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Proceedings Paper

Quantitative energy-dispersive x-ray diffraction for identification of counterfeit medicines: a preliminary study
Author(s): Chiaki C. E. Crews; Daniel O'Flynn; Aiden Sidebottom; Robert D. Speller
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Paper Abstract

The prevalence of counterfeit and substandard medicines has been growing rapidly over the past decade, and fast, nondestructive techniques for their detection are urgently needed to counter this trend. In this study, energy-dispersive X-ray diffraction (EDXRD) combined with chemometrics was assessed for its effectiveness in quantitative analysis of compressed powder mixtures. Although EDXRD produces lower-resolution diffraction patterns than angular-dispersive X-ray diffraction (ADXRD), it is of interest for this application as it carries the advantage of allowing the analysis of tablets within their packaging, due to the higher energy X-rays used. A series of caffeine, paracetamol and microcrystalline cellulose mixtures were prepared with compositions between 0 - 100 weight% in 20 weight% steps (22 samples in total, including a centroid mixture), and were pressed into tablets. EDXRD spectra were collected in triplicate, and a principal component analysis (PCA) separated these into their correct positions in the ternary mixture design. A partial least-squares (PLS) regression model calibrated using this training set was validated using both segmented cross-validation, and with a test set of six samples (mixtures in 8:1:1 and 5⅓:2⅓:2⅓ ratios) – the latter giving a root-mean square error of prediction (RMSEP) of 1.30, 2.25 and 2.03 weight% for caffeine, paracetamol and cellulose respectively. These initial results are promising, with RMSEP values on a par with those reported in the ADXRD literature.

Paper Details

Date Published: 3 June 2015
PDF: 11 pages
Proc. SPIE 9482, Next-Generation Spectroscopic Technologies VIII, 94820D (3 June 2015); doi: 10.1117/12.2176738
Show Author Affiliations
Chiaki C. E. Crews, Univ. College London (United Kingdom)
Daniel O'Flynn, Univ. College London (United Kingdom)
Aiden Sidebottom, Univ. College London (United Kingdom)
Robert D. Speller, Univ. College London (United Kingdom)


Published in SPIE Proceedings Vol. 9482:
Next-Generation Spectroscopic Technologies VIII
Mark A. Druy; Richard A. Crocombe; David P. Bannon, Editor(s)

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