Modern Magnetic Resonance (eBook)

Graham A. Webb has been actively engaged in research involving many aspects of NMR for about 25 years both at University College London and the University of Surrey, where he became a Professor of Physical Chemistry. During this time he has authored more than 400 published primary research papers, given presentations at about 200 international conferences dealing with NMR and supervised about 70 Ph.D. theses. He has been Editor of Annual Reports on NMR since 1975; the latest Volume to appear is number 55. In addition, he has edited The Royal Society of Chemistry Specialist Periodical Reports on NMR since 1978; the latest Volume is number 35. Professor Webb has also organised the biennial international conferences on Applications of NMR in Food Science since 1984.

Modern Magnetic Resonance Part 1: Applications in Chemistry, Biological and Marine Sciences 4
Contents 6
List of Section Editors 11
Preface 13
Part I Color Plate Section 14
Part I, Section 1: Applications in Chemistry 53
Foreword to Application in Chemistry 54
Abbreviations 55
Amyloids 58
Kinetics of Amyloid Fibril Formation of Human Calcitonin 59
Introduction 59
Conformational Changes of hCT 59
Kinetic Analysis of hCT Fibrillation 60
Mechanism of Fibril Formation 64
Conclusion 64
Acknowledgment 64
References 64
Polymorphism of Alzheimer’s Aß Fibrils 66
Abstract 66
References 71
Chemical Shifts and Spin-Couplings 75
13C, 15N, 1H, 2H, and 17O NMR Chemical Shift NMR for Hydrogen Bonds 76
NMR Chemical Shift Map 81
References 86
NMR Chemical Shifts Based on Band Theory 87
Introduction 87
Theoretical Aspects of Electronic State and Nuclear Shielding in Solid Polymers 87
Configuration 90
Crystal Structure 92
References 95
Modeling NMR Chemical Shifts 97
Abstract 97
Introduction 97
Theory of the Chemical Shieldings 98
Modeling Chemical Shieldings 98
References 105
Ab Initio Calculation of NMR Shielding Constants 107
Introduction 107
Ab Initio Program Packages Capable of Calculating NMR Chemical Shielding Tensors 110
Ab Initio Calculation of NMR Chemical Shielding Tensors for Large Molecules 111
References 113
Crystal Structure Re.nement Using Chemical Shifts 115
Introduction 115
BPT Calculation of Atomic Charges 116
Molecular Force Fields and Chemical Shift Pseudo-Forces 117
BPT Pseudo-Forces 118
Applications in Crystal Structure Re.nement 118
References 121
The Theory of Nuclear Spin–Spin Couplings 123
Introduction 123
Origin of the Indirect Nuclear Spin–Spin Coupling Interaction 123
Coupled Hartree–Fock Approximation 125
Triplet Instability of Coupled Hartree–Fock -A E - B Q1 Calculation . 126
Fibrous Proteins 128
Investigation of Collagen Dynamics by Solid-State NMR Spectroscopy 129
Solid-State NMR Studies of Elastin and Elastin Peptides 135
Structural Analysis of Silk Fibroins using NMR 142
Field Gradient NMR 148
NMR Diffusometry 149
Field Gradient NMR of Liquid Crystals 156
Field Gradient NMR for Polymer Systems with Cavities 162
NMR Measurements Using Field Gradients and Spatial Information 167
Theory and Application of NMR Diffusion Studies 173
Host–Guest Chemistry 182
Solid-State NMR in Host–Guest Chemistry 183
Imaging 191
Mapping of Flow and Acceleration with NMR Microscopy Techniques 192
Industrial Application of In situ NMR Imaging Experiments to Steel-Making Process 198
Biomedical NMR Spectroscopy and Imaging 207
Electron Spin Resonance Imaging in Polymer Research 213
NMR Imaging: Monitoring of Swelling of Environmental Sensitive Hydrogels 220
Inorganic Materials and Catalysis 227
Exploiting 1H.29Si Cross-Polarization Features forStructural Characterization of Inorganic Materials 228
Solid State NMR Characterization of Solid Surface of Heterogeneous Catalysts 235
