Since the development of the NMR spectrometer in the 1950s, NMR spectra have been widely used for the elucidation of the 2D structure of newly synthesized and natural compounds. In the 1980s, the high-resolution NMR spectrometer (> 300 Mhz) and 2D experiments were introduced, which opens up the possibility to determine the 3D structure of large molecules, especially biomolecules. However, NMR spectroscopy has been rarely applied to drug analysis.This book illustrates the power and versatility of NMR spectroscopy in the determination of impurities in and the content of drugs, the composition of polymer excipients, the characterization of isomeric drug mixtures, the complexity of drugs with small-size components or ions, and the behavior of drugs in acid and basic solution. In addition, NMR spectroscopy and especially the hyphenated technique with HPLC is shown to be a powerful tool to measure a drug and its metabolites in various body fluids. The solid state NMR technique can give information on the structure, especially the conformation of drugs and excipients in drug formulations. Recently, SAR by NMR, introduced by Fesik, impressively demonstrated the potential of NMR spectroscopy in drug development and in the characterization of the interaction between large molecules and ligands. The complexation between proteins, lipids and cyclodextrins with drugs is described. Finally, NMR imaging (MRI and MRS) can be used to characterize the liberation of drugs from a drug formulation. Furthermore, the distribution of substances in plants, in animals, in tissues and in humans can be visualized by imaging.In short, this book covers all aspects of drug analysis.
Ulrike Holzgrabe and Iwona Wawer are the authors of NMR Spectroscopy in Drug Development and Analysis, published by Wiley.
PrefaceContributorsChapter 1 Introduction 1Chapter 2 NMR Spectroscopy in the European Regulatory Dossier 5Chapter 3 Analysis of Drugs 16Chapter 4 pH-Dependent NMR Measurements 61Chapter 5 Complexation Behaviour of Drugs Studied by NMR 77Chapter 6 Determination of the Isomeric Composition of Drugs 82Chapter 7 On-Line Coupling of HPLC or SFC 101Chapter 8 NMR of Body Fluids 118Chapter 9 NMR as a Tool in Drug Research 134Chapter 10 Ligand-Cyclodextrin Complexes 154Chapter 11 Ligand-Membrane Interaction 174Chapter 12 Solid-State NMR in Drug Analysis 231Chapter 13 MR Imaging and MR Spectroscopy 257Concluding Remarks 294