Quantitative analysis of mannitol polymorphs: X-ray powder diffractometry—exploring preferred orientation effects
Campbell Roberts, S. N. C., Williams, A. C., Grimsey, I. M. and Booth, S. W. (2002) Quantitative analysis of mannitol polymorphs: X-ray powder diffractometry—exploring preferred orientation effects. Journal of Pharmaceutical and Biomedical Analysis, 28 (6). pp. 1149-1159. ISSN 0731-7085
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To link to this article DOI: 10.1016/S0731-7085(02)00053-5
Mannitol is a polymorphic pharmaceutical excipient, which commonly exists in three forms: alpha, beta and delta. Each polymorph has a needle-like morphology, which can give preferred orientation effects when analysed by X-ray powder diffractometry (XRPD) thus providing difﬁculties for quantitative XRPD assessments. The occurrence of preferred orientation may be demonstrated by sample rotation and the consequent effects on X-ray data can be minimised by reducing the particle size. Using two particle size ranges (less than 125 and 125–500�microns), binary mixtures of beta and delta mannitol were prepared and the delta component was quantiﬁed. Samples were assayed in either a static or rotating sampling accessory. Rotation and reducing the particle size range to less than�125 microns halved the limits of detection and quantitation to 1 and 3.6%, respectively. Numerous potential sources of assay errors were investigated; sample packing and mixing errors contributed the greatest source of variation. However, the rotation of samples for both particle size ranges reduced the majority of assay errors examined. This study shows that coupling sample rotation with a particle size reduction minimises preferred orientation effects on assay accuracy, allowing discrimination of two very similar polymorphs at around the 1% level
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