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  • 1
    Digitale Medien
    Digitale Medien
    Trends in product analysis for research in the pharmaceutical industry (1991)
    Springer
    Microchimica acta 104 (1991), S. 103-112 
    Details
    ISSN: 1436-5073
    Schlagwort(e): product analysis ; pharmaceutical industry ; research in analytical chemistry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Abstract Characterization of substances and formulations with respect to purity and stability is a major analytical chemical task during product development in the pharmaceutical industry. The importance of separation methods, especially liquid chromatography, is shown with some examples from work with omeprazole. The role of mass spectrometry (MS) for structure elucidation is emphasized. Dissolution testing comprises a large number of samples and adaptation to standardized procedures is important. Work is exemplified with dissolution testing of felodipine. Automation and robots with multivariate calibration are necessary approaches. Macromolecular characterization is exemplified from the fields of biomolecules and macromolecular excipients. Separation methods and MS are important tools. New challenges in the area of process analytical chemistry are discussed and chemometrics will play an important role. In all fields method validation is stressed, but should not require more power than necessary in a specification.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF01245501
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  • 2
    Digitale Medien
    Digitale Medien
    Analysis of α-hydroxy metabolites of metoprolol in human urine after phosgene/trimethylsilyl derivatizationPresented at a Symposium on Analytical Techniques in Studies on Metabolism, April 1985, Stockhoim, Sweden. (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 543-548 
    Details
    ISSN: 0887-6134
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Three metoprolol metabolites containing an α-hydroxy group were identified in human urine by capillary column gas chromatography/mass spectrometry. After aqueous phase cyclization with phosgene the neutral or acidic derivatives formed were isolated by solvent extraction at pH 10 or 3, respectively. Following silylation the electron impact mass spectra of the metabolites exhibited a characteristic ion at m/z 336 of high abundance which originated from cleavage of the bond adjacent to the a-OTMS group. Most probably the identified compounds were formed by further biotransformations of α-hydroxy metoprolol, which is a primary metabolite. The analytical method is applicable to detect the metoprolol metabolites reported so far. A quantitative assay for one of the metabolites (H 119/72) with nitrogen selective detection is described. The total amount of this metabolite excreted by one subject within 24 h after dosing was about 0.25% of the given dose.
    Zusätzliches Material: 8 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200141003
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  • 3
    Digitale Medien
    Digitale Medien
    Immobilized vancomycin as chiral stationary phase in packed capillary liquid chromatography (1998)
    New York, NY [u.a.] : Wiley-Blackwell
    Chirality 10 (1998), S. 273-280 
    Details
    ISSN: 0899-0042
    Schlagwort(e): direct chiral separation ; mobile phase composition ; NSAIDs ; retention model ; vancomycin ; Chemistry ; Organic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Fused silica-packed capillary columns containing vancomycin immobilized by reductive amination on an aldehyde-silica were used to separate enantiomers of some non-steroidal anti-inflammatory drugs. Attempts have been made to qualitatively explain the influence of various mobile phase compositions on the enantioselective retention. The effects of mobile phase pH, buffer, and organic modifier concentrations were investigated as well as the influence of salts of hydrophobic ions added to the mobile phase to induce ion pair retention. Chirality 10:273-280, 1998. © 1998 Wiley-Liss, Inc.
    Zusätzliches Material: 8 Ill.
    Materialart: Digitale Medien
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  • 4
    Digitale Medien
    Digitale Medien
    Enantiomer separation by capillary SFC and GC on immobilized octakis(2,6-di-O-methyl-3-O-pentyl)-γ-cyclodextrin (1994)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 779-783 
    Details
    ISSN: 0935-6304
    Schlagwort(e): Enantioselective gas chromatography ; Enantioselective supercritical fluid chromatography ; Immobilized chiral stationary phases ; Modified cyclodextrin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Heptakis(2,6-di-O-methyl-3-O-pentyl) (2-O-methyl-6-O-oct-1-enyl-3-O-pentyl)-γ-cyclodextrin was immobilized to narrow-bore fused silica capillaries after selective modification. One tert-butyldimethylsilyl group was introduced into octakis-(2-O-methyl-3-O-pentyl)-γ-cyclodextrin in order to get a pure monofunctionalized cyclodextrin derivative. During synthesis the tert-butyldimethylsilyl group was replaced by an anchoring group to bind the cyclodextrin to a polysiloxane. After thermal immobilization of the modified polysiloxane this new chiral stationary phase was applied in GC and SFC. High efficiency separations were obtained in GC. In SFC very polar compounds could be chromatographed at low temperatures resulting in higher separation factors as compared to GC.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/jhrc.1240171110
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