Isotope Labeling 242
Recent Developments in Stable-Isotope-Aided Methods for Protein NMR Spectroscopy 243
Structural Glycobiology by Stable-isotope-assisted NMR Spectroscopy 251
Lipid Bilayer and Bicelle 258
Development and Application of Bicelles for Use in Biological NMR and Other Biophysical Studies 259
Nuclear Magnetic Resonance of Oriented Bilayer Systems 266
Solid-State Deuterium NMR Spectroscopy of Membranes 273
Solid State 19F-NMR Analysis of Oriented Biomembranes 285
Membrane-Associated Peptides 292
Solid-State NMR Studies of the Interactions Structure of Antimicrobial Peptides in Model Membranes 293
Anisotropic Chemical Shift Perturbation Induced by Ions in Conducting Channels 301
NMR Studies of Ion-Transporting Biological Channels 306
Membrane Proteins 310
Site-Directed NMR Studies on Membrane Proteins 311
Structure of Membrane-Binding Proteins Revealed by Solid-State NMR 318
Solid-State NMR of Memrane-Active Proteins and Peptides 323
Magnetic Resonance Spectroscopic Studies of the Integral Membrane Protein Phospholamban 330
NMR Studies of the Interactions Between Ligands and Membrane-Embedded Receptors: New Methods for Drug Discovery 336
Photosynthetic Antennae and Reaction Centers 344
Insight into Membrane Protein Structure from High-Resolution NMR 351
New Developments 360
Fast Multidimensional NMR: New Ways to Explore Evolution Space 361
High-Sensitivity NMR Probe Systems 367
CRAMPS 376
Mobile NMR 385
Rheo-NMR 395
Analytical Aspects of Solid-State NMR Spectroscopy 401
3H NMR and Its Application 407
On-line SEC–NMR 411
NOE and Chemical Exchange 418
The Nuclear Overhauser Effect 419
Solute–Solvent Interactions Examined by the Nuclear Overhauser Effect 423
Chemical Exchange 431
NQR & ESR
Separated Detection of H-Transfer Motions in Multi-H-Bonded Systems Studied by Combined 1H NMR and 35Cl NQR Measurements 439
EPR: Principles 447
Zero Field NMR: NMR and NQR in Zero Magnetic Field 453
Organo Metallic Chemistry 460
Organoboron Chemistry 461
Organogermanium Chemistry 464
Paramagnetic Effects 469
1H and 13C High-Resolution Solid-State NMR of Paramagnetic Compounds Under Very Fast Magic Angle Spinning 470
Paramagnetic Effects of Dioxygen in Solution NMR—Studies of Membrane Immersion Depth, Protein Topology, and Protein Interactions 478
Protein Structure 487
TROSY NMR for Studies of Large Biological Macromolecules in Solution 488
NMR Insight of Structural Stability and Folding of Calcium-Binding Lysozyme 498
NMR Investigation of Calmodulin 503
Analytical Framework for Protein Structure Determination by Solid-State NMR of Aligned Samples 517
Determining Protein 3D Structure by Magic Angle Spinning NMR 527
19F NMR Study of b-Type Haemoproteins 531
Polymer Structure 539
I NMR in Dry or Swollen Temporary or Permanent Networks 540
Crystalline Structure of Ethylene Copolymers and Its Relation to the Comonomer Content 543
Isomorphism in Bacterially Synthesized Biodegradable Copolyesters 548
Two-Dimensional NMR Analysis of Stereoregularity of Polymers 553
Quantitative Analysis of Conformations in Disordered Polymers by Solid-State Multiple-Quantum NMR 559
Polymer Microstructure: The Conformational Connection to NMR 563
Solid-State NMR Characterization of Polymer Interfaces 571
The Structure of Polymer Networks 578
1H CRAMPS NMR of Polypeptides in the Solid State 585
Polymer Dynamics 599
Dynamics of Amorphous Polymers 600
Molecular Motions of Crystalline Polymers by Solid-State MAS NMR 607
Dynamics in Polypeptides by Solid State 2H NMR 612
Polymer Blends 619
Polymer Blends 620
Configurational Entropy and Polymer Miscibility: New Experimental Insights From Solid-State NMR 625
Quantum Information Processing 633
