Verfügbarkeit: Modern magnetic resonance

Modern magnetic resonance: 3 Applications in materials science and food science

Gespeichert in:

Bibliographische Detailangaben
Format:	Buch
Sprache:	English
Veröffentlicht:	Berlin Springer 2006
Online-Zugang:	Inhaltsverzeichnis
Beschreibung:	LV, LXXII, S. 1417 - 1927 Ill., graph. Darst.

Internformat

MARC


LEADER	00000nam a2200000 cc4500
001	BV021482926
003	DE-604
005	20070116
007	t
008	060221s2006 gw ad\|\| \|\|\|\| 00\|\|\| eng d
035			\|a (OCoLC)635043310
035			\|a (DE-599)BVBBV021482926
040			\|a DE-604 \|b ger \|e rakwb
041	0		\|a eng
044			\|a gw \|c XA-DE-BE
049			\|a DE-29 \|a DE-355 \|a DE-91G \|a DE-19 \|a DE-11
245	1	0	\|a Modern magnetic resonance \|n 3 \|p Applications in materials science and food science \|c Graham A. Webb (ed.)
264		1	\|a Berlin \|b Springer \|c 2006
300			\|a LV, LXXII, S. 1417 - 1927 \|b Ill., graph. Darst.
336			\|b txt \|2 rdacontent
337			\|b n \|2 rdamedia
338			\|b nc \|2 rdacarrier
700	1		\|a Webb, Graham A. \|e Sonstige \|4 oth
773	0	8	\|w (DE-604)BV021482869 \|g 3
856	4	2	\|m HBZ Datenaustausch \|q application/pdf \|u http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=014665296&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA \|3 Inhaltsverzeichnis
999			\|a oai:aleph.bib-bvb.de:BVB01-014665296

Datensatz im Suchindex

_version_	1804135164908929024
adam_text	Contents List of Section Editors V Preface VII Foreword (Application in Chemistry) IX Listof Tables XLIX Color Plate Section LVII PARTI G lossary 1 Amyloids 5 Kinetics of Amyloid Fibril Formation of Human Calcitonin 7 Introduction 7 Properties of Fibril Formation of hCT 7 Conformational Changes of hCT 7 Kinetic Analysis of hCT Fibrillation 8 Mechanism of Fibril Formation 12 Conclusion 12 Acknowledgment 12 References 12 Polymorphism of Abheimer s Aß Amyloid Fibrils 15 Acknowledgments 20 References 20 Chemical Shifts and Spin-Couplings 25 13C, 15N, 1H, 2H, and 17O NMR Chemical Shift NMR for Hydrogen Bonds 27 Introduction 27 Hydrogen-bonded Structure and 13C Chemical Shift 27 Hydrogen-bonded Structure and 15N NMR Chemical Shift 28 Hydrogen-bonded Structure and lH NMR Chemical Shift 28 Hydrogen-bonded Structure and 170 NMR Quadrupolar Coupling Constant and Chemical Shift 29 Hydrogen-bonded Structure and 2H Quadrupolar Coupling Constant 30 Conclusion 31 References 31 NMR Chemical Shift Map 33 References 38 NMR Chemical Shifts Based on Band Theory 39 Introduction 39 Theoretical Aspects of Electronic State and Nuclear Shielding in Solid Polymers 39 Interpretation of Nuclear Shielding by the TB Method 41 References 47 Modeling NMR Chemical Shifts 49 Introduction 49 Theory of the Chemical Shieldings 50 Modeling Chemical Shieldings 50 Acknowledgments 57 References 57 Ab Jnitio Calculation of NMR Shielding Constants 59 Introduction 59 Overview of the Theoretical Background 59 Ablnitio Program Packages Capable of Calculating NMR ChemicaL Shielding Tensors 62 Ab Initio Calculation of NMR Chemical Shielding Tensors for Large Molecules 63 References 65 Crystal Structure Refinement Using Chemical Shifts 67 Introduction 67 ComputationaL Methods 67 Applications in Crystal Structure Refinement 70 References 73 The Theory of Nuclear Spin-Spin Couplings 75 Introduction 75 Origin of the Indirect Nuclear Spin-Spin Coupling Interaction 75 Coupled Hartree-Fock Approximation 77 Triplet Instability of Coupled Hartree-Fock Calculation 78 Electron Correlation Effects 78 References 79 Fibrous Proteins 81 Investigation of Collagen Dynamics by Solid-State NMR Spectroscopy 83 Introduction 83 Investigation of Collagen Dynamics by Static Solid-State NMR 83 Application of CP MAS Methods to Study the Molecular Properties of Collagen 85 What Has Been Learned from Solid-State NMR Studies of Collagen? 87 Acknowledgments 88 References 88 Solid-State NMR Studies of Elastin and Elastin Peptides 89 Introduction 89 Studies of Native Elastin Focus Mainly on the Natural-Abundance 13C PopuLations 90 A New Approach for Production of Isotopically Labeled Elastin Utilizes a Mammalian Cell Culture 92 Information on the Hydrophobie Domain of Elastin is Gleaned from Repeating Polypeptides 93 Concluding Remarks 94 Acknowledgments 94 References 94 Structural Analysis of Silk Fibroins using NMR 97 Introduction 97 Structure of B. mori Silk Fibroin Before Spinning (Silk I) 97 Structure of B. mori Silk Fibroin After Spinning (Silk II) 98 Structure of Nephilo davipes Dragline Silk (MaSpl) 100 References 102 Field Gradient NMR 103 NMR Diffusometry 105 Diffusion as a Probe 105 Gradient-Based Diffusion Measurements 105 Experimental Complications 106 Diffusion in Complex Systems 108 Acknowledgment HO References HO Field Gradient NMR of Liquid Crystals 113 Introduction 113 NMR Methods and Diffusion in LCs 113 Lyotropic Applications 115 Thermotropic Applications 116 Other Applications of Field Gradients 117 References 117 Field Gradient NMR for Polymer Systems with Cavities 119 Introduction 119 Diffusion in Polymer Gel Systems 119 Conclusion Remarks 123 References 123 NMR Measurements Using Field Gradients and Spatial Information 125 Introduction 125 Diffusion Coefficient Measurements 125 NMR Imaging 127 Selection of Coherence 128 References 130 Theory and Apptication of NMR Diffusion Studies 131 Theoretical Aspects 131 AppLications of Diffusion NMR 132 References 139 Host-Guest Chemistry 141 Solid-State NMR in Host-Guest Chemistry 143 Introduction 143 The Solid-State Spectrum 143 General Characterization 144 Structural Information from Spin Vz Nuclei 144 Distance Measurements 146 Spin Counting 146 Probing Pore Spaces 146 MRI 147 Dynamics 147 References 148 Imaging 151 Mapping of Flow and Acceleration with NMR Microscopy Techniques 153 Introduction 153 Encoding Principles and Pulse Sequences 153 Experiments 156 Conduding Remarks 157 References 158 Industrial Application of In situ NMR Imaging Experiments to Steel-Making Process 159 References 166 Biomedkal NMR Spectroscopy and Imaging 169 Introduction 169 Tracking of Metabolites: In Vivo 13C NMR Images with H-l Detection 169 Physiological Properties: pH 170 Temperature Image and Navigation Surgery Under MRI Guidance 171 Cellular Tracking 172 Concluding Remarks 174 References 174 Electron Spin Resonance Imaging in Polymer Research 175 Introduction 175 ESR Spectra in the Presence of Field Gradients 175 Spatially-Resolved Degradation from ESRI Experiments 177 Acknowledgments 179 References 180 NMR Imaging: Monitoring of Swelling of Environmental Sensitive Hydrogels 183 Hydrogels 183 Swelling Process 183 Advantages of NMR Imaging and Application on Network Characterization 183 Experimental 184 Volume Phase Transition, Net Chain Mobility, and T-Stimulus 186 Diffusion of Low Molecular Weight Compounds 186 Distribution of Water Inside the Gel 187 Diffusion Coefficients Inside the Gel—Structure of Non-homogeneous Networks 187 Acknowledgment 189 References 189 Inorganic Materials and Catalysis 191 Exploiting JH- 29Si Cross-Polarization Features for Structural Characterization of Inorganic Materials 193 Introduction 193 1H- 29 Si CP Dynamics: Basic Features and Pitfalls 193 Silica Gels 195 Layered Sodium Hydrous Silicates 196 Probing the Geometry of Strongly Hydrogen-Bonded Silanols 197 Conclusions 199 References 199 Solid State NMR Characterization of Solid Surface of Heterogeneous Catalysts 201 Surface Acidity of Heterogeneous Catalysts 201 Catalytic Reaction on the Surface of Heterogeneous Catalysts 203 References 207 Isotope Labeling 209 Recent Developments in Stable-Isotope-Aided Methods for Protein NMR Spertroscopy 211 Introduction 211 Positive Labeling (Use of 13C and 15N) 211 Negative Labeling (Use of2H) 214 Concluding Remarks 217 Acknowledgment 217 References 217 Structural Glycobiology by Stable-isotope-assisted NMR Spertroscopy 219 Introduction 219 Three-Dimensional HPLC Mapping 219 Stable Isotope Labeling of Glycoproteins 219 Carbohydrate-Protein Interactions 223 Concluding Remarks 223 Acknowledgments 223 References 224 Lipid Bilayer and Bicelle 227 Development and Application of Bicelles for Use in Biological NMR and Other Biopriysical Studies 229 Bicelle Roots 229 Early 1990s 230 Late 1990s 231 2000-2005 231 Conclusion: How Good are Bicelles as Model Membranes? 232 Acknowledgment 233 References 233 Nuclear Magnetic Resonance of Oriented Bilayer Systems 237 Introduction 237 Magnetically Oriented Bilayer Systems 237 Mechanically Oriented Bilayer Systems 239 Orientation Dependence of Chemical Shift Interaction 240 Orientation Dependence of Di polar Interaction 241 Structure Determination of Membrane Associated Peptides in the Magnetically Oriented Systems 242 Conclusions 242 References 243 Solid-State Deuterium NMR Spectroscopy of Membranes 245 Equilibrium and Dynamical Properties of Membrane Lipids are Studied by Solid-State Deuterium NMR 245 Deuterium NMR Spectroscopy Allows Direct Observation of Coupling Tensors Related to Molecular Structure and Dynamics 246 Molecular Structures and Motions are Revealed by Deuterium NMR Lineshapes 247 Deuterium NMR Provides Order Parameters Related to Average Membrane Properties 248 Deuterium Spin-Lattice Relaxation Times Reveal Dynamical Properties of Lipid Membranes 250 Model-Free Analysis Suggests that Collective Membrane Motions Govern the Relaxation 251 Spectral Densities and Correlation Functions are Derived for Simplified Models in Closed Form 252 Deuterium NMR Relaxation Allows Detailed Comparison of the Structural and Dynamical Properties of Membranes 254 Acknowledgments 255 References 255 Solid State 19F-NMR Analysis of Oriented Biomembranes 257 Introduction 257 19F-NMRExperimentalAspects 257 Strategies for Structure Analysis 257 19F-Labelingof Peptides 259 Structure Analysis of Membrane-Associated Peptides 259 Fusogenic Peptide B18 260 Antimicrobial Peptide Gramicidin S 261 Antimicrobial Peptide PGLa 261 Antimicrobial Peptide K3 262 Perspectives 262 Acknowledgments 262 References 262 Membrane-Assoriated Peptides 265 Solid-State NMR Studies of the Interactions and Strurture of Antimicrobial Peptides in Model Membranes 267 Introduction 267 Effects of Antimicrobial Peptides on Model Lipid Membranes 267 Study of Antimicrobial Peptides in Membranes 269 Conclusions 273 References 273 Anisotropie Chemical Shift Perturbation Induced by Ions in Conducting Channels 275 Acknowledgments 279 References 279 NMR Studies of Ion-Transporting Biological Channels 281 References 283 Membrane Proteins 285 Site-Directed NMR Sitidies on Membrane Proteins 287 Introduction 287 Conformation-Dependent 13C Chemical Shifts 287 Site-Directed Assignment of 13C NMR Signals 288 Dynamic Aspect of Membrane Proteins 289 Surface Structures 290 Site-Directed 13C NMR on Membrane Proteins Present as Monomers 290 Concluding Remarks 292 References 292 Strurture of Membrane-Binding Proteins Revealed by Solid-State NMR 295 Dynamic Structure of the Membrane-Binding Proteins at the Membrane Surface 296 Application of the Solid-State NMR on the PLC-61 PH Domain 296 References 299 Solid-State NMR of Membrane-Active Proteins and Peptides 301 Chemical Shift Anisotropy (CSA) 302 Quadrupolar Coupling 304 31Pand2HNMRof Lipids 305 Dipolar (Re)-Coupling 305 Conclusion 306 References 306 Magnetic Resonance Spectroscopic Studies of the Integral Membrane Protein Phospholamban 309 Phospholamban 309 Solid-State NMR Spectroscopic Studies of PLB 310 Magnetic Resonance Spectroscopic Studies of the AFA-PLB Monomer 312 Acknowledgments 313 References 313 NMR Studies of the Interactions Between Ligands and Membrane-Embedded Receptors: New Methods for Drug Discovery 315 Introduction 315 Choice of Technique 315 Solution NMR Methods ......... ... ............!!..... 