Molecules, Vol. 24, Pages 1764: A Deeper Investigation of Drug Degradation Mixtures Using a Combination of MS and NMR Data: Application to Indapamide
Molecules, Vol. 24, Pages 1764: A Deeper Investigation of Drug Degradation Mixtures Using a Combination of MS and NMR Data: Application to Indapamide
Molecules doi: 10.3390/molecules24091764
Authors:
Cécile Palaric
Roland Molinié
Dominique Cailleu
Jean-Xavier Fontaine
David Mathiron
François Mesnard
Yoann Gut
Tristan Renaud
Alain Petit
Serge Pilard
A global approach that is based on a combination of mass spectrometry (MS) and nuclear magnetic resonance (NMR) data has been developed for a complete and rapid understanding of drug degradation mixtures. We proposed a workflow based on a sample preparation protocol that is compatible to MS and NMR, the selection of the most appropriate experiments for each technique, and the implementation of prediction software and multivariable analysis method for a better interpretation and correlation of MS and NMR spectra. We have demonstrated the efficient quantification of the remaining active pharmaceutical ingredient (API). The unambiguous characterization of degradation products (DPs) was reached while using the potential of ion mobility-mass spectrometry (IM-MS) for fragment ions filtering (HDMSE) and the implementation of two-dimensional (2D) NMR experiments with the non-uniform sampling (NUS) method. We have demonstrated the potential of quantitative NMR (qNMR) for the estimation of low level DPs. Finally, in order to simultaneously monitor multi-samples, the contribution of partial least squares (PLS) reg...
Source: Molecules - Category: Chemistry Authors: C écile Palaric Roland Molini é Dominique Cailleu Jean-Xavier Fontaine David Mathiron Fran çois Mesnard Yoann Gut Tristan Renaud Alain Petit Serge Pilard Tags: Article Source Type: research