Quantum Information Processing as Studied by Molecule-Based Pulsed ENDOR Spectroscopy 634
Residual Dipolar Couplings and Nucleic Acids 642
New Applications for Residual Dipolar Couplings: Extending the Range of NMR in Structural Biology 643
Refinement of Nucleic Acid Structures with Residual Dipolar Coupling Restraints in Cartesian Coordinate Space 651
Conformational Analysis of DNA and RNA 657
Solid-State NMR Technique 663
Analytical and Numerical Tools for Experiment Design in Solid-State NMR Spectroscopy 664
Homonuclear Shift-Correlation Experiment in Solids 673
Two-Dimensional 17O Multiple-Quantum Magic-Angle Spinning NMR of Organic Solids 678
A Family of PISEMA Experiments for Structural Studies of Biological Solids 685
Structural Constraints in Solids 692
Rotational-Echo, Double-Resonance NMR 693
REDOR in Multiple Spin System 699
Torsion Angle Determination by Solid-State NMR 706
Secondary Structure Analysis of Proteins from Angle-Dependent Interactions 713
Telomeric DNA Complexes 719
Comparison of DNA-Binding Activities Between hTRF2 and hTRF1 with hTRF2 Mutants 720
Part I Section: 2 Applications in B iological Sciences 729
Abbreviations 730
Optimization of MRI Contrast for Pre-Clinical Studies at High Magnetic Field 733
The Application of In Vivo MRI and MRS in Phenomic Studies of Murine Models of Disease 743
Experimental Models of Brain Disease: MRI Contrast Mechanisms for the Assessment of Pathophysiological Status 760
Experimental Models of Brain Disease: MRI Studies 773
Application of MRS in Cancer in Pre-clinical Models 794
Experimental Cardiovascular MR in Small Animals 805
Application of Pharmacological MRI to Preclinical Drug Discovery and Development 824
Application of MRI to Cell Tracking 847
Part I Section 3: Applications in Marine Science 859
Foreword to Applications in Marine Science 860
Abbreviations 861
Comprehensive Compositional Analysis of Fish Feed by Time Domain NMR 862
Low Field NMR Studies of Atlantic Salmon (Salmo salar) 869
Water Distribution and Mobility in Fish Products in Relation to Quality 878
Proton NMR of Fish Oils and Lipids 882
Determination of Fatty Acid Composition and Oxidation in Fish Oils by High Resolution Nuclear Magnetic Resonance Spectroscopy 887
Resonance Spectroscopy to Study Lipid Oxidation in Fish and Fish Products 894
Omega-3 Fatty Acid Content of Intact Muscle of Farmed Atlantic Salmon (Salmo salar) Examined by 1H MAS NMR Spectroscopy 902
HR MAS NMR Spectroscopy of Marine Microalgae, Part 1: Classi.cation and Metabolite Composition from HR MAS 1H NMR Spectra and Multivariate Analysis 907
HR MAS NMR Spectroscopy of Marine Microalgae, Part 2: 13C and 13C HR MAS NMR Analysis Used to Study Fatty Acid Composition and Polysaccharide Structure 912
Post-mortem Studies of Fish Using Magnetic Resonance Imaging 917
How is the Fish Meat Affected by Technological Processes? 925
Author Index 930
Subject Index 932
Modern Magnetic Resonance Part 2: Applications in Medical and Pharmaceutical Sciences 954
Contents 956
Preface 960
Color Plate Section 961
Part II, Section 1: Applications in Medical Science 976
Foreword to Applications in Medical Science 977
Abbreviations 978
Glossary of Terms 981
Acquiring Neurospectroscopy in Clinical Practice 984
Application of Magnetic Resonance for the Diagnosis of Infective Brain Lesions 1003
Application of 2D Magnetic Resonance Spectroscopy to the Study of Human Biopsies 1012
Correlation of Histopathology with Magnetic Resonance Spectroscopy of Human Biopsies 1023
Functional MRI 1033
High Resolution Magic Angle Spinning (HRMAS) Proton MRS of Surgical Specimens 1047
Intraoperative MRI 1061
In Vivo Magnetic Resonance Spectroscopy in Breast Cancer 1073
