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Quantitative analyses of complex pharmaceutical mixtures by the Rietveld method

Published online by Cambridge University Press:  05 March 2012

Sampath S. Iyengar ,
Neelima V. Phadnis  and
Raj Suryanarayanan
Sampath S. Iyengar*
Affiliation:
College of Pharmacy, 308 Harvard Street SE, University of Minnesota, Minneapolis, Minnesota 55455
Neelima V. Phadnis*
Affiliation:
College of Pharmacy, 308 Harvard Street SE, University of Minnesota, Minneapolis, Minnesota 55455
Raj Suryanarayanan*
Affiliation:
College of Pharmacy, 308 Harvard Street SE, University of Minnesota, Minneapolis, Minnesota 55455
*
a)Also at: Technology of Materials, 2922 De la Vina Street, Suite C, Santa Barbara, CA 93105.
b)Current address: SmithKline Beecham Consumer Healthcare, 1500 Littleton Road, Parsippany, NJ 07054.
c)Author to whom correspondence should be addressed; electronic mail: surya001@tc.umn.edu
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Abstract

The object was to perform simultaneous quantitative analyses of complex pharmaceutical solid mixtures by the Rietveld method. Mixtures consisting of anhydrous β-carbamazepine, anhydrous α-carbamazepine, and carbamazepine dihydrate were chosen as the model system. Lithium fluoride was used as the internal standard. Mixtures of various compositions were prepared and subjected to X-ray powder diffractometry (XRD). The XRD pattern of each mixture was analyzed by the Rietveld method and at the end of the refinement, the goodness of fit was evaluated. When the analyte concentration was high (≥20%), the relative error in the determination was <±5%. The detection of analyte was possible even when its concentration was low (<1% w/w). A unique advantage of the method is that it enables simultaneous quantitative analyses of multiple phases without the requirement of “standard curves.” © 2001 International Centre for Diffraction Data.

Keywords

carbamazepinedihydratepolymorphX-ray powder diffractometryRietveld
Type
Technical Articles
Information
Powder Diffraction , Volume 16 , Issue 1 , March 2001 , pp. 20 - 24
Copyright
Copyright © Cambridge University Press 2001

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