Optimising NMR Spectroscopy Through Method and Software Development (Springer Theses)

This book provides a comprehensive overview of Nuclear Magnetic Resonance (NMR) theory, its applications, and advanced techniques to improve the quality and speed of NMR data acquisition. In this book, the author expands his outstanding Ph.D. thesis and provides a valuable resource for researchers, professionals, and students in the field of NMR spectroscopy. The book covers quantum mechanics basics, and topics like density operators, pulse sequences, 1D pulse acquisition, INEPT (Insensitive nuclei enhancement by polarization transfer), product operators, and 2D NMR principles. It also explores innovative experiments like States HSQC (Heteronuclear Single Quantum Coherence) and echo-antiecho HSQC with gradients. In the subsequent chapters, the author discusses Pure Shift NMR, including PSYCHE (Pure Shift Yielded by Chirp Excitation) and its optimizations, such as waveform parameterization and time-reversal methods. The 'Discrete PSYCHE' approach and Ultrafast PSYCHE-iDOSY (Diffusion-ordered spectroscopy) are also highlighted. This book presents the POISE (Parameter Optimisation by Iterative Spectral Evaluation) software for real-time NMR experiment optimization, including pulse width calibration and Ernst angle optimization, and demonstrates applications across various NMR experiments. Lastly, the book examines accelerated 2D NMR data collection and the NOAH (NMR by Ordered Acquisition using 1H detection) supersequences, emphasizing automated pulse program creation using GENESIS (GENEration of Supersequences In Silico). Covered NMR experiments include 13C sensitivity-enhanced HSQC, 15N HMQC (Heteronuclear Multiple Quantum Coherence), dual HSQC, HSQC-TOCSY (Total Correlation Spectroscopy), HMBC (Heteronuclear Multiple Bond Correlation), and ADEQUATE (Adequate Sensitivity Double-Quantum Spectroscopy). Supervisor's Foreword Abstract Preface Pulse Sequence Notation Software Samples Used Publications Acknowledgements Contents Acronyms List of Figures List of Tables List of Code Listings 1 NMR Theory 1.1 Quantum Mechanics 1.2 The Rotating Frame 1.3 Density Operators 1.4 Pulse Sequences 1.4.1 1D Pulse–Acquire 1.4.2 INEPT and Product Operators 1.4.3 2D NMR: General Principles 1.4.4 The States HSQC Experiment 1.4.5 The Echo–Antiecho HSQC: Gradients and Coherence Selection References 2 Pure Shift NMR 2.1 Theoretical Background 2.2 Pure Shift in Practice 2.2.1 Acquisition Modes 2.2.2 Pure Shift Elements 2.2.3 PSYCHE in Detail 2.3 PSYCHE with a Variable Number of Saltires 2.3.1 Quadruple-Saltire PSYCHE 2.3.2 Single-Saltire PSYCHE 2.4 Direct Optimisation of PSYCHE Waveform 2.4.1 Techniques for Pure Shift Optimisations 2.4.2 Flip Angle Optimisation 2.4.3 Waveform Parameterisation and Optimisation 2.5 Time-Reversal Method 2.6 `Discrete PSYCHE' 2.6.1 Speeding up dPSYCHE Simulations 2.6.2 Optimisations and Experimental Evaluation 2.7 Ultrafast PSYCHE-iDOSY 2.8 Conclusion References 3 POISE 3.1 Introduction 3.2 Technical Overview 3.2.1 Routines 3.2.2 The Experiment 3.2.3 Optimisation Options 3.2.4 Optimisation Algorithms 3.2.5 Implementation Details 3.3 What POISE Is Not 3.4 Applications 3.4.1 Pulse Width Calibration 3.4.2 Ernst Angle Optimisation 3.4.3 Inversion–Recovery 3.4.4 NOE Mixing Time 3.4.5 ASAP-HSQC Excitation Delay 3.4.6 Ultrafast NMR 3.4.7 HMBC Low-Pass J-Filter 3.4.8 PSYCHE Pure Shift NMR 3.4.9 Water Suppression 3.4.10 Diffusion NMR 3.5 POISE for ESR 3.6 Conclusion References 4 NOAH 4.1 Introduction 4.1.1 Time Savings and Sensitivity Analyses 4.1.2 Magnetisation Pools 4.1.3 Case Studies 4.2 GENESIS: Automated Pulse Program Creation 4.2.1 Motivation 4.2.2 Implementation Details 4.2.3 Processing Improvements 4.3 Discussion of Individual Modules 4.3.1 13C Sensitivity-Enhanced HSQC 4.3.2 15N HMQC 4.3.3 15N Sensitivity-Enhanced HSQC 4.3.4 Dual HSQC and HSQC-TOCSY 4.3.5 HSQC-COSY 4.3.6 2DJ and PSYCHE 4.3.7 HMBC 4.3.8 ADEQUATE 4.4 Solvent Suppression in NOAH 4.4.1 Presaturation 4.4.2 Intrinsic Suppression 4.4.3 Excitation Sculpting 4.5 Parallel and Generalised NOAH Supersequences 4.5.1 Parallel NOAH Supersequences 4.5.2 Generalised Supersequences 4.6 Conclusion References Appendix Peak Assignments for Selected Samples A.1 Andrographolide A.2 Cyclosporin A.3 Ferulic Acid A.4 Gramicidin A.5 Brucine A.6 Zolmitriptan