TY  - JOUR
VL  - 151
ID  - discovery10042461
AV  - public
SP  - 186
A1  - Crews, C
A1  - Kenny, PS
A1  - O'Flynn, D
A1  - Speller, RD
KW  - Chemometrics
KW  -  Counterfeit medicines
KW  -  EDXRD
KW  -  Quantitative analysis
KW  -  X-ray diffraction
SN  - 1873-264X
EP  - 193
Y1  - 2018/01/09/
UR  - http://dx.doi.org/10.1016/j.jpba.2017.12.036
N2  - 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.
TI  - Multivariate calibration of energy-dispersive X-ray diffraction data for predicting the composition of pharmaceutical tablets in packaging
N1  - Open Access funded by Engineering and Physical Sciences Research Council.
Under a Creative Commons license Attribution 4.0 International (CC BY 4.0).
JF  - Journal of Pharmaceutical and Biomedical Analysis
ER  -