Application of new methodologies based on design of experiments, independent component analysis and design space for robust optimization in liquid chromatography
[en] HPLC separations of an unknown sample mixture and a pharmaceutical formulation have been optimized using a recently developed chemometric methodology proposed by W. Dewé et al. in 2004 and improved by P. Lebrun et al. in 2008. This methodology is based on experimental designs which are used to model retention times of compounds of interest. Then, the prediction accuracy and the optimal separation robustness, including the uncertainty study, were evaluated. Finally, the design space (ICH Q8(R2) guideline) was computed as the probability for a criterion to lie in a selected range of acceptance. Furthermore, the chromatograms were automatically read. Peak detection and peak matching were carried out with a previously developed methodology using independent component analysis published by B. Debrus et al. in 2009. The present successful applications strengthen the high potential of these methodologies for the automated development of chromatographic methods.
Boulanger, Bruno ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Hubert, Philippe ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Language :
English
Title :
Application of new methodologies based on design of experiments, independent component analysis and design space for robust optimization in liquid chromatography
Dewé W., Marini R., Chiap P., Hubert P., Crommen J., Boulanger B. Chemom. Intell. Lab. Syst. 2004, 74:263-268. http://hdl.handle.net/2268/6036.
International Conference on Harmonization (ICH) of Technical Requirements for registration of Pharmaceuticals for Human Use, Topic Q8(R2): Pharmaceutical Development, Geneva, 2005.
Peterson J.J. J. Qual. Tech. 2004, 36:139-153.
De Backer B., Debrus B., Lebrun P., Theunis L., Dubois N., Decock L., Verstraete A., Hubert Ph., Charlier C. J. Chromatogr. B 2009, 877:4115-4124. http://hdl.handle.net/2268/4442.
Martens H., Martens M. Multivariate Analysis of Quality. An Introduction 2001, Wiley, Chichester.
International Conference on Harmonization (ICH) of Technical Requirements for registration of Pharmaceuticals for Human Use, Topic Q2(R1): Validation of Analytical Procedures: Text and Methodology, Geneva, 1996.