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  • 1
    Electronic Resource
    Electronic Resource
    Mathematical model for the optimization of the reaction between 2,3-bis(m-tolyl)quinolizinium bromide and piperidine using a factorial design (1992)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 6 (1992), S. 1-10 
    Details
    ISSN: 0886-9383
    Keywords: Derivatization reaction ; Factorial design ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A number of nucleophiles have been successfully identified and quantified using the Kröhnke reaction with 2,3-diphenyl derivatives of quinolizinium salts. Optimization of the reaction conditions by means of a mathematical model involving analysis of the response surface has led to a better understanding of the factors exerting an influence on the above reaction.The parameters chosen were temperature, reaction time, base concentration, water concentration and nucleophile concentration. The reaction was developed in polar aprotic solvents (acetone, acetonitrile). To facilitate the nucleophilic attack, the presence of an organic base (triethylamine) was necessary, although concentrations in excess of 0·15M did not alter the development of the reaction. Since pharmaceutical solutions are often aqueous, the influence of water on the reaction was studied. Low water volumes have no significant influence on the opening of the quinolizinium ring by the nucleophilic reagent. However, when the water proportion exceeded that of the organic solvent, the fluorescence intensity was lower than expected. Development of the fluorescent reaction product was first detected 5 min after the reaction started. The fluorescence intensity reached its optimum value after 138 min.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cem.1180060102
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    Paper (German National Licenses)
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  • 2
    Electronic Resource
    Electronic Resource
    Matrix-assisted laser desorption ionization for rapid determination of the sequences of biologically active peptides isolated from support-bound combinatorial peptide libraries (1994)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 8 (1994), S. 77-81 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A termination synthesis approach has been developed to encode each resin bead in support-bound combinatorial peptide libraries with the information needed to establish the sequence of the full-length products also contained on the beads. Matrix-assisted laser desorption ionization mass spectrometry was then used to rapidly read the appropriate sequences. In addition to rapid peptide sequencing, the technique allows direct assessment of the quality of the synthetic library, since deletion peptides, side-reaction products and incomplete-deprotection products are readily observed. An anti-gp120 monoclonal antibody was screened against a hexapeptide library, and eight active peptides were isolated. Six of the eight peptides were shown to possess the exact recognition sequence for the antibody.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290080115
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    Paper (German National Licenses)
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  • 3
    Electronic Resource
    Electronic Resource
    Thin layer chromatography/mass spectrometry: The advantages of tandem mass spectrometry (1992)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 6 (1992), S. 608-615 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The results of thin layer chromatography/mass spectrometry (TLC/MS) and thin layer chromatography/tandem mass spectrometry (TLC/MS/MS) experiments are described. Spectra from the analytes were obtained directly from the absorbent without the need for extraction prior to analysis by mass spectrometry. These results illustrate the added specificity that the tandem mass spectrometer can afford in the detection and characterization of a range of compounds separated by TLC.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290061005
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  • 4
    Electronic Resource
    Electronic Resource
    Antisense DNA oligonucleotides II: The use of matrix-assisted laser desorption/ionization mass spectrometry for the sequence verification of methylphosphonate oligodeoxyribonucleotides (1993)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 7 (1993), S. 195-200 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry has been used to measure accurately the molecular masses of synthetic methylphosphonate oligodeoxyribonucleotides, up to 18 nucleotides in length. A simple method has been developed for the complete sequence verification of these compounds, which are intractable by classical means. Sequencing from the 5′ end of the molecule is possible because of inefficiencies in the synthetic procedure. Complementary information from the 3′ end can be obtained by partial hydrolysis of the methylphosphonate backbone.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290070306
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  • 5
    Electronic Resource
    Electronic Resource
    Enhanced Resolution of Conjugated Linoleic Acid Isomers by Tandem-Column Silver-Ion High Performance Liquid Chromatography (1999)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 144-148 
    Details
    ISSN: 0935-6304
    Keywords: Conjugated linoleic acid (CLA) ; silver-ion high performance liquid chromatography (Ag+-HPLC) ; cheese ; analysis ; silver-ion chromatography ; tandem-column Ag+-HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A commercial mixture of conjugated linoleic acid (CLA) isomers, reportedly consisting of six components, was recently resolved into 12 peaks attributed to CLA isomers using silver-ion high performance liquid chromatography (Ag+-HPLC). In this study, the coupling of two analytical silver-ion high performance liquid chromatography columns (tandem-column Ag+-HPLC) in series led to the enhanced resolution of CLA isomers. Many CLA isomers were baseline resolved and the pair 18 : 2 8,10 c/t and 18 : 2 7,9 c/t found in cheese products, was resolved for the first time. In this work, a similar commercial CLA mixture was separated into 16 peaks, while CLA isomers from cheese also gave rise to 16 peaks. As expected, the CLA isomers were separated into three geometric groups in the order trans,trans, cis/trans, and cis,cis. Semi-preparative Ag+-HPLC, followed by gas chromatography-mass spectroscopy of the dimethyloxazoline derivatives, was used to confirm the identity of the newly resolved positional CLA isomers. The double bond configuration of CLA isomers was established by gas chromatography-Fourier transform infrared spectroscopy. Two minor t,t CLA isomers found in cheese, presumably 18 : 2 t6t8 and 18 : 2 t13t15, were also separated. The CLA isomeric composition of 16 commercial cheese products was determined.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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    Paper (German National Licenses)
  • 6
    Electronic Resource
    Electronic Resource
    Calculation of 2J(HH) and 1J(CH) for transition metal methyl compounds; evidence for geometric dependence of 2J(HH) (1987)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 25 (1987), S. 544-549 
    Details
    ISSN: 0749-1581
    Keywords: NMR Coupling constants ; TiCH3Cl3 Agostic ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Calculations of 2J(HH) and 1J(CH) for CH4, TiCl3CH3, Mn(CO)5CH3 and Zn(CH3)2 as a function of C-H distance and M—C—H angle have been carried out, based on the extended Hückel method. The positive geminal coupling constant found for TiCl3CH3 is shown to be caused by the small Ti—C—H angle, and the results suggest that the sign and magnitude of the geminal coupling constant in methyl groups could be a useful probe of their solution structure.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260250618
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