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Analyses of Multi- Phase Pharmaceuticals Using SImultaneous Differential Scanning Calorimetry and X-Ray Diffraction

  • T. G. Fawcett (a1), E. J. Martin (a1), C. E. Crowder (a1), P. J. Kincaid (a1), A. J. Strandjord (a1), J. A. Blazy (a1), D. N. Armentrout (a1) and R. A. Newman (a1)...

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The analysis of multi-phase pharmaceuticals, particularly when similar structures are involved (i.e. polymorphs, salts or hydrates), can often be a difficult task. Historically, x-ray powder diffraction (XRD) and differential scanning calorimetry (DSC) have been utilized to study pharmaceutical samples. Relative to other materials, diffraction data for pharmaceuticals are often complex due to the large number of diffraction maxima caused by the size of the molecule and/or the molecular symmetry. Multi-phase mixtures tend to have a large number of overlapping peaks which can hinder the difftactionist's ability to identify phases and interpret the data. When similar structures are analyzed calorimetrically, their thermal events may severely overlap (as will be shown), preventing accurate interpretation of the data. In addition there are several types of thermal events which may not be related to structural transitions. A common one in pharmaceuticals is the loss of solvent or absorbed (versus molecular) water.

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References

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1. Fawcett, T.G., Crowder, C.E., Whiting, L.F., Tou, J.C., Scott, W.F., Newman, R.A., Harris, W.C., Knoll, F.J., Caldecourt, V.J., The Rapid Simultaneous Measurement of Thermal and Structural Data by a Novel DSC/XRD Instrument, Adv. in X-Ray Analysis. 28, 227 (1985).
2. Brown, A., Edmonds, J.W., The Fitting of Powder Diffraction Profiles to an Analytical Expression and the Influence of Line Broadening Factors, Adv. in X-Ray Analysis. 23, 361 (1980).
3. Fawcett, T.G., Moore Kirchhoff, P., Newman, R.A., The Measurement of. Thermally Induced Structural Changes by High Temperature (900°C) Guinier X-Ray Powder Diffraction Techniques, Adv. in X-Ray Analysis. 26, 171 (1983).
4. Newman, R.A., Fawcett, T.G., Moore Kirchhoff, P., Evaluation of Straight and Curved Braun Position-Sensitive Proportional Counters on a Huber- Guinier X-Ray Diffraction System, Adv. in X-Ray Analysis. 27, 261 (1984).

Analyses of Multi- Phase Pharmaceuticals Using SImultaneous Differential Scanning Calorimetry and X-Ray Diffraction

  • T. G. Fawcett (a1), E. J. Martin (a1), C. E. Crowder (a1), P. J. Kincaid (a1), A. J. Strandjord (a1), J. A. Blazy (a1), D. N. Armentrout (a1) and R. A. Newman (a1)...

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