethyl Ester with Intermediate Reversible Removal of Cobalt
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.197919790611
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  • 4
    Electronic Resource
    Electronic Resource
    Soft ionization of biomolecules: A comparison of ten ionization methods for corrins and vitamin B12Devoted to Professor Dr. H. D. Beckey on occasion of his 65th birthday. (1986)
    New York, NY [u.a.] : Wiley-Blackwell
    Mass Spectrometry Reviews 5 (1986), S. 249-311 
    Details
    ISSN: 0277-7037
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Additional Material: 43 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mas.1280050303
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  • 5
    Electronic Resource
    Electronic Resource
    Synthesis of Deoxyoligonucleotide Linker Fragments for Genetic Engineering Using Improved Preparative and Analytical Techniques (1984)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1984 (1984), S. 835-853 
    Details
    ISSN: 0170-2041
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese von Desoxyoligonucleotid-Fragmenten zur Anwendung in der Genverknüpfung unter Einsatz verbesserter präparativer und analytischer MethodenZur Untersuchung der Expression rekombinanter DNS haben wir Oligonucleotide als Genverknüpfungsfragmente dargestellt, die spezifische Spaltstellen sowohl in die DNA wie in das zugehörige Protein einführen. Ihr Aufbau ist so, daß die Spaltung eines Fusionsproteins entweder durch Bromcyan oder durch Kollagenase erfolgen kann. Die Synthese wurde nach dem Triesterschema durchgeführt, wobei schnellere und einfachere Wege zu funktionalisierten Dinucleotid-Baueinheiten entwickelt wurden. Die Felddesorptions-Massenspektrometrie diente als Routine-methode für den Strukturbeweis und die Reinheitskontrolle dieser Baueinheiten.
    Notes: For studies on the expression of recombinant DNA, linker fragments have been prepared which serve to introduce specific points of cleavage on the DNA as well as the protein level. Such linkers were designed for cyanogen bromide as well as for collagenase cleavage of fused proteins. The preparation was done according to the triester synthesis scheme using improved and simpler routes to functionalized dinucleotide building blocks. Field desorption mass spectrometry was used as a routine tool for the identification and control of the purity of these units.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.198419840502
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  • 6
    Electronic Resource
    Electronic Resource
    Structural Investigations of 13-O-Demethyl-FK506 and Its Isomers Generated by in vitro Metabolism of FK506 Using Human-Liver Microsomes (1993)
    New York, NY : Wiley-Blackwell
    Helvetica Chimica Acta 76 (1993), S. 2288-2302 
    Details
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: FK506 is currently under investigation as immunosuppressant after organ transplantation and in immune diseases. The structure of a demethylated metabolite 1 of FK506 isolated after in vitro metabolism by human-liver microsomes was established using two-dimensional homo- and heteronuclear NMR experiments. The demethylation position was found to be at O—C(13) using HMBC spectra. In contrast to FK506, 7 different isomers could be differentiated in COSY, HMBC, and HMQC spectra. The intensity of their signals was 50:18:11:9:6:6 (one isomer could not be quantified). This isomerization may be explained by epimerization at C(10) or alternative formations of the hemiketal ring between C(10) and C(13) or C(9) and C(13), in addition to cis/trans-isomerism about the amide bond (see Scheme). The structural variation is possible by participation of the OH group at C(13) formed after demethylation and could be derived from HMBC spectra. Chemical exchange evidenced by ROESY spectra proved the rotational isomerism. NMR investigation of the structure of 13-O-demethyl-FK 506 (1) revealed at least seven isomers.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/hlca.19930760614
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