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    Methods for Increasing Sensitivity and Throughput of Solid-State NMR Spectroscopy of Pharmaceutical Solids

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    Schieber_ku_0099D_10723_DATA_1.pdf (8.489Mb)
    Issue Date
    2010-01-22
    Author
    Schieber, Loren J.
    Publisher
    University of Kansas
    Format
    241 pages
    Type
    Dissertation
    Degree Level
    Ph.D.
    Discipline
    Pharmaceutical Chemistry
    Rights
    This item is protected by copyright and unless otherwise specified the copyright of this thesis/dissertation is held by the author.
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    Abstract
    Solid-state nuclear magnetic resonance (SSNMR) spectroscopy has been demonstrated to be a powerful technique for investigating solid dosage formulations. SSNMR has the ability to determine physical form, molecular structure, and dynamics of a pure or formulated active pharmaceutical ingredient (API). To overcome the major shortcomings of SSNMR, acquisition time and sensitivity, a two-sample probe was designed, developed, and tested. The probe allowed for two samples to be acquired simultaneously while being shuttled through the magnet bore with a stepper motor, and exhibited signal to noise ratio (SNR) values comparable to current probes. Pharmaceutical relevance was demonstrated by acquiring spectra of ibuprofen and aspirin simultaneously. 19F SSNMR was used to examine low-level amorphous impurities in crystalline physical mixtures. The model compound was chosen for amorphous form stability, cost, and 19F SSNMR spectral resolution between the crystalline and amorphous solid forms. Triamcinolone was selected for quantitation studies using 19F SSNMR.
    URI
    http://hdl.handle.net/1808/6279
    Collections
    • Dissertations [4473]
    • Pharmaceutical Chemistry Dissertations and Theses [141]

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    785-864-8983

    KU Libraries
    1425 Jayhawk Blvd
    Lawrence, KS 66045
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    Contact KU ScholarWorks
    785-864-8983
    KU Libraries
    1425 Jayhawk Blvd
    Lawrence, KS 66045
    785-864-8983

    KU Libraries
    1425 Jayhawk Blvd
    Lawrence, KS 66045
    Image Credits
     

     

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