In Vivo Molecular MR Imaging: Potential and Limits 1083
In vivo 13C MRS 1095
Magnetic Resonance Spectroscopy and Spectroscopic Imaging of the Prostate, Breast, and Liver 1109
MR-Mammography 1122
Phosphorus Magnetic Resonance Spectroscopy on Biopsy and In Vivo 1137
Radio Frequency Coils for Magnetic Resonance Spectroscopy 1156
Spatially Resolved Two-Dimensional MR Spectroscopy in vivo 1164
Part II, Section 2: Applications in Pharmaceutical Science 1177
Foreword to Applications in Pharmaceutical Science 1178
Key Terms for Applications in Pharmaceutical Science 1179
Overview of NMR in the Pharmaceutical Sciences 1184
Instrumentation 1192
Applications of Cryogenic NMR Probe Technology for the Identi.cation of Low-Level Impurities in Pharmaceuticals 1193
Flow NMR Techniques in the Pharmaceutical Sciences 1201
Developments in NMR Hyphenation for Pharmaceutical Industry 1208
LC-NMR in Dereplication and Structure Elucidation of Herbal Drugs 1216
Techniques 1223
New Approaches to NMR Data Acquisition, Assignment and Protein Structure Determination: Potential Impact in Drug Discovery 1224
Transferred Cross-Correlated Relaxation: Application to Drug/Target Complexes 1232
Novel Uses of Paramagnets to Solve Complex Protein Structures 1240
Fast Assignments of 15N-HSQC Spectra of Proteins by Paramagnetic Labeling 1247
Phospholipid Bicelle Membrane Systems for Studying Drug Molecules 1254
Partial Alignment for Structure Determination of Organic Molecules 1261
Measurement of Residual Dipolar Couplings and Applications in Protein NMR 1268
Using Chemical Shift Perturbations to Validate and Re.ne the Docking of Novel IgE Antagonists to the High-Af.nity IgE Receptor 1273
Dual-Region Hadamard-Encoding to Improve Resolution and Save Time 1279
Nonuniform Sampling in Biomolecular NMR 1285
Applications 1292
Structural Characterization of Antimicrobial Peptides by NMR Spectroscopy 1293
Pharmaceutical Applications of Ion Channel Blockers: Use of NMR to Determine the Structure of Scorpion Toxins 1302
Structure and Dynamics of Inhibitor and Metal Binding to Metallo-ß-Lactamases 1308
NMR Spectroscopy in the Analysis of Protein–Protein Interactions 1315
Identification and Characterization of Ternary Complexes Using NMR Spectroscopy 1323
The Transferred NOE 1333
NMR Kinetic Measurements in DNA Folding and Drug Binding 1339
The Use of NMR in the Studies of Proteins: Relation to Protein Function and Stability 1344
NMR-based Metabonomics Techniques and Applications 1352
Protein Misfolding Disease: Overview of Liquid and Solid-State High Resolution NMR Studies 1361
19F NMR Spectroscopy for Functional and Binding High-Throughput Screening 1366
Applications of Receptor-Based NMR Screening in Drug Discovery 1373
NMR SHAPES Screening 1380
NMR-Based Screening Applied to Drug Discovery Targets 1389
NMR and Structural Genomics in the Pharmaceutical Sciences 1399
Author Index 1405
Subject Index 1407
Modern Magnetic Resonance Part 3: Applications in Materials Science and Food Science 1418
Contents 1422
Preface 1427
Color Plate Section 1428
Part III, Section 1: Applications in Materials Science 1443
Foreword to Applications in Materials Science 1444
Acoustically Stimulated NMR Relaxometry: Application to the Study of Molecular Dynamics in Liquid Crystalline Materials 1446
Characterization of Elastomers Based on Monitoring Ultraslow Dipolar Correlations by NMR 1452
Correlating Molecular and Macroscopic Properties of Elastomers by NMR Relaxometry and Multi-pulse NMR Techniques 1461
Determining Structural and Dynamic Distribution Functions from Inhomogeneously Broadened NMR Spectra: The Conjugate Orthogonal Functions Approach 1468
Fluid Diffusion in Partially Filled Nanoscopic and Microscopic Porous Materials 1475
