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Solid-state carbon NMR characterization of the polymorphs of roxifiban
Rodney D Vickery1, Gregory A Nemeth, Michael B Maurin
1Bristol-Myers Squibb Pharmaceutical Research Institute, PO Box 80353, Wilmington, DE 19880-0353, USA. rodney.vickery@bms.com
Abstract:
Roxifiban, an experimental antithrombotic prodrug, exists as crystalline forms I and II. A quantitative solid-state nuclear magnetic resonance (NMR) method was developed to characterize the two polymorphs of roxifiban. The differences in the NMR spectra of the polymorphs were utilized in analyses of physical blends of the pure crystalline forms to establish a calibration curve. A detection limit of 9% form II in form I was determined from analysis of a 10% form II blend. Solid-state NMR was a valuable technique to quantify the polymorphic purity of roxifiban where other techniques such as differential scanning calorimetry (DSC) could not be used for this purpose.