On‐Line LC‐NMR And Related Techniques

Abstract

Contributors. Preface. 1. LC NMR: Theory and Experiment (Klaus Albert). 1.1 Introduction. 1.2 NMR in a Flowing Liquid. 1.3 Design of Continuous Flow NMR Probes. 1.4 Experimental Arrangement for HPLC 1H NMR Coupling. 1.5 Practical Considerations, Solvent Suppression Techniques, Gradient Elution and Purity of HPLC Solvents. References. 2. LC NMR: Automation (Ulrich Braumann and Manfred Spraul). 2.1 Practical Use of LC NMR and LC NMR/MS. 2.2 Different Working Modes in LC NMR. 2.3 Use of Mass Spectrometry in the Set Up. 2.4 Measurement Procedures. 2.5 Conclusions. References. 3. Biomedical and Pharmaceutical Applications of HPLC NMR and HPLC NMR MS (John C. Lindon, Jeremy K. Nicholson and Ian D. Wilson). 3.1 Introduction. 3.2 Technical and Operational Overview. 3.3 Applications in Combinatorial Chemistry. 3.4 Application to Chemical Impurities. 3.5 Application to Chiral Separations of Pharmaceutical Mixtures. 3.6 Application to Natural Products. 3.7 Application to Chemical Reactivity of Drug Glucuronides. 3.8 Application to Futile Deacetylation Reactions. 3.9 Application to Trapping of Reactive Intermediates. 3.10 Application to Uptake and Transformation of Xenobiotics by Plants. 3.11 Separation of Lipoproteins and their Characterisation using HPLC NMR. 3.12 Superheated Water HPLC NMR and HPLC NMR MS Studies on Pharmaceuticals. 3.13 Application of Hypernation to a Mixture of Non Steroidal Anti Inflammatory Drugs. 3.14 Concluding Remarks. References. 4. Application of On Line LC NMR and Related Techniques to Drug Metabolism Studies (John P. Shockcor). 4.1 Introduction. 4.2 LC NMR Techniques. 4.3 Application of LC NMR MS to Drug Metabolism: The Structure Elucidation of Rat Urinary Metabolites of Efavirenz by LC NMR MS. Conclusions. References. 5. LC NMR for Natural Products Analysis. 5.1 Application of LC NMR and LC NMR MS Hyphenation to Natural Products Analysis (Martin Sandvoss). References. 5.2 Hyphenation of Modern Extraction Techniques to LC NMR for the Analysis of Geometrical Carotenoid Isomers in Functional Food and Biological Tissues (Tobias Glaser and Klaus Albert). References. 6. LC NMR in Environmental Analysis (Alfred Preiss and Markus Godejohann). 6.1 Introduction. 6.2 Target and Non Target Analysis. 6.3 LC NMR Coupling in Non Target Analysis. 6.4 Application of LC NMR and LC NMR in Combination with LC MS to Environmental Samples. 6.5 Simulation of Environmental Processes. 6.6 Conclusions. References. 7. Related Techniques Introduction. 7.1 GPC NMR Coupling (Heidrun Handel and Klaus Albert). References. 7.2 SFC NMR and SFE NMR (Holger Fischer and Klaus Albert). 7.3 Nanoliter NMR. 8. Future Developments Introduction. 8.1 HPLC 13C NMR (Klaus Albert). 8.2 Parallel NMR Detection (Andrew G. Webb, Jonathan V. Sweedler and Daniel Raftery). Concluding Remarks (Klaus Albert). Index.