316 Solid-State NMR Methods 317 A Case Study: Solid-State NMR Investigations of Ion Pump Inhibitors 320 Future Prospects 321 References 322 Photosynthetic Antennae and Reaction Centers 323 Introduction 323 Structure-Function Studies of Antenna Systems and RCs 323 MAS NMR Structure Determination: Chlorosomes and LH2 326 References 329 Insight into Membrane Protein Structure from High-Resolution NMR 331 Introduction 331 Membrane Protein Structure—Current Status 331 Peptides frorn Helices and Turns have Intrinsic Structures that can Provide Secondary Structure Information About the Parent Soluble Protein 331 Structures of Peptide Fragments from Membrane Proteins can Provide Secondary Structure Information 332 Protein Fragments of Other Membrane Proteins 334 General Features of the Studies on Membrane Protein Fragments 335 How Sparse Long-Distance Experimental Constraints can be Combined with Fragment Structures to Build a Structure of the Intact Membrane Protein 336 New High-Resolution NMRStudies on Intact Membrane Proteins 337 References 337 New Developments 341 Fast Multidimensional NMR: New Ways to Explore Evolution Space 343 The Filter DiagonaLization Method 343 Spatially Encoded Single-Scan NMR 345 Fiadamard Encoding 345 Projection-Reconstruction 347 Acknowledgments 348 References 348 High-Sensitivity NMR Probe Systems 349 Sensitivity Issues in NMR Spectroscopy 349 Thermodynamics 350 Polarization Transfer 350 Optimized Detection Coil Design 353 Magnetic Resonance Force Microscopy 354 References 357 CRAMPS 359 Introduction 359 Theory 359 Experimental 363 Applications 365 Acknowledgments 366 References 366 Mobile NMR 369 Introduction 369 Measurement Methods 369 Applications 372 Summa ry 375 Acknowledgments 375 References 376 Rheo-NMR 379 Suggested Reading 383 Analytical Aspects of Solid-State NMR Spectroscopy 385 Introduction 385 Uses of Isotropie Shielding to Identify MateriaLs 385 Uses of Shielding Tensors to Identify Materials 386 Using Quadrupolar Coupling to Identify Materials 387 Structure Determination 388 Quantification with Solid-State NMR Spectroscopy 388 Summary 389 Acknowledgment 389 References 389 3H NMR and Its Application 391 Introduction 391 Radiochemical Facilities and Radiation Safety 391 Tritiation Procedures 391 Tritium NMR Spectroscopy 392 Applications 393 Conclusions 394 References 394 On-line SEC-NMR 395 On-line Coupling of LC and NMR 395 On-line SEC-NMR 395 Molecular Weight Determination of Polymers 396 LCCAP-NMR 400 References 401 NOE and Chemical Exchange 403 The Nuclear Overhauser Effect 405 Introduction 405 Theoretical Background 405 Applications of the NOE 407 References 408 Solute-Solvent Interactions Examined by the Nuclear Overhauser Effect 409 Background 409 Intramolecular NOEs 409 Intermolecular NOEs 410 Magnitudes of Intramolecular and Intermolecular NOEs 410 Solute-Solvent Interactions 410 Experimental Detection of Intermolecular Cross-Relaxation 412 Xenon-Solvent Interactions 412 Small Molecule-Water Interactions 412 Micelle-Water Interactions 412 Small Molecule-Organic Solvent Interactions 413 Selective Solute Interactions in Mixed Solvent Systems 413 Biomolecule-Water Interactions 414 Summary 415 References 416 Chemical Exchange 417 Introduction 417 Types of Chemical Exchange 417 Theory 419 Kinetics 419 Experimental Precautions 420 Intermediate Exchange 420 Slow Exchange 421 Fast Exchange 422 Summary 422 References 422 NQR ESR 425 Separated Detection of H-Transfer Motions in Multi-H-Bonded Systems Studied by Combined H NMR and 35Cl NQR Measurements 427 Introduction 427 High Sensitivity of NQR Shown in 4-Chlorobenzoic Add 427 Separated Detections of H-Transfer Modes in Multi-H-Bonded Systems 428 Conclusion 432 References 434 EPR: Principles 435 Angular Momentum 435 Spin-Orbit Interaction 435 Zeeman Interaction 435 Spin Hamiltonian 436 S = y2 Systems 436 NO Molecule 437 5 % Systems «9 References 440 Zero Field NMR: NMR and NQR in Zero Magnetic Field 441 An Historical Perspective: Field-Cyding NMR 441 Sensitivity Enhancement of Low-y Nuclear Quadrupole Resonance 442 Zero Field NMR: Experimental Details 442 Extensions of Zero Field NMR and NQR 446 Zero Field NMR and NQR: Limitations and Prospects? 446 References 447 Organo Metallic Chemistry 449 Organoboron Chemistry 451 References 453 Organogermanium Chemistry 455 References 455 Organotin Chemistry 457 References 459 ! Paramagnetic Effects 461 aH and 13C High-Resolution Solid-State NMR of Paramagnetic Compounds Under Very Fast Magic Angle Spinning 463 Introduction 463 One-Dimensional (1D) aH SSNMR for Paramagnetic Systems 463 1D 13C VFMAS SSNMR for Paramagnetic Systems 465 Signal Assignments and Multi-dimensional NMR 468 Experimental Aspects 469 Conclusion 469 Acknowledgments 469 References 469 Paramagnetic Effects of Dioxygen in Solution NMR—Studies of Membrane Immersion Depth, Protein Topology, and Protein Interactions 471 Introduction 471 Spin-Lattice Relaxation 471 Chemical Shift Perturbations 472 Immersion Depth 472 Membrane Protein Topology 474 Protein-Protein Interactions 477 Additional Applications: Family Fold Recognition and O2 Migration Pathways 478 Final Comments 478 References 478 Protein Structure 481 TROSY NMR for Studies of Large BiologicaL Macromolecules in Solution 483 Introduction 483 Technical ßackground 483 TROSY Applications for Studies of Large ßiological Macromolecules 486 Cross-Correlated Relaxation-Induced Polarization Transfer for Studies of Very Large Structures 490 Conclusion and Outlook 490 Acknowledgments 491 References 491 NMR Insight of Structural Stability and Folding of Calcium-Binding Lysozyme 493 Lysozyme and Calcium Binding of the Homologous Proteins 493 Protein Folding Mechanism 493 1H Chemical Shift Calculation of the Calcium-Binding LYS in the Structural Intermediate 494 H/D Exchange of Calcium-Binding LYS in the Native and the Structural Intermediate 495 References 497 NMR Investigation of Calmodulin 499 Biological Functions 499 Two-Dimensiona^H NMR 500 Multidimensional and Heteronuclear NMR of CaM 501 Solution Structure of CaM 501 Metal and CaM Interactions 501 Calcium-Calmodulin-Peptide Complexes 504 Acknowledgment 509 References 509 Analytical Framework for Protein Structure Determination by Solid-State NMR of Aligned Samples 513 Introduction 513 A Spherical-Basis Treatment of Experimental Angular Constraints for Protein Structure Determination 515 Examples of Structural Fitting 517 Conclusions 521 Acknowledgements 521 References 521 Determining Protein 3D Structure by Magic Angle Spinning NMR 523 Introduction 523 SampLe Preparation and Methodology 523 Applications 524 Conclusions 525 Acknowledg ments 525 References 525 19F NMR Study of 6-Type Haemoproteins 527 Introduction 527 19F Labeling of 6-Type Haemoproteins Using Reconstitution 528 19F NMR vs. rH NMR 529 Haem Disorder 533 MbO2 vs. MbCO 533 Summary 533 References 533 Polymer Structure 535 NMR in Dry or Swollen Temporary or Permanent Networks 537 Introduction 537 Polymeric Dynamics 537 Effect of Local Friction and Spin-Lattice Relaxation 537 Chain Diffusion 538 Statistical Polymeric Structures and Spin-Spin Relaxation 538 ConcLusion 539 References 539 Crystalline Structure of Ethylene Copolymers and Its Relation to the Comonomer Content 541 Polymorphism of Ethylene Copolymers 541 The Biexponential 13C h Relaxation Behavior of the Crystalline Region 542 References 545 Isomorphism in Bacterially Synthesized Biodegradable Copolyesters 547 Introduction 547 Isomorphous Behavior of Bacterially Synthesized Copolyesters 547 Cocrystallization and Phase Segregation in P(3HB)/P(3HB-co-3HV) Blends 549 References ^ 51 Two-Dimensional NMR Analysis of Stereoregularity of Polymers 553 Poly(Methyl Methacrylate) 553 Methyl Acrylate (A)/Methyl Methacrylate (B) Copolymer 554 References 558 Quantitative Analysis of Conformations in Disordered Polymers by Solid-State Multiple-Quantum NMR 559 Introduction 559 Characterization of Conformations in Atactic Polymers by Two-Dimensional Experiments 559 Selective Observation of Respective Conformers in Polymers by Zero-Quantum (ZQ) Experiments 560 References 562 Polymer Microstructure: The Conformational Connection to NMR 563 Introduction 563 13C NMR Spectral Assignments 563 •y-Gauche-Effect 564 Example of the -y-Gauche-Effect 565 PP Stereosequences From 13C NMR 566 13C NMR of Solid Polymers 566 Application of Solid-State 13C NMR to Polymers 568 Summary 569 References 570 Solid-State NMR Characterization of Polymer Interfaces 571 Overview 571 Solid-State Proton NMRStudies 571 Solid-State Heteronuclear NMRStudies 574 Dynamics at the Interface 575 Outlook and Conclusions 577 References 577 The Structure of Polymer Networks 579 Introduction 579 The Chemical Structure of Polymer Networks 579 The Physical Structure of Polymer Networks 582 Summary 584 References 584 H CRAMPS NMR of Polypeptides in the Solid State 587 Introduction 587 Experimental Evidence 587 References 599 Polymer Dynamics 601 Dynamics of Amorphous Polymers 603 Introduction 603 Spin Relaxation 603 One-Dimensional MAS Spectra 604 Lineshape Analyses 605 20 Exchange Spectra 607 References 608 Molecular Motions of Crystalline Polymers by Solid-State MAS NMR 611 Overview 611 1D-MAS Exchange NMR 611 Mechanical Property vs. Chain Dynamics 611 Crystal Transformation vs. Molecular Dynamics 612 Concluding Remarks 614 References 614 Dynamics in Polypeptides by Solid State 2H NMR 617 Introduction 617 Methyl Group 617 Phenyl Ring 618 Side Chain of Poly(-y-benzyl L-glutamate) (PBLG) 619 Main Chain Dynamics 622 Acknowledgments 623 References 623 Polymer Blends 625 Polymer Blends 627 Overview 627 Interaction in Polymer Blends 627 Miscibility 628 Phase Separation Process 630 Conclusion Remarks 631 References 631 Configurational Entropy and Polymer Miscibility: New Experimental Insights From Solid-State NMR 633 Introduction 633 Experimental NMR Methods 634 Choice of PoLymer Blend System 635 129Xe NMR of Absorbed Xenon Gas 635 Two-Dimensional Exchange NMR to Probe Slow-Chain Reorientation 636 2H NMR Data and Simulations 638 Conclusions 640 References 640 Quantum Information Processing 641 Quantum Information Processing as Studied by Molecule-Based Pulsed ENDOR Spectroscopy 643 Introduction 643 Pseudo-Pure States and Quantum Entanglements 643 Molecular ENDOR Based Quantum Computer 644 Preparation of the Molecular Entity for QC-ENDOR 646 Implementation of SDC by Pulsed ENDOR 647 Conclusion * 49 References 650 Residual Dipolar Couplings and Nucleic Acids 651 New Applications for Residual Dipolar Couplings: Extending the Range of NMR in Structural Biology 653 Background 653 Theory 653 Protein Structures 654 DNA/RNA 654 Pseudocontact Shifts 656 Unfolded Denatured Proteins 657 Oügosaccharides and SmallOrganic Molecules 657 Conclusions 658 References 658 Refinement of Nucleic Acid Structures with Residual Dipolar Coupling Restraints in Cartesian Coordinate Space 661 Introduction 661 Loop ß RNA from Domain IV of the Enterovirus Internat Ribosome Entry Site 662 Structural Restraints 662 Structure Refinement 663 References 665 Conformational Analysis of DNA and RNA 667 Introduction 667 Conformation of Nucleotides 667 NMR Signal for DNA and RNA and Their Assignment 667 Structural Analysis 669 References 671 Solid-State NMR Technique 673 Analytical and Numerical Tools for Experiment Design in Solid-State NMR Spectroscopy 675 Introduction 675 Tools for Systematic Experiment Design 675 Systematic Design of Solid-State NMR Experiments 679 Conclusions 682 Acknowledgements 682 References 682 Homonuclear Shift-Correlation Experiment in Solids 685 References 689 Two-Dimensional 170 Multiple-Quantum Magic-Angle Spinning NMR of Organic Solids 691 Introduction 691 Pulse Sequence, Data Processing, and Spectral Analysis 691 Sensitivity of 170 MQMAS Experiments 694 Conclusion 694 Acknowledgment 696 References 696 A Family of PISEMA Experiments for Structural Studies of Biological Solids 699 An Ideal SLF Sequence 699 Offset Effects 699 Offset Compensation by BB-SEMA 700 SEMA Requires Very High RF Power 702 TANSEMAfor Low RF Power Experiments 703 PISEMA of SIn 703 Summary 704 Acknowledgments 704 References 704 Structural Constraints in Solids 707 Rotational-Echo, Double-Resonance NMR 709 Introduction 709 Dipolar Recoupling 709 Practical Details 710 References 714 REDOR in Multiple Spin System 715 Introduction 715 Dipolar Dephasing of REDOR in I-S„ Multiple Spin System 715 Obtaining Accurate Internuclear Distances by REDOR 717 DipoLar Dephasing of REDOR in Multiple Spin System 719 Conclusions 720 References 720 Torsion Angle Determination by Solid-State NMR 723 Static Tensor Correlation Techniques 723 MAS Tensor Correlation Techniques 723 Distance Methods for Determining Torsion Angles 728 Conclusion 728 References 728 Secondary Structure Analysis of Proteins from Angle-Dependent Interactions 731 Introduction 731 NMR Methods for the Secondary Structure Analysis of Proteins 731 Torsion Angle Measurements from the Mutual Orientation of Anisotropie Interactions for the Secondary Structure Analysis 734 References 735 Telomeric DNA Complexes 737 Comparison of DNA-Binding Activities Between hTRF2 and hTRFl with hTRF2 Mutants 739 Introduction 739 Results 739 Acknowledgments 745 References 747 Glossary 749 Optimization of MRI Contrast for Pre-Clinical Studies at High Magnetic Field 753 Introduction 753 Physics Background for Contrast Optimization 753 MR Contrast Agents for Animal Imaging Studies 758 Conclusion 761 Acknowledgement 761 References 761 The Application of In Vivo MRI and MRS in Phenomic Studies of Murine Models of Disease 763 Introduction 763 Magnetic Resonance Imaging 763 Magnetic Resonance Spectroscopy 770 Conclusions 776 Acknowledgement 776 References 776 Experimental Models of Brain Disease: MRI Contrast Mechanisms for the Assessment of Pathophysiological Status 781 Introduction 781 Image Contrast and Intrinsic MR Parameters 781 Taking Advantage of MR Sensitivity to Dynamic Physiological Processes 783 Using Exogenous Contrast Agents to Enhance Image Contrast 784 Manipulating the MR Signal to Measure Physiological Parameters 786 Conclusions 791 Acknowledgments 792 References 79Z Experimental Models of Brain Disease: MRI Studies 795 Introduction 795 Practical Issues 795 CerebraL Ischemia 797 Spreading Depression 800 Epilepsy 80l Neurodegenerative Disorders 803 CNS Inflammation 804 Traumatic Brain Injury 806 Conclusion 808 Acknowledgments 808 References 808 Application of MRS in Cancer in Pre-clinical Models 817 Introduction 817 Tumor BioLogy and Physiology 817 Condusion 824 Acknowledgement 824 References 824 Experimental Cardiovascular MRin Small Animals 829 Introduction 829 Methods and Requirements 829 Global Cardiac Function 833 Myocardial Tissue Contractility 836 Multinuclear MR Spectroscopy 839 VascularMRI 842 Conclusion and Future Perspective 843 Acknowledgements 843 References 844 Application of Pharmacological MRI to Preclinical Drug Discovery and Development 849 Introduction 849 Surrogate Markers of Neuronal Activity 849 Image Acquisition Strategies for Preclinical phMRI 852 Effects of Anesthesia 854 Data Analysis 