Multivariate calibration of energy-dispersive X-ray diffraction data for predicting the composition of pharmaceutical tablets in packaging

Crews, Chiaki; Kenny, Peter S.; O’Flynn, Daniel and Speller, Robert D. (2018). Multivariate calibration of energy-dispersive X-ray diffraction data for predicting the composition of pharmaceutical tablets in packaging. Journal of Pharmaceutical and Biomedical Analysis, 151 pp. 186–193.

DOI: https://doi.org/10.1016/j.jpba.2017.12.036

Abstract

A system using energy-dispersive X-ray diffraction (EDXRD) has been developed and tested using multivariate calibration for the quantitative analysis of tablet-form mixtures of common pharmaceutical ingredients. A principal advantage of EDXRD over the more traditional and common angular dispersive X-ray diffraction technique (ADXRD) is the potential of EDXRD to analyse tablets within their packaging, due to the higher energy X-rays used.

In the experiment, a series of caffeine, paracetamol and microcrystalline cellulose mixtures were prepared and pressed into tablets. EDXRD profiles were recorded on each sample and a principal component analysis (PCA) was carried out in both unpackaged and packaged scenarios. In both cases the first two principal components explained >98% of the between-sample variance. The PCA projected the sample profiles into two dimensional principal component space in close accordance to their ternary mixture design, demonstrating the discriminating potential of the EDXRD system.

A partial least squares regression (PLSR) model was built with the samples and was validated using leave-one-out cross-validation. Low prediction errors of between 2% and 4% for both unpackaged and packaged tablets were obtained for all three chemical compounds. The prediction capability through packaging demonstrates a truly non-destructive method for quantifying tablet composition and demonstrates good potential for EDXRD to be applied in the field of counterfeit medicine screening and pharmaceutical quality control.

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• Item ORO ID
• 71057
• Item Type
• Journal Item
• ISSN
• 0731-7085
• Project Funding Details

• Funded Project Name	Project ID	Funding Body
  Not Set	EP/G037264/1	EPSRC (Engineering and Physical Sciences Research Council)

• Keywords
• Counterfeit medicines; Quantitative analysis; X-ray diffraction; EDXRD; Chemometrics
• Academic Unit or School
• Faculty of Science, Technology, Engineering and Mathematics (STEM) > Physical Sciences
  Faculty of Science, Technology, Engineering and Mathematics (STEM)
• Research Group
• ?? space ??
  Centre for Electronic Imaging (CEI)
• Copyright Holders
• © 2018 The Authors
• Depositing User
• Chiaki Crews