Gas Adsorption on Carbon Nanotubes 1482
Magnetic Resonance Studies of the Heterogeneous Rotational and Translational dynamics in Disordered Materials 1489
Nuclear Magnetic Resonance in Ferromagnetic Multilayers and Nanocomposites: Investigations of Their Structural and Magnetic Properties 1495
1H Solid-State NMR of Supramolecular Systems 1501
Quadrupolar NMR of Inorganic Materials: The Multiple-Quantum Magic Angle Spinning Experiment 1509
Rheo-NMR Spectroscopy 1517
Advances in Single-Sided NMR 1524
Site-specific Characterization of Structure and Dynamics of Complex Materials by EPR Spin Probes 1529
NMR of Organic Semiconductors 1538
Solid State NMR of Xerogels 1545
Solid-State 17O NMR Spectroscopy of High-Pressure Silicates 1549
The Structure of Oxide Glasses: Insights from 17O NMR 1560
Studies of the Local Structure of Silk Using Solid-State NMR 1566
Velocity Imaging of Granular Materials 1577
Part III, Section 2: Applications in Food Science 1584
Foreword to Applications in Food Science 1585
Glossary 1586
High Resolution Solution State Methods 1588
Characterization of the Chemical Composition of Beverages by NMR Spectroscopy 1589
High Resolution NMR of Carrageenans 1596
Flavor–Food Compound Interactions by NMR Spectroscopy 1602
High-Resolution Nuclear Magnetic Resonance Spectroscopy of Fruit Juices 1607
High-Resolution NMR Spectroscopy in Human Metabolism and Metabonomics 1612
High-Resolution NMR of Milk and Milk Proteins 1620
High-Resolution 13C Nuclear Magnetic Resonance in the Study of Oils 1625
High-Resolution 1H Nuclear Magnetic Resonance in the Study of Oils 1632
SNIF-NMR—Part 3: From Mechanistic Af.liation to Origin Inference 1655
SNIF-NMR—Part 4: Applications in an Economic Context: The Example of Wines, Spirits, and Juices 1667
High-Resolution Nuclear Magnetic Resonance Spectroscopy of Wine, Beer, and Spirits 1674
Relaxation Time Methods 1680
NMR Relaxation of Dairy Products 1681
Characterization of Molecular Mobility in Carbohydrate Food Systems by NMR 1686
Diffusion and Relaxation in Gels 1696
NMR Relaxation and Diffusion Studies of Horticultural Products 1703
Proton NMR Relaxometry in Meat Science 1710
Time-Domain NMR in Quality Control: More Advanced Methods 1715
Time-Domain NMR in Quality Control: Standard Applications in Food 1719
Nuclear Magnetic Relaxation in Starch Systems 1724
High Resolution Solid State Methods 1734
Magic Angle Spinning NMR of Flours and Doughs 1735
High-Resolution Magic Angle Spinning NMR Spectroscopy of Fruits and Vegetables 1742
High-Resolution Solid-State NMR of Gluten and Dough 1746
High-Resolution Solid-State NMR as an Analytical Tool to Study Plant Seeds 1754
High-Resolution Solid-State NMR Spectroscopy of Starch Polysaccharides 1759
Imaging and Related Techniques 1768
NMR Imaging of Bread and Biscuit 1769
NMR Imaging of Dairy Products 1774
NMR Imaging of Dough 1780
MRI in Food Process Engineering 1786
Rheo-NMR: Applications to Food 1792
Temperature Measurements by Magnetic Resonance 1798
Statistical Methods 1804
Chemometric Analysis of NMR Data 1805
Direct Exponential Curve Resolution by SLICING 1816
ESR Methods 1824
ESR as a Technique for Food Irradiation Detection 1825
ESR Spectroscopy for the Study of Oxidative Processes in Food and Beverages 1831
Applications to Food Systems 1837
Magnetic Resonance of Food Freezing 1838
Nuclear Magnetic Resonance Studies on the Glass Transition and Crystallization in Low Moisture Sugars 1848
Probing the Sensory Properties of Food Materials with Nuclear Magnetic Resonance Spectroscopy and Imaging 1858
Single-Sided NMR in Foods 1864
Applications of NMR in the Studies of Starch Systems 1867
Author Index 1876