856 Using Dopamine Receptor Agonists as Prototypical Agents for Animal phMRI 859 The Future of phMRI 867 References 868 Application of MRI to Cell Tracking 873 Introduction 873 Intracellular MRI Contrast Agents 873 Properties of a Good Contrast Agent for CelL Tracking 874 MRI Contrast Agent for Cell Tracking 874 Paramagnetic Agents 874 Superparamagnetic Agents 874 Engineering Delivery Systems for Iran Oxide Contrast Agents 875 Delivery of Contrast Agent with Transfection Agents 875 Delivery of Contrast Agent Using Specifk Targeting 875 Cytotoxicity and Metabolism 877 Conjugation Chemistry: Attaching Contrast Agent to Delivery Ligand 877 MRI Tracking of Stem Cells in the Heart 879 MRI Tracking of Stern CeLLs in the CNS 880 MRI Tracking of Cell-Based Tumor Therapy 882 Acknowledgment 882 References 883 Glossary 885 Introduction 886 Comprehensive Compositional Analysis of Fish Feed by Time Domain NMR 887 Introduction 887 Experimental 887 Results and Discussion 890 Conclusions 892 AcknowLedgments 893 References 893 Low Field NMR Studies of Atlantic Satmon (Salmo salar) 895 Introduction 895 Materials and Methods 896 ResuLts and Oiscussion 899 Conclusion 902 References 902 Water Distribution and Mobility in Fish Products in Relation to Quality 905 Introduction 905 Algorithms 905 Applications 906 References 908 Proton NMR of Fish Oils and Lipids 909 Introduction 909 aH-NMR Spectra of Fish Oils and Lipids Extracted from Fish Musdes 909 Quantitative Determination of n-3 PUFAs 909 Proton NMR and Lipolysis 911 Oxidation Products 912 Application Remarks 913 References 913 Determination of Fatty Arid Composition and Oxidation in Fish Oils by High Resolution Nuclear Magnetic Resonance Spectroscopy 915 Fatty Acid Analysis of Fish Oils 915 The !H NMR Spectra of Fish Oils 915 The 13C NMR Spectra of Fish Oils 915 Fish Oil Oxidation and its Evaluation by NMR 917 Conclusions 91^ Acknowledgments ° References 920 Resonance Spectroscopy to Study Lipid Oxidation in Fish and Fish Products 923 Electron Spin Resonance Spectroscopy 923 Investiqation of Free Radicals in Marine Lipids 924 NMR... 926 Concluding Remarks 928 Acknowledgements 929 References 930 Omega-3 Fatty Acid Content of Intact Muscle of Farmed Atlantic Salmon (Salmosalar) Examined by JH MAS NMR Spectroscopy 931 Introduction 931 Experimental Procedures 931 Results and Discussion 932 References 935 HR MAS NMR Spectroscopy of Marine Microalgae, Part 1: Classification and Metabolite Composition from HR MAS 1H NMR Spectra and Multivariate Analysis 937 Introduction 937 Results and Discussion 937 Conclusion 940 References 941 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 943 Introduction 943 Results and Discussion 944 Conclusion 946 References 947 Post-mortem Studies of Fish Using Magnetic Resonance Imaging 949 Introduction 949 Materials and Methods 950 Results and Discussion 951 Conclusions 955 Acknowtedgment 956 References 956 Howis the Fish Meat Afferted by Technological Processes? 957 Introduction 957 Study of SaLt Interaction in Smoked Salmon by SQ and DQF MRS 957 MRI Study of Salt and Fat Distribution in Smoked Salmon 958 Conclusion 961 References 961 PART II Foreword 963 Abbreviations 964 Metabolite Abbreviations 965 Glossary of Terms 967 Acquiring Neurospectroscopy in Clinical Practice 971 Part I: Seven Secrets to Successful Spectroscopy 971 Introduction 971 Signal and Homogeneity 971 Acquisition Paradigms 972 Patient Positioning 972 Sequences 974 Echo Time 974 VoxelSize 975 Number of Averages 976 Voxel Position 976 Consistency 978 Multivoxel Spectroscopy 979 Part II: Neurospectroscopy Protocols 980 Protocol 1: Standard Gray Matter (GM) or Posterior Cingulate Gyrus (PCG) 981 Protocol 2: Standard White Matter 983 Protocol 3: Frontal GM 983 Protocol 4: Hippocampus/Temporal Lobe 983 Protocol 5: Multivoxel Neurospectroscopy (For Focal Use Only) 986 Summary 988 Acknowledgments 989 Suggested Reading List for Clinical Neurospectroscopy Protocols 989 Application of Magnetic Resonance for the Diagnosis of Infective Brain Lesions 991 Introduction 991 Magnetic Resonance Techniques 991 Contrast Enhancement 993 Conventional MRI of Infective Brain Lesions 993 Other MRI Methods 994 Magnetic Resonance Spectroscopy 995 Data Analysis 996 Summary 997 Glossary of Terms 997 References 997 Application of 2D Magnetic Resonance Spectroscopy to the Study of Human Biopsies 1001 Introduction 1001 Application of 2D NMR Spectroscopy to Cells and Tissues 1002 Data Acquisition 1005 Data Processing 1006 Concluding Remarks 1010 Acknowledgments 1010 References 1010 Correlation of Histopathology with Magnetic Resonance Spectroscopy of Human Biopsies 1013 Introduction 1013 Histopathology—Strengths and Limitations 1013 Collection and Storage of Biopsy Specimens for Analysis 1014 Collection of a FNAB 1015 Preparation of Specimens for MRS 1016 ExperimentalTemperature 1017 Magnetic Field Strength 1017 MR Spectroscopy Methods 1017 After MR Spectroscopy 1018 Assignments and Visual Inspection of the Data 1018 The Complexity of Tumor Development and Progression 1018 Pattern Recognition Methods 1018 Regression Analysis 1021 Future Challenges 1021 Acknowledgments 1021 References 1021 Functional MRI 1023 Principi.es offMRI 1023 Design offMRI Trials 1023 Prindples of ExperimentaL Design 1025 Prinriples of Analysis 1026 Artifactsand Pitfalis 1027 Practicai AppLications 1028 Conclusion 1032 Abbreviations 1035 Further Reading 1035 High Resolution Magic Angle Spinning (HRMAS) Proton MRS of Surgical Sperimens 1037 List of Abbreviations 1037 Introduction 1037 Methodology 1038 HRMAS MRS of Human SurgicaiSpecimens 1040 Future Developments and Conciusions 1048 Giossary of Terms 1048 Acknowledg ments 1049 References 1049 Intraoperative MRI 1051 Historical Miiestones in Neurotogy 1051 Principles of Intraoperative Imaging 1051 Hardware and Configuration 1051 Clinical AppLications of iMRI 1053 Neoplasia 1055 Epilepsy 1055 Vascular disorders 1058 Spine 1059 Future Directions 1059 Bioi nformatics 1061 Acknowledgments 1062 References 1062 In Vivo Magnetic Resonance Spectroscopy in Breast Cancer 1063 Introduction 1063 In vivo Localization in MRS 1063 31P M R Spectroscopy 1064 JH MR Spectroscopy of Breast 1065 Future Directions and Conciusions 1070 Acknowledgments 1071 References 1071 In Vivo Molecular MR Imaging: Potential and Limits 1073 Introduction 1073 Detectability 1073 Cell Labeling 1076 In vivo MRI Experiments 1077 Biological Aspects of Cell Labeling 1078 Summary 1081 Outlook 1081 Acknowledgment 1081 GLossary of Terms 1081 References 1082 In vivo 13C MRS 1085 Introduction 1085 Methods 1085 Pulse Sequences for in vivo 13C MRS 1088 Checking System Performance 1089 Data Processing 1091 Modeling and Determination of Flux Rates 1092 MisceLlaneous 1093 Applications 1093 Hyperpolarized 13C Compounds 1096 Acknowledgments 1096 Glossary 1096 References 1098 Magnetic Resonance Spectroscopy and Spectroscopic Imaging of the Prostate, Breast, and Liver 1099 Introduction 1099 Techniques for Spectroscopy and Spectroscopic Imaging of the Body 1100 Applications in the Prostate, Breast, and Liver 1105 Summary 1107 Acknowledgments 1108 Glossary of Terms 1108 References 1109 MR-Mammography 1113 Introduction 1113 History of MRM 1113 Pathophysiological Background of MRM 1114 Technique 1122 Indications for MRM 1122 Discrepancies and Pitfalls 1123 Future Challenges 1124 References 1125 Internet Resources 1127 Phosphorus Magnetic Resonance Spectroscopy on Biopsy and In Vivo 1129 Features of 31P MRS in Tissues 1129 31P MRS of Tissue Biopsy Samples 1132 31PMRSJf7 Vivo 1137 References 1144 Radio Frequency Coils for Magnetic Resonance Spectroscopy 1149 The Requirements 1149 The Issues 1H9 The Solenoid Coil and Saddle-Shape Coil 1150 SurfaceCoil 1150 Superconducting rf Coils 1152 PhasedArray 1152 ßi Homogeneity Vs. SNR 1152 Transmit-Only and Receive-Only Coils 1153 LocaL rf CoiLs with Improved ßi Homogeneity and SNR 1154 Implanted rf Coils 1154 Microcoils 1154 Dual Frequency rf Coils 1155 Summary 1155 Glossary of Terms 1155 References 1155 Spatially Resolved Two-Dimensional MR Spectroscopy in vivo 1157 Introduction 1157 Single- and Multi-voxel Based 1D aH MR Spectroscopy 1157 Single Volume Localized 2D XH MR Spectroscopy 1159 Artefacts in Localized ZD MRS and SimuLation 1166 Multi-Voxel Based 2D 1H MR Spectroscopy 1166 Summary 1168 Acknowledgment 1168 References 1168 Glossary 1171 Overview of NMR in the Pharmaceutical Sciences 1171 Applications of Cryogenic NMR Probe Technology for the Identification of Low-Level Impurities in Pharmaceuticals 1171 Flow NMR Techniques in the Pharmaceutical Sciences 1171 Developments in NMR Hyphenation for Pharmaceutical Industry 1171 LC-NMR in Dereplication and Stracture Elucidation of Herbai Drugs 1171 New Approaches to NMR Data Acquisition, Assignment and Protein Structure Determination: Potential Impact in Drug Discovery 1171 Transferred Cross-CorreLated Relaxation: Application to Drug/Target Complexes 1172 Novel Uses of Paramagnets to Solve Complex Protein Structures 1172 Fast Assignments of 15N-HSQC Spectra of Proteins by Paramagnetic Labeling 1172 Phospholipid Bicelle Membrane Systems for Studying Drug Molecules 1172 Partial Alignmentfor Structure Determination of Organic Molecules 1172 Measurement of Residual Dipolar Couplings and Applications in Protein NMR 1172 Using Chemical Shift Perturbations to Validate and Refine the Docking of Novel IgE Antagonists to the High-Affinity IgE Receptor 1172 Dual-Region Hadamard-Encoding to Improve Resolution and Save Time 1172 Nonuniform Sampling in Biomolecular NMR 1173 Structural Characterization of Antimicrobial Peptides by NMR Spectroscopy 1173 Pharmaceutical Applications of Ion Channel Blockers: Use of NMR to Determine the Structure of Scorpion Toxins 1173 Structure and Dynamics of Inhibitor and Metal Binding to Metallo-ß-Lactamases 1173 NMR Spectroscopy in the Analysis of Protein-Protein Interactions 1173 Identification and Characterization of Ternary Complexes Using NMR Spectroscopy 1173 The Transferred NOE 1173 NMR Kinetic Measurements in DNA Folding and Drug Binding 1174 The Use of NMR in the Studies of Highly Flexible States of Proteins: Relation to Protein Function and Stability 1174 NMR-based Metabonomics Techniques and Applications 1174 Protein Misfolding Disease: Overview of Liquid and Solid-State High Resolution NMR Studies 1174 19F NMR Spectroscopy for Functional and Binding High-Throughput Screening 1174 Applications of Receptor-Based NMR Screening in Drug Discovery. .. . 1174 NMR SHAPES Screening 1175 NMR-Based Screening Applied to Drug Discovery Targets 1175 NMR and Structural Genomics in the Pharmaceutical Sciences 1175 Section Preface 1176 Overview of NMR in the Pharmaceutical Sciences 1177 Introduction 1177 Technical. Developments 1178 Structure-based Design 1179 NMR Screening 1181 Studies of Drug Effects 1182 Future Directions 1182 Acknowledgments 1182 References 1183 Instrumentation 1185 Applications of Cryogenic NMR Probe Technology for the Identification of Low-Level Impurities in Pharmaceuticals 1187 Introduction 1187 Cryogenic NMR Probes 1187 Sample Preparation 1188 Identification of Degradants 1188 Applications of Cryogenic NMR Probe Technology 1189 Condusions 1193 References 1193 Flow NMR Techniques in the Pharmaceutical Sciences 1195 Introduction 1195 LC-NMR 1195 LC-NMR-MS 1196 Other Detectors in LC-NMR 1197 Other Chromatography in LC-NMR 1197 Other Plumbing Schemes: Loop-Collection LC-NMR and Solid-Phase Extraction NMR (SPE-NMR) 1197 Applications of LC-NMR 1197 Limitations of LC-NMR 1197 Flow-Injection Analysis NMR (FIA-NMR) 1197 Direct Injection NMR (DI-NMR) 1198 Complementary Technologies 1199 Condusions 1200 References 1200 Developments in NMR Hyphenation for Pharmaceutical Industry 1203 Introduction 1203 On-Flow LC-NMR 1203 Direct Stop-Flow 1204 Loop Collection 1206 Post-Column Solid Phase Extraction 1206 Cryogenic Probes for LC-NMR 1208 Improvements in the LC Peak Detection by Integrating Mass Spectroscopy into the LC-NMR Setup 1209 Conclusion and Outlook 1209 References 1210 LC-NMR in Dereplication and Structure Elucidation of Herbai Drugs 1211 Introduction 1211 Dereplication of Skullcap Herb 1212 Structure Elucidation of Aloe MetaboLites 1214 References 1217 Techniques 1219 New Approaches to NMR Data Acquisition, Assignment and Protein Structure Determination: Potential Impact in Drug Discovery 1221 Introduction 1221 Fast Multidimensional NMR Spectroscopy 1221 Speeding Up the Assignment Process 1223 Automated Protein Structure Determination 1225 Condusion 1227 References 1227 Transferred Cross-Correlated Relaxation: Application to Drug/Target Complexes 1229 Introduction 1229 Cross-Correlated Relaxation forthe Measurement of Projection Angles between Tensors 1229 Application to the Epothilone/Tubulin Complex 1234 Condusion 1235 References 1235 Novel Uses of Paramagnets to Solve Complex Protein Structures 1237 Introduction 1237 Methods to Bind Paramagnets to Non-Metalloproteins 1237 PCS Assignment and Ilse of PCSs and pmiRDCs as Structural Restraints 1239 New Approaches to Measurement of Small, ParamagneticaLly Induced RDCs 1240 Structural Applications of PCSs and pmiRDCs 1240 Condusion 1242 References 1242 Fast Assignments of 15N-HSQC Spectra of Proteins by Paramagnetic Labeling 1245 Introduction 1245 £186-8 Complex 1245 Paramagnetic Restraints Derived from 15N-HSQC Spectra of Paramagnetic and Diamagnetic E186-8 Complexes 1246 PLATYPUS Algorithm for Resonance Assignments from Paramagnetic Restraints 1247 Results Obtained with Selectively Labeled £186-8 Complexes 1248 Alternative Methods 1249 Outlook 1249 Acknowledgments 1250 References 1250 Phospholipid Bicelle Membrane Systems for Studying Drug Molecules 1253 Introduction 1253 Membrane Systems for NMR Studies 1254 Optimizing Isotropie Bicelles for Drug Conformational Studies 1255 Magnetkally Aligned Bicelles for Studying Drug Orientation 1257 Condusion 1258 References 1258 Partial Alignment for Structure Determination of Organic Molecules 1261 Introduction 1261 Residual Dipolar Couplings 1261 The Alignment Tensor 1261 Alignment Media 1262 RDC Measurement 1263 Applications 1265 Conclusion 1266 References 1266 Measurement of Residual Dipolar Couplings and Applications in Protein NMR 1269 Introduction 1269 Measurement of Backbone Residual Dipolar Couplings in Proteins 1270 AppLications of Residual Dipolar Couplings in Proteins 1271 Discussion 1272 Acknowledgments 1273 References 1273 Using Chemical Shift Perturbations to Validate and Refine the Docking of Novel IgE Antagonists to the High-Affinity IgE Receptor 1275 Hairpin Peptide Structure 1275 Zeta Peptide Structure 1275 Receptor Binding 1276 Conclusion 1280 References 1280 Dual-Region Hadamard-Encoding to Improve Resolution and Save Time 1281 References 1286 Nonuniform Sampling in Biomolecular NMR 1287 MaxEnt Reconstruction 1288 Nonuniform Sampling 1289 Example Applications 1289 Concluding Remarks 1293 Acknowledgments 1293 References 1293 Applications 1295 Structural Characterization of Antimicrobial Peptides by NMR Spectroscopy 1297 Introduction 1297 Solution Structures of Antimicrobial Peptides 1297 Solid-State NMR Experiments: Peptide Orientation in Bilayers 1302 Conclusions and Future Directions 1303 Acknowledgments 1303 References 1303 Pharmaceutical Applications of Ion Channel Blockers: Use of NMR to Determine the Structure of Scorpion Toxins 1307 Introduction 1307 Use of NMR to Determine the Structure of Rare Components 1307 NMR Structures of Toxins Active on Sodium Channels 1309 NMR Structures of Toxins Active on Potassium Channels 1309 Conclusion 1311 References 1311 Structure and Dynamics of Inhibitor and Metal Binding to Metallo-ß-Lactamases 1313 Introduction 1313 Effect of Inhibitor Binding on the ßackbone Amide Resonances 1314 Effect of Inhibitor Binding on the Imidazole Resonances of the Metal Ligands 1314 Direct Observation of the Active-Site Metals 1316 Effects of Thiomandelate Binding on the 113Cd Spectrum 1317 Conclusion 1318 References 1318 NMR Spectroscopy in the Analysis of Protein-Protein Interactions 1321 Introduction 1321 Tackling the Size Issue for Larger Protein Complexes 1321 Reducing Complexity: Differential Isotope Labeling 1322 Obtaining Long-Range Structural Information 1323 Mapping Protein-Protein Interfaces 1324 Protein-Protein Interactions and Chemical Exchange 1325 Stitching Up Proteins for Improved Stability 1326 Docking Protein Complexes 1326 Summary 1327 References 1327 Identification and Characterization of Ternary Complexes Using NMR Spectroscopy 1329 Introduction 1329 Borate Complexes and Their Study by NMR Spectroscopy 1329 Ternary Complexes Involving Organic Molecules 1332 ILOE Observations—Type II Dihydrofolate Reductase 1336 Summary 1338 References 1338 The Transferred NOE 1339 Affinities and Timescales 1339 The NOE 1340 Spin Diffusion 1341 The Transferred NOE 1341 Related Experiments 1344 References 1344 NMR Kinetic Measurements in DNA Folding and Drug Binding 1345 Drug-Quadruplex Interactions Studied by NMR 1345 Exchange Rates for Drug Binding to Quadruplex DNA 1345 DNA Hairpin Folding and Slow Exchange Equilibria 1346 Slow Exchange Between Two Conformers 1346 DNA Hairpin Folding Kinetics by Magnetization Transfer 1348 Acknowledgments 1348 References 1348 The Use of NMR in the Studies of Highly Flexible States of Proteins: Relation to Protein Function and Stability 1351 Introduction 1351 Insulin Flexibility and Activity 1352 The Acid State of Human Growth Hormone 1354 Acknowledgement 1357 References 1357 NMR-based Metabonomics Techniques and Applications 1359 Introduction 1359 Metabonomics Analytical Technologies 1359 Selected Applications of Metabonomics 1363 Conclusions 1366 References 1367 Protein Misfolding Disease: Overview of Liquid and Solid-State High Resolution NMR Studies 1369 Protein Misfolding Diseases 1369 Natively Unfolded Proteins Involved in Protein Misfolding Diseases 1369 Brief Background in NMR Parameters 1369 Proteins Involved in Misfolding Diseases Studied by NMR 1370 Amyloid Precursor Protein 1371 Prion Protein 1371 ot-Synudein 1371 Cu-Zn-Superoxide Dismutase 1372 Transthyretin 1372 References 1372 19F NMR Spectroscopy for Functional and Binding High-Throughput Screening 1375 FAXS 1375 3-FABS 1378 Conclusion 1380 References 1381 Applications of Receptor-Based NMR Screening in Drug Discovery 1383 Introduction 1383 Fragment-Based Screening: Identifying Hot Spots on Protein Surfaces 1383 Receptor-Based NMR Screening 1384 Utilization of Fragment Leads in Drug Design 1385 Core Replacement 1385 High-Throughput Core Elaboration 1386 Fragment Linking 1387 Receptor-Based Methods for Lead Validation and Characterization 1387 Summary 1388 References 1388 NMR SHAPES Screening 1391 Introduction 1391 Principles of SHAPES Screening 1391 Design of the SHAPES Compound Library 1391 NMR Methods for Screening Compound Libraries 1392 Implementation of SHAPES Screening 1394 Pre-HTS Screening 1394 Post-HTS Screening 1396 Lead Optimization 1396 Conclusion 1397 References 1398 NMR-Based Screening Applied to Drug Discovery Targets 1401 NMR for Lead Discovery 1401 NMR-Based Screening Techniques 1401 NMR-Based Screening Applied to Drug Targets 1405 Condusion 1407 References 1409 NMR and Structural Genomics in the Pharmaceutfcal Sdences 111 Introduction 1411 Strategies and Targets in Structural Genomics 1411 Advantages and Disadvantages of NMR for Structural Genomics 1411 Advances in NMR Instrumentation and Methodology 1415 Outlook and Conclusions 1416 References 1416 PART III Introduction 1417 References 1418 Acoustically Stimulated NMR Relaxometry: Application to the Study of Molecular Dynamics in Liquid Crystalline Materials 1419 Introduction 1419 Why Field-Cycling Experiments in Liquid Crystals? 1419 Relevant Properties of Liquid Crystals 1419 Order Director Fluctuations 1420 Seif Diffusion 1421 Molecular Reorientations 1421 Proton FC Relaxometry in Liquid Crystals 1421 Ultrasound Induced Relaxometry 1422 Outlook 1423 Acknowledgment 1424 References 1424 Characterization of Elastomers Based on Monitoring Ultraslow Dipolar CorreUtions by NMR 1425 Introduction 1425 Background of the Dipolar Correlation Effect 1426 The DCEin Elastomers 1427 Imaging on the Basis of the DCE 1431 Concluding Remarks 1432 References 1432 Correlating Molecular and Macroscopic Properties of Elastomers by NMR Relaxometry and Multi-pulse NMR Techniques 1435 Introduction 1435 Theoretical Background 1435 Relaxometry Experiments 1436 Double Quantum Experiments 1439 Summary 1440 Acknowledgments 1441 References 1441 Determining Structural and Dynamic Distribution Functions from Inhomogeneously Broadened NMR Spectra: The Conjugate Orthogonal Functions Approach 1443 Introduction 1443 Conjugate Orthogonal Functions 1443 Orientational Order 1445 Conclusions 1449 Acknowledgments 1449 References 1449 Fluid Diffusion in Partially Filled Nanoscopic and Microscopic Porous Materials 1451 Introduction 1451 The Two-Phase Exchange Model in NMR Diffusometry 1451 Experi mental 1454 Discussion and ConcLusions 1456 Acknowledg ments 1456 References 1457 Gas Adsorption on Carbon Nanotubes 1459 Introduction 1459 NMR Spectroscopy of CNTs 1459 ESR Spectroscopy of CNTs 1460 Gas Adsorption on MWNTs 1460 Gas Adsorption on SWNTs 1463 Summary 1463 Acknowledg ments 1464 References 1464 Magnetic Resonance Studies of the Heterogeneous Rotational and Translational dynamics in Disordered Materials 1467 Introduction 1467 Rotational Dynamics Near the Vitrification Transition 1468 Freezing in GLassy Crystals 1468 Heterogeneous Transport in Ionic Conductors 1469 Probing Secondary Relaxations 1470 Single-Molecule Spectroscopy 1471 Conclusion 1471 References 1471 Nuclear Magnetic Resonance in Ferromagnetic Multilayers and Nanocomposites: Investigations of Their Structural and Magnetic Properties 1473 Introduction 1473 NMR and Atomic Structure 1473 Local Magnetic Moments—Hyperfine Field and Magnetization Profiles 1474 Zero-Field NMR—Local Restoring Field and Magnetic Stiffness 1474 Magnetic Phase Separation 1476 In Field NMR—Local Magnetic Anisotropy 1477 Conclusions 1477 References 1478 1H Solid-State NMR of Supramolecular Systems 1479 Introduction 1479 High Resolution Solid-State NMR 1479 Applications to Supramolecular Structures 1482 References 1486 Quadrupolar NMR of Inorganic Materials: The Multiple-Quantum Magic Angle Spinning Experiment 1487 Introduction 1487 Multiple-Quantum MAS 1487 Pulse Sequencesfor MQMAS 1489 Spectral Analysis 1491 Application to Disordered and Amorphous SoLids 1492 Summary 1^94 Acknowledgments 1494 References 1494 Rheo-NMR Spectroscopy 1495 Introduction 1495 Experimental Aspects 1495 Nematic Liquid CrystaLs 1496 Hexagonal and Lamellar Lyomesophases 1498 Shear-Induced Phase Transitions 1500 Conclusions 1500 References 1500 Advances in Single-Sided NMR 1503 Introduction 1503 Material Characterization via Relaxometry by the NMR-MOUSE 1503 3D Imaging with a Single-Sided Sensor 1504 Flow Characterization with a Single-Sided Sensor 1505 Conclusions and Remarks 1506 References 1506 Site-specific Characterization of Structure and Dynamics of Complex Materials by EPRSpin Probes 1509 Introduction 1509 Addressing Specific Sites by Spin Probes and Spin Labels 1509 Oetecting Supramolecular Interactions by Changes in Probe Dynamics 1510 Characterization of Broad Distance Distributions 1510 Concatenated Macrocycles in Frozen Solution 1511 Polyelectrolytes: Probing Polyion-Counterion Interaction in Fluid and Frozen Solution 1514 References 1516 NMR of Organic Semiconductors 1519 Introduction 1519 Ligand Dynamics in ALq3 1520 Characterizing the Isomers of Alq3 1522 Variable Deposition Rate Studies 1523 Conclusions 1525 Acknowledgments 1525 References 1525 Solid State NMR of Xerogels 1527 Acknowledgments 1530 References 1530 Solid-State 17O NMR Spectroscopy of High-Pressure Silicates 1531 Introduction 1531 Oxygen NMR 1531 Sample Preparation 1532 MQMAS NMR of Upper Mantle Silicates 1532 STMAS NMR of Dense Silicate Phases 1536 NMR of Hydrous Magnesium Silicates: Humite Minerals 1536 Discussion and Conclusions 1539 Acknowledgments 1540 References 1540 The Structure of Oxide Glasses: Insights frotn 170 NMR 1543 References 1547 Studies of the Local Structure of Silk Using Solid-State NMR 1549 Introduction 1549 The NMR Measurements of Torsion Angles 1549 Geometrical Information on the Molecular-to-Nanometer Scale 1550 Conclusions 1554 Acknowledgments 1556 References 1557 Velocity Imaging of Granulär Materials 1561 Introduction 1561 NMR of Transport in Granulär Media—an Overview 1561 Gas-Fluidized Bed 1562 Rotating Drum 1565 Summary 1566 Acknowledgments 1567 References 1567 Glossary 1569 Introduction 1571 References 1571 High Resolution Solution State Methods 1573 Characterization of the Chemical Composition of Beverages by NMR Spectroscopy 1575 Introduction 1575 Alcoholic Beverages 1575 Nonalcoholic Beverages 1578 References 1580 High Resolution NMR of Carrageenans 1583 Carrageenan Structure 1583 Experimental Setup 1583 Analysis of the Major Carrageenan Types 1584 Analysis of Minor Components 1585 References 1587 Flavor-Food Compound Interactions by NMR Spectroscopy 1589 References 1593 High-Resolution Nuclear Magnetic Resonance Spectroscopy of Fruit Juices 1595 References 1598 High-Resolution NMR Spectroscopy in Human Metabolism and Metabonomics 1601 Introduction 1601 Water Suppression 1602 Assignments of the Metabolite Resonances 1603 Spectral Editing in Biologkai NMR Spectroscopy 1603 Other Useful Techniques 1604 NMR-Based Metabonomics Techniques 1605 Future Perspectives 1606 References 1606 High-Resolution NMR of Milk and Milk Proteins 1609 GeneraL Remarks 1609 NMRSpectra of Milk 1609 NMR Studies of Milk Proteins 1611 References 1613 High-Resolution 13C Nuclear Magnetic Resonance in the Study of Oils 1615 Introduction 1615 Quantitative Determination of the Oils Major Components 1615 Minor Oil Components 1619 13C NMR Spectroscopy As a Discriminating forthe Varietal, Geographical, and Botanical Origin of Vegetable Oils 1620 13C NMR of Olive OiL Minor Compounds to Oetermine Oil Authenticity 1620 References 1621 High-Resolution 1H Nuclear Magnetic Resonance in the Study of Oils 1623 Introduction 1623 Triglycerides 1623 Minor Compounds 1625 Use of :H NMR Spectroscopy to Characterize Olive Oil Geographical Origin 1627 References 1628 SNIF-NMR—Part 1: Prinriples 1629 Introduction 1629 Isotopic Abundances and Isotopic Ratios 1629 Isotopic Fractionation 1630 Quantitative Deuterium-NMR 1631 Referencing of Isotopic Parameters 1632 Carbon SNIF-NMR 1635 References 1636 SNIF-NMR—Part 2: Isotope Ratios as Tracers of Chemical and Biochemical Mechanistic Pathways 1637 Introduction 1637 Influence of Phase Transitions and Transport Phenomena on the Isotopic Parameters 1637 Simultaneous Determination of Site-Specific Thermodynamic Isotope Effects 1638 Determination of Kinetic Isotope Effects 1639 Sperific Connections Between SNIF Parameters of Reactants and Products 1640 Elaboration of SNIF-NMR Probes: From Carbohydrates to Ethanol and Glycerol 1642 Access to Mechanistic Information on Enantiotopic Hydrogen Sites 1643 References 1644 SNIF-NMR—Part 3: From Mechanistic Affiliation to Origin Inference 1647 Introduction 1647 SNIF Parameters as Witnesses of Individual Mechanistic Routes of Atoms 1647 Identification of Starting Materials: The Nature Laboratory 1651 Experimental Strategies for Origin Inference of Products 1651 Natural or Synthetic Origin of Products 1652 Characterization of Chemical Processes 1653 Identification of Plant Precursors 1654 Climatic Effects and Geographicat Origin 1655 References 1657 SNIF-NMR—Part 4: Applications in an Economic Context: The Example of Wines, Spirits, and Juices 1659 Introduction 1659 Current Regulations About Wines and Juices 1659 Ethanol: A Reliable Isotopic NMR Probe for Characterizing Wines, Spirits, and Juices in an Industrial Context 1660 Origin Authentication and Data Banks 1661 NMR Methodologies in an OfficiaL and Economic Context 1662 Determination of Illegal Enrichments 1662 Isotopic Characterization of Concentrated Juices 1663 Multi-component and Multi-isotope Strategies in the Detection of Adulterations 1663 Detection of Exogeneous Minor Components 1664 References 1664 High-ResoLution Nuclear Magnetic Resonance Spectroscopy of Wine, Beer, and Spirits 1667 References 1670 Relaxation Time Methods 1673 NMR Relaxation of Dairy Products 1675 Introduction 1675 Water Relaxation 1675 Water Retention 1676 Water Diffusion 1677 Fat Relaxation 1677 Conclusion 1678 References 1678 Characterization of Molecular Mobility in Carbohydrate Food Systems byNMR 1681 Introduction 1681 Water Molecular Mobility by NMR 1681 NMR to Determine Various Populations of Water 1682 T2 Distribution of Water in Starch 1683 Solid-State Nuclear Magnetic Resonance 1683 Solid Mobility by Cross Relaxation 1686 NMR Mobility and Microbial Activity 1687 Concluding Remarks 1688 References 1689 Diffusion and Relaxation in Gels 1691 Introduction 1691 Diffusion 1691 Relaxation 1693 References 1696 NMR Relaxation and Diffusion Studies of Horticultural Products 1699 Introduction 1699 NMR Relaxation and Water Compartmentation 1699 NMR Diffusometry and Water Compartmentation 1700 Fruit and Vegetable Quality 1701 Conclusions 1703 Acknowledgment 1703 References 1703 Proton NMR Relaxometry in Meat Science 1707 Introduction 1707 Determination of Fat Content in Meat and Meat Products Using NMR Relaxometry 1707 T2 Relaxation in Meat 1707 Water-Holding Capacity 1708 Relaxometry Studies During Conversion of Muscle to Meat 1708 Relaxometry Applied During Meat Processing 1710 Conclusions 1710 References 1710 Time-Domain NMR in Quality Control: More Advanced Methods 1713 Introduction 1713 Gradient Experiments 1713 Combined Relaxation Analysis in Foods with High Water Content 1714 Conclusion 1716 Acknowledgements 1716 References 1716 Time-Domain NMR in Quality Control: Standard Applications in Food 1717 Introduction 1717 Time-Domain NMR (TD-NMR) 1717 A. Determination of the SFC in Fat Compositions 1717 B. Simultaneous Oil and Moisture Determination in Food (Moisture Content Below Approx. 15%) 1720 C. Oil Content Determination in Pre-Dried Olives 1721 Conclusion 1721 Acknowledgment 1721 References 1721 Nuclear Magnetic Relaxation in Starch Systems 1723 Introduction 1723 General Considerations for NMR of Starch Systems 1724 Solid Starch Systems 1726 Proton Spin-Spin Relaxation and Second Moment of Solid Starch Polysaccharides 1726 Water in Starch Systems 1729 Future Perspective 1730 References 1730 High Resolution Solid State Methods 1733 Magic Angle Spinning NMR of Flours and Doughs 1735 Introduction 1735 CCross Polarization MAS NMR of Flours 1735 1H High Resolution MAS NMR of Flours 1735 1H and 13C MAS NMR of Doughs 1736 References 1741 High-Resolution Magic Angle Spinning NMR Spectroscopy of Fruits and Vegetables 1743 References 1746 High-Resolution Solid-State NMR of Gluten and Dough 1747 Introduction 1747 Gluten 1748 Flour and Dough 1750 References 1754 High-Resolution Solid-State NMR as an Analytical Tool to Study Plant Seeds 1755 Introduction 1755 Spectral Edition Inside the Seeds 1755 Assignments of the NMR Signals 1756 Solid-State Proton NMR 1757 Conclusion and Prospects 1757 References 1759 High-Resolution Solid-State NMR Spectroscopy of Starch Polysaccharides 1761 Introduction 1761 NMR Techniques 1763 Spectral Editing Techniques 1766 Future Perspectives 1767 References 1768 Imaging and Related Techniques 1771 NMR Imaging of Bread and Biscuit 1773 Introduction 1773 Monitoring the Baking Process 1773 Monitoring the Post-Chilling and Freezing Steps 1775 Assessing the Bread Crumb Structure 1776 References 1777 NMR Imaging of Oairy Products 1779 Introduction 1779 Waterand Fat Content and Distribution 1779 Macrostructure Information 1780 Temperature and Flow 1782 Conclusion 1783 References 1783 NMR Imaging of Dough 1785 Introduction 1785 Assessment of Ice Fraction Cartographies During Freezing, Storage, and Thawing of Raw Dough 1785 Assessment of Porosity During the Proving Process 1787 References 1789 MRI in Food Process Engineering 1791 Introduction 1791 Structure and Changes 1791 References 1794 Rheo-NMR: Applications to Food 1797 Introduction 1797 Applications of Rheo-NMR 1798 Relevance of NMR for Process Engineering 1800 References 18°1 Temperature Measurements by Magnetic Resonance 1803 Introduction 1803 7i and Tz Relaxation Times 1803 Diffusion Coefficient 1803 Chemical Shift 1804 Summary 1807 References 1807 Statistical Methods 1809 Chemometric Analysis of NMR Data 1811 Introduction 1811 Unsupervised Data Exploration by PCA 1814 Supervised Data Exploration 1814 Conclusion 1821 References 1821 Direct Exponential Curve Resolution by Slicing 1823 Tri-Linear Models 1825 Data Slicing 1825 NMR Relaxometry: An Example 1827 Conclusion 1828 References . 1830 ESR Methods 1831 ESR as a Technique for Food Irradiation Detection 1833 Introduction 1833 Definition of the Absorbed Dose (kGy) 1833 LabeLing 1833 Interactions of Radiation with Matter 1833 Food Irradiation Detection 1834 Conclusion 1837 References 1837 ESR Spectroscopy for the Study of Oxidative Processes in Food and Beverages 1839 Introduction 1839 ESR Detection of Radicals in Foods 1839 Spin Trapping 1840 Prediction of Oxidative Stability of Foods 1840 Other Uses of ESR for Studies of Food Oxidation 1842 Perspective and Future Developments 1842 References 1843 Applications to Food Systems 1845 Magnetic Resonance Studies of Food Freezing 1847 Introduction 1847 Spin Relaxometry 1847 PFGSE Diffusion Measurements 1851 Magnetic Resonance Imaging 1851 Liquid Phase Chemical Spectroscopy 1853 Solid-State NMR 1853 Conclusion 1854 References 1854 Nuclear Magnetic Resonance Studies on the Glass Transition and Crystallization in Low Moisture Sugars 1857 Introduction 1857 Line Width and Shape Studies 1857 Deuterium Line Shape Studies 1859 Relaxation Studies 1859 High-Resolution Solid-State 13C NMR 1862 CPMAS NMR and CrystalLization 1864 Other NMR Techniques As Monitors of the Glass Transition 1865 Imaging in the Study of Glasses 1866 References 1866 Probing the Sensory Properties of Food Materials with Nuclear Magnetic Resonance Spectroscopy and Imaging 1867 Introduction 1867 Texture 1868 Taste 1870 Summary and Future Applications 1871 References 1871 Single-Sided NMR in Foods 1873 Introduction 1873 The Bruker Single-Sided NMR Device 1873 Experimental Approaches in Fat and Water Determination 1873 Conclusion 1875 Acknowledgment 1875 References 1875 Applications of NMR in the Studies of Starch Systems 1877 Introduction 1877 NMR Studies of Starch Systems 1878 Conclusion 1883 References 1883 Index 1887 List of Tables Part 1: Applications in Chemistry, Biological and Marine Sciences Kinetics of Amyloid Fibril Formation of Human Calcitonin Table 1 Kinetic parameters for the fibril formation of hCTs in various pH solution 11 NMR Chemical Shift Map Table 1 Calculated 13C chemical shifts (ppm) of L-aLanine residue Ca- and Cp-carbons by the 4-31G-GIA0-CHF method 36 Table 2 Observed 13C chemical shifts of L-alanine residue Ca- and Cß-carbons for peptides including L-alanine residues in the solid state, as determined by 13C CP-MAS NMR, and their geometrical parameters 36 NMR Chemical Shifts Based on Band Theory Table 1 Observed and calculated 13C chemical shifts and shieldings of an isolated polyglycine chain 42 Table 2 Calculated 15N shieldings and band gaps for aromatic and quinoid polypyrrole modeis using INDO/S TB MO 44 Table 3 Total energies, band gaps, and NMR chemical shieldings for a Single chain of os- and tram-polyacetylenes and for a 30 crystal of eis- and trans-polyacetylenes as calculated by ob initio TB MO method within the framework of ST0-3G minimal basis set 46 Modeling NMR Chemical Shifts Table 1 Comparison of the calculated chemical shieldings using the KT1, KT2, and KT3 exchange-correlation functionals with those from other electronic strueture methods. The calculations were performed using the experimental geometries of the compounds. Data from references [46-49] in ppm, referenced to the bare nucleus (i.e. absolute shieldings) 51 Table 2 Parameters defining the linear correlation between calculated 1H chemical shieldings and measured chemicaL shifts in selected molecules from the G2 and G3 sets 53 Table 3 Parameters defining the linear correlation between calculated 13C chemical shieldings and measured chemical shifts in selected molecules from the G2 and G3 sets 54 Table 4 Parameters defining the linear correlation between calculated 15N chemical shieldings and measured chemical shifts in selected molecules from the G2 and G3 sets 55 Table 5 Parameters defining the linear correlation between calculated 15N chemical shieldings and measured chemical shifts in selected molecules from the G2 and G3 sets 56 Crystal Strueture Refinement Using Chemical Shifts Table 1 Energy contributions and chemical shift differences of the original and chemical shift refined cellulose Ia struetures 72 Industrial Application of In situ NMR Imaging Experiments to Steel-Making Process Table 1 The quantitative analysis of these chemical struetures between sample 1 and 3 after drying obtained by CRAMPS and MQMAS spectra 164 NMR Imaging: Monitoring of Sweüing of Environmental Sensitive Hydrogels Table 1 Water diffusion coefficientinside PVMEgelswith differentcross-linking densities (irradiation doses). A calibration of the signal (Figure 9) is necessary to calculate absolute values of D. This was done by means of measurements with pure water at different temperatures 188 Solid State NMR Characterization of Solid Surface of Heterogeneous Catalysts TabLe 1 13C MAS NMR isotopic chemical shift (in ppm) of carbonyl carbon of 2-13C-acetone on (or in) different solid (or liquid) acids 203 Solid State 19F-NMR Analysis of Oriented Biomembranes Table 1 CSA parameters of 19F-labeled amino acids used for structure analysis Two different sets of results are separated by a slash, namely of the polycrystalline amino acids (U. Dürr, PhD thesis, in preparation) and when they are incorporated into a lyophilized peptide 260 Site-Directed NMR Studies on Membrane Proteins Table 1 Conformation-dependent 13C chemical shifts of Ala residues (ppm from TMS) 288 3H NMR and Its Application Table 1 Important properties of tritium and its non-radioactive isotopes 392 On-line SEC-NMR Table 1 Effects of flow rate on the^ NMR signal of CHÜ3 in CDCl3 (5/95 v/v) measured at 750 MHz using an LONMR probe with a 60 ^ flow cell 396 Separated Detection of H-Transfer Motions in Multi-H-Bonded Systems Studied by Combined H NMR and 35Cl NQR Measurements Table 1 Theoretical values of quadrupole coupling constants (e2Qq), asymmetry parameters of electric field gradients (/j) and resonance frequencies (v) calcuLated for a neutral chloranilic acid molecule, and monovalent and divalent chloranilate ions in isolated states 429 EPR: Prinriples Table 1 Equations for the g matrix for the four possibLe cases using the d± and dxy basis functions for tz 438 Crystalline Structure of Ethylene Copolymers and Its Relation to the Comonomer Content Table 1 Specifications of EDAM and EMA copolymers 543 Two-Dimensional NMR Analysis of Stereoregularity of Polymers Table 1 Assignments of the methylene carbon resonances of methyl acrylate (A)/methyl methacrylate (B) copolymers from the HSQC spectrum 556 Table 2 1H-1H cross-correlations between non-equivalent geminal protons of methylene and between methine protons and methylene protons in methyl acrylate (A)/methyl methacrylate (B) copolymers observed from the TOCSY spectra 556 Table 3 Couplings of carbonyl carbon with cc-methyl protons («-CH3 and methylene protons observed from the 2D HMBC spectra 558 Polymer Microstructure: The Conformational Connection to NMR Table 1 Nonequivalent 13C NMR chemical shifts of the isopropyl methyl carbons in branched alkanes ... 565 Table 2 13C spin-lattice relaxation times, 7 i(s), for the crystalline carbons in s-PS polymorphs 569 H CRAMPS NMR of Polypeptides in the Solid State Table 1 H and 13C chemical shifts and characteristics of polypeptides and cyclic dipeptides 589 Table 2 1H and 13C chemical shifts, and conformational characteristics of silk fibroin and its model polypeptide sample 597 Table 3 JH chemical shifts and conformational characteristics of polypeptides 598 Quantum Information Processing as Studied by Molecule-Based Pulsed ENDOR Spectroscopy Table 1 ENDOR Systems regarding the satisfactions of the DiVincenzo criteria 645 Table 2 The spin Hamiltonian parameters of the malonyl radical 646 Table 3 The unitary Operation and corresponding pulse sequences for encoding 647 Table 4 Detection through angular dependence of the intensities of the electron spin echo 649 Refinement of Nucleic Acid Structures with Residual Dipolar Coupling Restraints in Cartesian Coordinate Space Table 1 Bond angles (degrees) involving hydrogen atoms in sugar-phosphate moieties 664 Two-Dimensional 17O Multiple-Quantum Magic-Angle Spinning NMR of Organic Solids Table 1 A summary of organic compounds studied by 170 MQMAS NMR 693 Rotational-Echo, Double-Resonance NMR Table 1 Phases of the xy-4 cycle and its supercycles 711 Table 2 Dipolar dephasing functions 713 Optimization of MRI Contrast for Pre-Clinical Studies at High Magnetic Field Table 1 Standard scan parameters 756 Table 2 T and Tz values for mouse and human tissue at different field strengths 757 The Application of In Vivo MRI and MRS in Phenomic Studies of Murine Models of Disease Table 1 In vivo MRI measurement of brain morphology 768 Application of MRS in Cancer in Pre-clinical Models Table 1 In vitro 1H NMR measurement of metabolites in wild-type (Hepa WT) and HIF-lß deficient (Hepa c4) tumor extracts (n = 4) 822 Experimental Cardiovascular MR in Small Animals Table 1 Relevant cardiac functional parameters 834 Comprehensive Compositional Analysis of Fish Feed by Time Domain NMR Table 1 StatisticaL analysis of the agreement between the NMR and the reference chemical methods ... 891 Table 2 Repeatability of the NMR measurements on a dry mixture sample 892 Water Distribution and Mobility in Fish Products in Relation to Quality TabLe 1 Application examples 907 Proton NMR of Fish Oils and Lipids Table 1 Assignment of the Signals of the 1H NMR spectra of anchovies lipids 910 Determination of Fatty Acid Composition and Oxidation in Fish Oils by High Resolution Nuclear Magnetic Resonance Spectroscopy Table 1 Fatty acid composition of depot fats from selected fishes 916 Resonance Spectroscopy to Study Lipid Oxidation in Fish and Fish Products Table 1 Relative intensity (ratio between the Signal amplitude and the reference sample (Manganese)) of spin adducts in cod liver oil added PBN as spin trap. The oil were pre-oxidised at 40 °C in 0, 1, 2, 3, and 4 weeks before addition of spin trap. Spectra were recorded after 0, 1, 2, 3, 4, 5, and 24, 48, 72, and 96 h of further oxidation at 40 C. Instrumental settings: sww 5mT, swT 2 min, Mod width 0.2 mT, cf 335.6 mT, timec ls (Jeol X-band). Unpublished data 928 Table 2 Chemical shift assignments of components in the !H NMR spectra associated with changes during lipid oxidation 929 Omega-3 Fatty Acid Content of Intact Muscle of Farmed Atlantic Salmon (Salmo salar) Examined by 1H MAS NMR Spectroscopy Table 1 Omega-3 fatty acid, DHA (C22:6 n-3) and cholesterol content (moL %) of white muscle of farmed AtLantic salmon examined by high-resolution 1H NMR spectroscopy 934 Table 2 Omega-3 fatty acid content (mol %) of white muscle of farmed Atlantic salmon measured on intact muscle and the lipid extracted from the corresponding muscle examined by 1H MAS NMR (200 MHz) and high-resolution :H NMR (500 MHz), respectively 934 HR MAS NMR Spectroscopy of Marine Microalgae, Part 1: CLassification and Metabolite Composition from HR MAS *H NMR Spectra and Multivariate Analysis Table 1 Tentative chemical shift assignment in 1H HR MAS spectra of whole cells of Thatassiosira pseudonana (Bacillariophyceae), referenced to TSP. Literature references: (1) Nicholson and Foxall; (2) Sitter et al. (2002); (3) Willker and Leibfritz (1998); (4) Lindon et ai; (5) Wardetal 939 HR MAS NMR Spectroscopy of Marine Microalgae, Part 2: 13C and 13C HR MAS NMR Analysis Used to Study Fatty Add Composition and Polysaccharide Structure Table 1 Assignments of fatty acid resonances from the 13C HR MAS NMR spectrum of C. miiUeri. Literature u^ed for the assignments 945 Table 2 Assignments of the carbohydrate resonances in the 13C NMR and HETCORR spectra 946 Table 3 Assignments of peaks in Figure 2 947 Post-mortem Studies of Fish Using Magnetic Resonance Imaging Table 1 Mean water and salt content in cod fillet pieces caLculated from the three MR slices images (see Fig. 3 and 4). The corresponding Variation ranges (minimal and maximal Contents) are given in the parentheses 954 Part 2: Applications in Medical and Pharmaceutical Sciences Acquiring Neurospectroscopy in Clinical Practice Table 1 Clinical protocoL decision matrix 981 Application of Magnetic Resonance for the Diagnosis of Infective Brain Lesions Table 1 Choline to creatine ratio determined by Integration of the resonances at 3.2 and 3.0 ppm, respectively. Ratios were determined for cystic GBMs, abscesses with growth of Streptococcus aureus and sterile abscesses 996 Application of 2D Magnetic Resonance Spectroscopy to the Study of Human Biopsies Table 1 Assignment of major cross peaks in 2D 1H-1H COSY MR spectra of thyroid biopsy tissue 1003 Correlation of Histopathology with Magnetic Resonance Spectroscopy of Human Biopsies Table 1 Resonances in one-dimensional JH MR spectra 1015 Table 2 Summary of classifiers and spectral regions using SCS 1016 High Resolution Magic Angle Spinning (HRMAS) Proton MRS of Surgical Spenmens Table 1 Matrix of selected brain metabolite concentrations measured with HRMAS MRS for differentiation between different pathological specimens NAA, in the table, includes both measured resonances of NAA at 2.01ppm and acetate at 1.92 ppm (see text for details); Numbers in parentheses represent resonance chemical shift in ppm. The resonance at 3.93 is tentatively assigned to the Cr metabolite. As an example of the use of this matrix, the Chol resonance can be used to differentiate low-grade/anaplastic astrocytomas from GBMs with a significance of / 0.05. Similarly, the glycine resonance (Gly) can be used to distinguish GBMs from Schwannomas with ap 0.005 1044 Intraoperative MRI Table 1 iMRI Systems with main advantage and disadvantage 1052 TabLe 2 Patient characteristics grouped by pathoLogical finding 1054 Table 3 Number and type of intraoperative MR imaging sequences 1055 In Vivo Magnetic Resonance Spectroscopy in Breast Cancer Table 1 Summary of experimental details used in various :H MRS studies 1066 In vivo 13C MRS Table 1 Equipment needed for 13C MRS beyond that required for Standard MR imaging 1086 Phosphorus Magnetic Resonance Spectroscopy on Biopsy and In Vivo Table 1 Summary of main metabolites detected by 31P MRS in vivo 1130 Table 2 Some measured concentrations of metabolites detected by 31P MRS in different human tissues (units of mM) 1133 Table 3A Published values of h relaxation times in different human tissues 1134 Table 3B Published values of Tz relaxation times in different human tissues 1135 Table 4 Relative merits of tissue extracts and in vivo 31P MRS measurements 1137 Table 5 A summary of the relative merits of STEAM, PRESS, and ISIS for singLe voxel acquisition of 31P MR spectroscopy data 1140 Table 6 Comparison of CSI and Single voxel techniques 1141 Table 7 Features of double resonance techniques 1141 Spatially Resolved Two-Dimensional MR Spectroscopy in vivo Table 1 Experimental parameters for 2D MRS 1164 Overview of NMR in the Pharmaceutical Sciences Table 1 NMR technologies used for structural characterization of receptors, ligands, and ligand-receptor complexes 1179 Table 2 NMR technologies used for high-throughput screening of ligand-receptor complexes 1181 Novel Uses of Paramagnets to Solve Complex Protein Structures Table 1 Magnitudes of pmiRDCs observed for various protein-metal complexes 1239 Measurement of Residual Di polar Couplings and Applications in Protein NMR Table 1 Modulation of the coupling Jmx evolution and 15N chemical shift frequency o n to the raw and manipulated FIDs in the 2D series for values of n from 1 to TDj/2 1271 Structural Characterization of Antimicrobial Peptides by NMR Spectroscopy Table 1 Examples of NMR derived high-resolution solution structures of antimicrobial peptides 1298 Protein Misfolding Disease: Overview of Liquid and Solid-State High Resolution NMR Studies Table 1 Overview of NMR parameters and their conformational dependence 1370 Applications of Receptor-Based NMR Screening in Drug Discovery Table 1 Published examples of receptor-based fragment approaches in the design of novel drug leads 1386 Table 2 Examples of receptor-based NMR methods for the validation of leads derived from HTS, affinity screening, and Virtual ligand screening campaigns 1388 NMR-Based Screening Applied to Drug Discovery Targets Table 1 NMR-based screening applied to drug discovery targets 1405 NMR and Structural Genomics in the Pharmaceutical Sciences Table 1 Summary of global structural genomics initiatives 1412 Part 3: Applications in Materials Science and Food Science Characterization of Elastomers Based on Monitoring Ultraslow Dipolar Correlations by NMR Table 1 Parameters of the Equations (11, 8) fitted to the experimental attenuation curves in dry and swollen samples of NR 1429 Fluid Diffusion in Partially Fitled Nanoscopic and Microscopic Porous Materials Tabte 1 The physical parameters of water and cyclohexane used in the fits of the theory to our experimental data 1455 Gas Adsorption on Carbon Nanotubes Table 1 Sample characteristics 1460 NMR of Organic Semiconductors Table 1 Rate constants determined by least- Squares fitting of the experimental H2 and H3 peak intensities. Error margins represent individual 95% confidence intervaLs 1522 Table 2 Activation parameters obtained from Eyring analysis of the rate constants given in Table 1 Standard errors of regression are indicated 1522 Solid-State 17O NMR Spectroscopy of High-Pressure Silicates Table 1 170 isotropic chemical shifts ( 5cs), quadrupolar products (Pq), quadrupolar coupling constants (Cq), asymmetries (?)), relative populations, and tentative assignments of the oxygen species a variety of silicate minerals 1534 High Resolution NMR of Carrageenans Table 1 Chemical shifts (ppm) of the a-anomeric protons of carrageenans referred to DSS as internal Standard at 0 ppma 1584 Table 2 13C NMR chemical shifts for the most common carrageenan structural unitsa 1586 Table 3 NMR chemical shifts for minor components and additives observed in carrageenan samples .... 1586 High-Resolution 13C Nuclear Magnetic Resonance in the Study of Oils Table 1 Quantitative 13C NMR determinations on oils 1616 High-Resolution 1H Nuclear Magnetic Resonance in the Study of Oils Table 1 Calculations of fatty arid composition of oils by signal intensities in the aH NMR spectrum .... 1624 Table 2 Chemical shift assignment of the selected resonances used for geographical origin discrimination of olive oils according to Ref. [31] 1628 SNIF-NMR—Part 2: Isotope Ratios as Tracers of Chemical and Biochemical Mechanistic Pathways Table 1 Site-specific unit fractionation factors, a, and thermodynamic isotope effects, ae, for liquid-vapor phase transition of methanol and ethanoL The 13C parameters are determined by isotope ratio mass spectrometry (IRMS) on the same distillate samples as those used in the hydrogen SNIF-NMR measurements 1638 Table 2 Isotopic redistribution coefficients, O/,, relating reactants (water, W, and sites 1-6 of glucose) and products (water, W, and sites I—methyl and II—methylene of ethanoL) in a fermentation reaction carried out with maize glucose and tap water [43]. The coefficients °I3/ °I4/ °B °m. 112/ Oii3/ °H5z and aus are close to zero and a small connection between site II of ethanol and site 4 of glucose is detected. Slightly different values have been measured in other series of experiments 1643 SNIF-NMR—Part 3: From Mechanistic Affiliation to Origin Inference Table 1 Site-specific hydrogen isotope ratios, (O/W), in ppm, of geraniol and ct-pinene 1648 SNIF-NMR—Part 4: Applications in an Economic Context: The Example of Wines, Spirits, and Juices TabLe 1 Conditions limiting the enrichment of musts in different regions A, B, and C. f% and c% are expressed in v/v of ethanol in wine and values into brackets correspond to red wines. For exampLe, zone A includes the 15 State Members but France, Greece, Portugal, and Spain, zone B is composed of the Northern and Central France, Austria, and the Baden region in Germany, and zones C include Southern France, Greece, Portugal, and Spain 1660 Table 2 Ranges of mean values exhibited by the isotopic ratios of ethanol samples obtained by fermenting different plant sugars, including grape, beet, and cane sugars. The carbon-13 deviation, S13C (%) (Part 1, Equation 5) has been measured by IRMS. (D/H)i (in ppm) is the isotope ratio of the methyl site of ethanol 1661 NMR Relaxation and Diffusion Studies of Horticultural Products Table 1 Comparison of theoretical and experimentalp, and o, in Equation (1) for apple parenchyma tissue 1701 Table 2 Summary of references to NMR studies of quality factors in the major types of fruit and vegetables 1702 Time-Domain NMR in Quality Control: Standard Applications in Food Table 1 Applications of TD-NMR for determination of moisture and oil 1720 Nuclear Magnetic Relaxation in Staren Systems Table 1 Proton relaxation data for D2O exchanged and saturated starch granules 1726 Magic Angle Spinning NMR of Flours and Doughs Table 1 Proton assignment of durum wheat flour lipid moieties (From ref. [6]) 1737 High-Resolution Solid-State NMR of Gluten and Dough Table 1 Resonances commonly resolved in proton MAS spectra of gluten, flour, and dough 1751 High-Resolution Solid-State NMR as an Analytical Tool to Study Plant Seeds Table 1 Assignment of 13C NMR SP/MAS spectrum of Pisum sativum 1758 Table 2 Assignment of 13C CP/MAS spectrum of Pisum sativum 1758 High-Resolution Solid-State NMR Spectroscopy of Starch Polysaccharides Table 1 Nuclear-spin interactions for 1H and 13C in a 9.4 T magnetic field 1763 Temperature Measurements by Magnetic Resonance Table 1 Sensitivity and aecuraey of the MRI parameters of water used to measure temperature in real and modelfood Systems (Taken from 2D slice images unless otherwise stated) 1804 ESR Spectroscopy for the Study of Oxidative Processes in Food and Beverages Table 1 ESR detection of radicals in dry foods 1841 Nuclear Magnetic Resonance Studies on the Glass Transition and Crystallization in Low Moisture Sugars Table 1 The frequency of perturbation associated with each experiment 1863 Table 2 Relaxation times for different carbons in the sucrose molecule, crystal (anhydrous) and glass (1-2% moisture), at ambient temperature (295-305 K). Anomeric data are for the F2 carbon of sucrose with no attached protons. The Gi anomeric carbon, having one attached proton, exhibits ring values. Typical or averaged values are shown where several carbons belong to one class. T{s in seconds, T p s in milliseconds, Tc-h in microseconds 1865
adam_txt	Contents List of Section Editors V Preface VII Foreword (Application in Chemistry) IX Listof Tables XLIX Color Plate Section LVII PARTI G lossary 1 Amyloids 5 Kinetics of Amyloid Fibril Formation of Human Calcitonin 7 Introduction 7 Properties of Fibril Formation of hCT 7 Conformational Changes of hCT 7 Kinetic Analysis of hCT Fibrillation 8 Mechanism of Fibril Formation 12 Conclusion 12 Acknowledgment 12 References 12 Polymorphism of Abheimer's Aß Amyloid Fibrils 15 Acknowledgments 20 References 20 Chemical Shifts and Spin-Couplings 25 13C, 15N, 1H, 2H, and 17O NMR Chemical Shift NMR for Hydrogen Bonds 27 Introduction 27 Hydrogen-bonded Structure and 13C Chemical Shift 27 Hydrogen-bonded Structure and 15N NMR Chemical Shift 28 Hydrogen-bonded Structure and lH NMR Chemical Shift 28 Hydrogen-bonded Structure and 170 NMR Quadrupolar Coupling Constant and Chemical Shift 29 Hydrogen-bonded Structure and 2H Quadrupolar Coupling Constant 30 Conclusion 31 References 31 NMR Chemical Shift Map 33 References 38 NMR Chemical Shifts Based on Band Theory 39 Introduction 39 Theoretical Aspects of Electronic State and Nuclear Shielding in Solid Polymers 39 Interpretation of Nuclear Shielding by the TB Method 41 References 47 Modeling NMR Chemical Shifts 49 Introduction 49 Theory of the Chemical Shieldings 50 Modeling Chemical Shieldings 50 Acknowledgments 57 References 57 Ab Jnitio Calculation of NMR Shielding Constants 59 Introduction 59 Overview of the Theoretical Background 59 Ablnitio Program Packages Capable of Calculating NMR ChemicaL Shielding Tensors 62 Ab Initio Calculation of NMR Chemical Shielding Tensors for Large Molecules 63 References 65 Crystal Structure Refinement Using Chemical Shifts 67 Introduction 67 ComputationaL Methods 67 Applications in Crystal Structure Refinement 70 References 73 The Theory of Nuclear Spin-Spin Couplings 75 Introduction 75 Origin of the Indirect Nuclear Spin-Spin Coupling Interaction 75 Coupled Hartree-Fock Approximation 77 Triplet Instability of Coupled Hartree-Fock Calculation 78 Electron Correlation Effects 78 References 79 Fibrous Proteins 81 Investigation of Collagen Dynamics by Solid-State NMR Spectroscopy 83 Introduction 83 Investigation of Collagen Dynamics by Static Solid-State NMR 83 Application of CP MAS Methods to Study the Molecular Properties of Collagen 85 What Has Been Learned from Solid-State NMR Studies of Collagen? 87 Acknowledgments 88 References 88 Solid-State NMR Studies of Elastin and Elastin Peptides 89 Introduction 89 Studies of Native Elastin Focus Mainly on the Natural-Abundance 13C PopuLations 90 A New Approach for Production of Isotopically Labeled Elastin Utilizes a Mammalian Cell Culture 92 Information on the Hydrophobie Domain of Elastin is Gleaned from Repeating Polypeptides 93 Concluding Remarks 94 Acknowledgments 94 References 94 Structural Analysis of Silk Fibroins using NMR 97 Introduction 97 Structure of B. mori Silk Fibroin Before Spinning (Silk I) 97 Structure of B. mori Silk Fibroin After Spinning (Silk II) 98 Structure of Nephilo davipes Dragline Silk (MaSpl) 100 References 102 Field Gradient NMR 103 NMR Diffusometry 105 Diffusion as a Probe 105 Gradient-Based Diffusion Measurements 105 Experimental Complications 106 Diffusion in Complex Systems 108 Acknowledgment HO References HO Field Gradient NMR of Liquid Crystals 113 Introduction 113 NMR Methods and Diffusion in LCs 113 Lyotropic Applications 115 Thermotropic Applications 116 Other Applications of Field Gradients 117 References 117 Field Gradient NMR for Polymer Systems with Cavities 119 Introduction 119 Diffusion in Polymer Gel Systems 119 Conclusion Remarks 123 References 123 NMR Measurements Using Field Gradients and Spatial Information 125 Introduction 125 Diffusion Coefficient Measurements 125 NMR Imaging 127 Selection of Coherence 128 References 130 Theory and Apptication of NMR Diffusion Studies 131 Theoretical Aspects 131 AppLications of Diffusion NMR 132 References 139 Host-Guest Chemistry 141 Solid-State NMR in Host-Guest Chemistry 143 Introduction 143 The Solid-State Spectrum 143 General Characterization 144 Structural Information from Spin Vz Nuclei 144 Distance Measurements 146 Spin Counting 146 Probing Pore Spaces 146 MRI 147 Dynamics 147 References 148 Imaging 151 Mapping of Flow and Acceleration with NMR Microscopy Techniques 153 Introduction 153 Encoding Principles and Pulse Sequences 153 Experiments 156 Conduding Remarks 157 References 158 Industrial Application of In situ NMR Imaging Experiments to Steel-Making Process 159 References 166 Biomedkal NMR Spectroscopy and Imaging 169 Introduction 169 Tracking of Metabolites: In Vivo 13C NMR Images with H-l Detection 169 Physiological Properties: pH 170 Temperature Image and Navigation Surgery Under MRI Guidance 171 Cellular Tracking 172 Concluding Remarks 174 References 174 Electron Spin Resonance Imaging in Polymer Research 175 Introduction 175 ESR Spectra in the Presence of Field Gradients 175 Spatially-Resolved Degradation from ESRI Experiments 177 Acknowledgments 179 References 180 NMR Imaging: Monitoring of Swelling of Environmental Sensitive Hydrogels 183 Hydrogels 183 Swelling Process 183 Advantages of NMR Imaging and Application on Network Characterization 183 Experimental 184 Volume Phase Transition, Net Chain Mobility, and T-Stimulus 186 Diffusion of Low Molecular Weight Compounds 186 Distribution of Water Inside the Gel 187 Diffusion Coefficients Inside the Gel—Structure of Non-homogeneous Networks 187 Acknowledgment 189 References 189 Inorganic Materials and Catalysis 191 Exploiting JH- 29Si Cross-Polarization Features for Structural Characterization of Inorganic Materials 193 Introduction 193 1H- 29 Si CP Dynamics: Basic Features and Pitfalls 193 Silica Gels 195 Layered Sodium Hydrous Silicates 196 Probing the Geometry of Strongly Hydrogen-Bonded Silanols 197 Conclusions 199 References 199 Solid State NMR Characterization of Solid Surface of Heterogeneous Catalysts 201 Surface Acidity of Heterogeneous Catalysts 201 Catalytic Reaction on the Surface of Heterogeneous Catalysts 203 References 207 Isotope Labeling 209 Recent Developments in Stable-Isotope-Aided Methods for Protein NMR Spertroscopy 211 Introduction 211 Positive Labeling (Use of 13C and 15N) 211 Negative Labeling (Use of2H) 214 Concluding Remarks 217 Acknowledgment 217 References 217 Structural Glycobiology by Stable-isotope-assisted NMR Spertroscopy 219 Introduction 219 Three-Dimensional HPLC Mapping 219 Stable Isotope Labeling of Glycoproteins 219 Carbohydrate-Protein Interactions 223 Concluding Remarks 223 Acknowledgments 223 References 224 Lipid Bilayer and Bicelle 227 Development and Application of Bicelles for Use in Biological NMR and Other Biopriysical Studies 229 Bicelle Roots 229 Early 1990s 230 Late 1990s 231 2000-2005 231 Conclusion: How Good are Bicelles as Model Membranes? 232 Acknowledgment 233 References 233 Nuclear Magnetic Resonance of Oriented Bilayer Systems 237 Introduction 237 Magnetically Oriented Bilayer Systems 237 Mechanically Oriented Bilayer Systems 239 Orientation Dependence of Chemical Shift Interaction 240 Orientation Dependence of Di polar Interaction 241 Structure Determination of Membrane Associated Peptides in the Magnetically Oriented Systems 242 Conclusions 242 References 243 Solid-State Deuterium NMR Spectroscopy of Membranes 245 Equilibrium and Dynamical Properties of Membrane Lipids are Studied by Solid-State Deuterium NMR 245 Deuterium NMR Spectroscopy Allows Direct Observation of Coupling Tensors Related to Molecular Structure and Dynamics 246 Molecular Structures and Motions are Revealed by Deuterium NMR Lineshapes 247 Deuterium NMR Provides Order Parameters Related to Average Membrane Properties 248 Deuterium Spin-Lattice Relaxation Times Reveal Dynamical Properties of Lipid Membranes 250 Model-Free Analysis Suggests that Collective Membrane Motions Govern the Relaxation 251 Spectral Densities and Correlation Functions are Derived for Simplified Models in Closed Form 252 Deuterium NMR Relaxation Allows Detailed Comparison of the Structural and Dynamical Properties of Membranes 254 Acknowledgments 255 References 255 Solid State 19F-NMR Analysis of Oriented Biomembranes 257 Introduction 257 19F-NMRExperimentalAspects 257 Strategies for Structure Analysis 257 19F-Labelingof Peptides 259 Structure Analysis of Membrane-Associated Peptides 259 Fusogenic Peptide B18 260 Antimicrobial Peptide Gramicidin S 261 Antimicrobial Peptide PGLa 261 Antimicrobial Peptide K3 262 Perspectives 262 Acknowledgments 262 References 262 Membrane-Assoriated Peptides 265 Solid-State NMR Studies of the Interactions and Strurture of Antimicrobial Peptides in Model Membranes 267 Introduction 267 Effects of Antimicrobial Peptides on Model Lipid Membranes 267 Study of Antimicrobial Peptides in Membranes 269 Conclusions 273 References 273 Anisotropie Chemical Shift Perturbation Induced by Ions in Conducting Channels 275 Acknowledgments 279 References 279 NMR Studies of Ion-Transporting Biological Channels 281 References 283 Membrane Proteins 285 Site-Directed NMR Sitidies on Membrane Proteins 287 Introduction 287 Conformation-Dependent 13C Chemical Shifts 287 Site-Directed Assignment of 13C NMR Signals 288 Dynamic Aspect of Membrane Proteins 289 Surface Structures 290 Site-Directed 13C NMR on Membrane Proteins Present as Monomers 290 Concluding Remarks 292 References 292 Strurture of Membrane-Binding Proteins Revealed by Solid-State NMR 295 Dynamic Structure of the Membrane-Binding Proteins at the Membrane Surface 296 Application of the Solid-State NMR on the PLC-61 PH Domain 296 References 299 Solid-State NMR of Membrane-Active Proteins and Peptides 301 Chemical Shift Anisotropy (CSA) 302 Quadrupolar Coupling 304 31Pand2HNMRof Lipids 305 Dipolar (Re)-Coupling 305 Conclusion 306 References 306 Magnetic Resonance Spectroscopic Studies of the Integral Membrane Protein Phospholamban 309 Phospholamban 309 Solid-State NMR Spectroscopic Studies of PLB 310 Magnetic Resonance Spectroscopic Studies of the AFA-PLB Monomer 312 Acknowledgments 313 References 313 NMR Studies of the Interactions Between Ligands and Membrane-Embedded Receptors: New Methods for Drug Discovery 315 Introduction 315 Choice of Technique 315 Solution NMR Methods .'.'.!!. 316 Solid-State NMR Methods 317 A Case Study: Solid-State NMR Investigations of Ion Pump Inhibitors 320 Future Prospects 321 References 322 Photosynthetic Antennae and Reaction Centers 323 Introduction 323 Structure-Function Studies of Antenna Systems and RCs 323 MAS NMR Structure Determination: Chlorosomes and LH2 326 References 329 Insight into Membrane Protein Structure from High-Resolution NMR 331 Introduction 331 Membrane Protein Structure—Current Status 331 Peptides frorn Helices and Turns have Intrinsic Structures that can Provide Secondary Structure Information About the Parent Soluble Protein 331 Structures of Peptide Fragments from Membrane Proteins can Provide Secondary Structure Information 332 Protein Fragments of Other Membrane Proteins 334 General Features of the Studies on Membrane Protein Fragments 335 How Sparse Long-Distance Experimental Constraints can be Combined with Fragment Structures to Build a Structure of the Intact Membrane Protein 336 New High-Resolution NMRStudies on Intact Membrane Proteins 337 References 337 New Developments 341 Fast Multidimensional NMR: New Ways to Explore Evolution Space 343 The Filter DiagonaLization Method 343 Spatially Encoded Single-Scan NMR 345 Fiadamard Encoding 345 Projection-Reconstruction 347 Acknowledgments 348 References 348 High-Sensitivity NMR Probe Systems 349 Sensitivity Issues in NMR Spectroscopy 349 Thermodynamics 350 Polarization Transfer 350 Optimized Detection Coil Design 353 Magnetic Resonance Force Microscopy 354 References 357 CRAMPS 359 Introduction 359 Theory 359 Experimental 363 Applications 365 Acknowledgments 366 References 366 Mobile NMR 369 Introduction 369 Measurement Methods 369 Applications 372 Summa ry 375 Acknowledgments 375 References 376 Rheo-NMR 379 Suggested Reading 383 Analytical Aspects of Solid-State NMR Spectroscopy 385 Introduction 385 Uses of Isotropie Shielding to Identify MateriaLs 385 Uses of Shielding Tensors to Identify Materials 386 Using Quadrupolar Coupling to Identify Materials 387 Structure Determination 388 Quantification with Solid-State NMR Spectroscopy 388 Summary 389 Acknowledgment 389 References 389 3H NMR and Its Application 391 Introduction 391 Radiochemical Facilities and Radiation Safety 391 Tritiation Procedures 391 Tritium NMR Spectroscopy 392 Applications 393 Conclusions 394 References 394 On-line SEC-NMR 395 On-line Coupling of LC and NMR 395 On-line SEC-NMR 395 Molecular Weight Determination of Polymers 396 LCCAP-NMR 400 References 401 NOE and Chemical Exchange 403 The Nuclear Overhauser Effect 405 Introduction 405 Theoretical Background 405 Applications of the NOE 407 References 408 Solute-Solvent Interactions Examined by the Nuclear Overhauser Effect 409 Background 409 Intramolecular NOEs 409 Intermolecular NOEs 410 Magnitudes of Intramolecular and Intermolecular NOEs 410 Solute-Solvent Interactions 410 Experimental Detection of Intermolecular Cross-Relaxation 412 Xenon-Solvent Interactions 412 Small Molecule-Water Interactions 412 Micelle-Water Interactions 412 Small Molecule-Organic Solvent Interactions 413 Selective Solute Interactions in Mixed Solvent Systems 413 Biomolecule-Water Interactions 414 Summary 415 References 416 Chemical Exchange 417 Introduction 417 Types of Chemical Exchange 417 Theory 419 Kinetics 419 Experimental Precautions 420 Intermediate Exchange 420 Slow Exchange 421 Fast Exchange 422 Summary 422 References 422 NQR ESR 425 Separated Detection of H-Transfer Motions in Multi-H-Bonded Systems Studied by Combined H NMR and 35Cl NQR Measurements 427 Introduction 427 High Sensitivity of NQR Shown in 4-Chlorobenzoic Add 427 Separated Detections of H-Transfer Modes in Multi-H-Bonded Systems 428 Conclusion 432 References 434 EPR: Principles 435 Angular Momentum 435 Spin-Orbit Interaction 435 Zeeman Interaction 435 Spin Hamiltonian 436 S = y2 Systems 436 NO" Molecule 437 5 % Systems «9 References 440 Zero Field NMR: NMR and NQR in Zero Magnetic Field 441 An Historical Perspective: Field-Cyding NMR 441 Sensitivity Enhancement of Low-y Nuclear Quadrupole Resonance 442 Zero Field NMR: Experimental Details 442 Extensions of Zero Field NMR and NQR 446 Zero Field NMR and NQR: Limitations and Prospects? 446 References 447 Organo Metallic Chemistry 449 Organoboron Chemistry 451 References 453 Organogermanium Chemistry 455 References 455 Organotin Chemistry 457 References 459 ! Paramagnetic Effects 461 aH and 13C High-Resolution Solid-State NMR of Paramagnetic Compounds Under Very Fast Magic Angle Spinning 463 Introduction 463 One-Dimensional (1D) aH SSNMR for Paramagnetic Systems 463 1D 13C VFMAS SSNMR for Paramagnetic Systems 465 Signal Assignments and Multi-dimensional NMR 468 Experimental Aspects 469 Conclusion 469 Acknowledgments 469 References 469 Paramagnetic Effects of Dioxygen in Solution NMR—Studies of Membrane Immersion Depth, Protein Topology, and Protein Interactions 471 Introduction 471 Spin-Lattice Relaxation 471 Chemical Shift Perturbations 472 Immersion Depth 472 Membrane Protein Topology 474 Protein-Protein Interactions 477 Additional Applications: Family Fold Recognition and O2 Migration Pathways 478 Final Comments 478 References 478 Protein Structure 481 TROSY NMR for Studies of Large BiologicaL Macromolecules in Solution 483 Introduction 483 Technical ßackground 483 TROSY Applications for Studies of Large ßiological Macromolecules 486 Cross-Correlated Relaxation-Induced Polarization Transfer for Studies of Very Large Structures 490 Conclusion and Outlook 490 Acknowledgments 491 References 491 NMR Insight of Structural Stability and Folding of Calcium-Binding Lysozyme 493 Lysozyme and Calcium Binding of the Homologous Proteins 493 Protein Folding Mechanism 493 1H Chemical Shift Calculation of the Calcium-Binding LYS in the Structural Intermediate 494 H/D Exchange of Calcium-Binding LYS in the Native and the Structural Intermediate 495 References 497 NMR Investigation of Calmodulin 499 Biological Functions 499 Two-Dimensiona^H NMR 500 Multidimensional and Heteronuclear NMR of CaM 501 Solution Structure of CaM 501 Metal and CaM Interactions 501 Calcium-Calmodulin-Peptide Complexes 504 Acknowledgment 509 References 509 Analytical Framework for Protein Structure Determination by Solid-State NMR of Aligned Samples 513 Introduction 513 A Spherical-Basis Treatment of Experimental Angular Constraints for Protein Structure Determination 515 Examples of Structural Fitting 517 Conclusions 521 Acknowledgements 521 References 521 Determining Protein 3D Structure by Magic Angle Spinning NMR 523 Introduction 523 SampLe Preparation and Methodology 523 Applications 524 Conclusions 525 Acknowledg ments 525 References 525 19F NMR Study of 6-Type Haemoproteins 527 Introduction 527 19F Labeling of 6-Type Haemoproteins Using Reconstitution 528 19F NMR vs. rH NMR 529 Haem Disorder 533 MbO2 vs. MbCO 533 Summary 533 References 533 Polymer Structure 535 NMR in Dry or Swollen Temporary or Permanent Networks 537 Introduction 537 Polymeric Dynamics 537 Effect of Local Friction and Spin-Lattice Relaxation 537 Chain Diffusion 538 Statistical Polymeric Structures and Spin-Spin Relaxation 538 ConcLusion 539 References 539 Crystalline Structure of Ethylene Copolymers and Its Relation to the Comonomer Content 541 Polymorphism of Ethylene Copolymers 541 The Biexponential 13C h Relaxation Behavior of the Crystalline Region 542 References 545 Isomorphism in Bacterially Synthesized Biodegradable Copolyesters 547 Introduction 547 Isomorphous Behavior of Bacterially Synthesized Copolyesters 547 Cocrystallization and Phase Segregation in P(3HB)/P(3HB-co-3HV) Blends 549 References ^ 51 Two-Dimensional NMR Analysis of Stereoregularity of Polymers 553 Poly(Methyl Methacrylate) 553 Methyl Acrylate (A)/Methyl Methacrylate (B) Copolymer 554 References 558 Quantitative Analysis of Conformations in Disordered Polymers by Solid-State Multiple-Quantum NMR 559 Introduction 559 Characterization of Conformations in Atactic Polymers by Two-Dimensional Experiments 559 Selective Observation of Respective Conformers in Polymers by Zero-Quantum (ZQ) Experiments 560 References 562 Polymer Microstructure: The Conformational Connection to NMR 563 Introduction 563 13C NMR Spectral Assignments 563 •y-Gauche-Effect 564 Example of the -y-Gauche-Effect 565 PP Stereosequences From 13C NMR 566 13C NMR of Solid Polymers 566 Application of Solid-State 13C NMR to Polymers 568 Summary 569 References 570 Solid-State NMR Characterization of Polymer Interfaces 571 Overview 571 Solid-State Proton NMRStudies 571 Solid-State Heteronuclear NMRStudies 574 Dynamics at the Interface 575 Outlook and Conclusions 577 References 577 The Structure of Polymer Networks 579 Introduction 579 The Chemical Structure of Polymer Networks 579 The Physical Structure of Polymer Networks 582 Summary 584 References 584 H CRAMPS NMR of Polypeptides in the Solid State 587 Introduction 587 Experimental Evidence 587 References 599 Polymer Dynamics 601 Dynamics of Amorphous Polymers 603 Introduction 603 Spin Relaxation 603 One-Dimensional MAS Spectra 604 Lineshape Analyses 605 20 Exchange Spectra 607 References 608 Molecular Motions of Crystalline Polymers by Solid-State MAS NMR 611 Overview 611 1D-MAS Exchange NMR 611 Mechanical Property vs. Chain Dynamics 611 Crystal Transformation vs. Molecular Dynamics 612 Concluding Remarks 614 References 614 Dynamics in Polypeptides by Solid State 2H NMR 617 Introduction 617 Methyl Group 617 Phenyl Ring 618 Side Chain of Poly(-y-benzyl L-glutamate) (PBLG) 619 Main Chain Dynamics 622 Acknowledgments 623 References 623 Polymer Blends 625 Polymer Blends 627 Overview 627 Interaction in Polymer Blends 627 Miscibility 628 Phase Separation Process 630 Conclusion Remarks 631 References 631 Configurational Entropy and Polymer Miscibility: New Experimental Insights From Solid-State NMR 633 Introduction 633 Experimental NMR Methods 634 Choice of PoLymer Blend System 635 129Xe NMR of Absorbed Xenon Gas 635 Two-Dimensional Exchange NMR to Probe Slow-Chain Reorientation 636 2H NMR Data and Simulations 638 Conclusions 640 References 640 Quantum Information Processing 641 Quantum Information Processing as Studied by Molecule-Based Pulsed ENDOR Spectroscopy 643 Introduction 643 Pseudo-Pure States and Quantum Entanglements 643 Molecular ENDOR Based Quantum Computer 644 Preparation of the Molecular Entity for QC-ENDOR 646 Implementation of SDC by Pulsed ENDOR 647 Conclusion * 49 References 650 Residual Dipolar Couplings and Nucleic Acids 651 New Applications for Residual Dipolar Couplings: Extending the Range of NMR in Structural Biology 653 Background 653 Theory 653 Protein Structures 654 DNA/RNA 654 Pseudocontact Shifts 656 Unfolded Denatured Proteins 657 Oügosaccharides and SmallOrganic Molecules 657 Conclusions 658 References 658 Refinement of Nucleic Acid Structures with Residual Dipolar Coupling Restraints in Cartesian Coordinate Space 661 Introduction 661 Loop ß RNA from Domain IV of the Enterovirus Internat Ribosome Entry Site 662 Structural Restraints 662 Structure Refinement 663 References 665 Conformational Analysis of DNA and RNA 667 Introduction 667 Conformation of Nucleotides 667 NMR Signal for DNA and RNA and Their Assignment 667 Structural Analysis 669 References 671 Solid-State NMR Technique 673 Analytical and Numerical Tools for Experiment Design in Solid-State NMR Spectroscopy 675 Introduction 675 Tools for Systematic Experiment Design 675 Systematic Design of Solid-State NMR Experiments 679 Conclusions 682 Acknowledgements 682 References 682 Homonuclear Shift-Correlation Experiment in Solids 685 References 689 Two-Dimensional 170 Multiple-Quantum Magic-Angle Spinning NMR of Organic Solids 691 Introduction 691 Pulse Sequence, Data Processing, and Spectral Analysis 691 Sensitivity of 170 MQMAS Experiments 694 Conclusion 694 Acknowledgment 696 References 696 A Family of PISEMA Experiments for Structural Studies of Biological Solids 699 An Ideal SLF Sequence 699 Offset Effects 699 Offset Compensation by BB-SEMA 700 SEMA Requires Very High RF Power 702 TANSEMAfor Low RF Power Experiments 703 PISEMA of SIn 703 Summary 704 Acknowledgments 704 References 704 Structural Constraints in Solids 707 Rotational-Echo, Double-Resonance NMR 709 Introduction 709 Dipolar Recoupling 709 Practical Details 710 References 714 REDOR in Multiple Spin System 715 Introduction 715 Dipolar Dephasing of REDOR in I-S„ Multiple Spin System 715 Obtaining Accurate Internuclear Distances by REDOR 717 DipoLar Dephasing of REDOR in Multiple Spin System 719 Conclusions 720 References 720 Torsion Angle Determination by Solid-State NMR 723 Static Tensor Correlation Techniques 723 MAS Tensor Correlation Techniques 723 Distance Methods for Determining Torsion Angles 728 Conclusion 728 References 728 Secondary Structure Analysis of Proteins from Angle-Dependent Interactions 731 Introduction 731 NMR Methods for the Secondary Structure Analysis of Proteins 731 Torsion Angle Measurements from the Mutual Orientation of Anisotropie Interactions for the Secondary Structure Analysis 734 References 735 Telomeric DNA Complexes 737 Comparison of DNA-Binding Activities Between hTRF2 and hTRFl with hTRF2 Mutants 739 Introduction 739 Results 739 Acknowledgments 745 References 747 Glossary 749 Optimization of MRI Contrast for Pre-Clinical Studies at High Magnetic Field 753 Introduction 753 Physics Background for Contrast Optimization 753 MR Contrast Agents for Animal Imaging Studies 758 Conclusion 761 Acknowledgement 761 References 761 The Application of In Vivo MRI and MRS in Phenomic Studies of Murine Models of Disease 763 Introduction 763 Magnetic Resonance Imaging 763 Magnetic Resonance Spectroscopy 770 Conclusions 776 Acknowledgement 776 References 776 Experimental Models of Brain Disease: MRI Contrast Mechanisms for the Assessment of Pathophysiological Status 781 Introduction 781 Image Contrast and Intrinsic MR Parameters 781 Taking Advantage of MR Sensitivity to Dynamic Physiological Processes 783 Using Exogenous Contrast Agents to Enhance Image Contrast 784 Manipulating the MR Signal to Measure Physiological Parameters 786 Conclusions 791 Acknowledgments 792 References 79Z Experimental Models of Brain Disease: MRI Studies 795 Introduction 795 Practical Issues 795 CerebraL Ischemia 797 Spreading Depression 800 Epilepsy 80l Neurodegenerative Disorders 803 CNS Inflammation 804 Traumatic Brain Injury 806 Conclusion 808 Acknowledgments 808 References 808 Application of MRS in Cancer in Pre-clinical Models 817 Introduction 817 Tumor BioLogy and Physiology 817 Condusion 824 Acknowledgement 824 References 824 Experimental Cardiovascular MRin Small Animals 829 Introduction 829 Methods and Requirements 829 Global Cardiac Function 833 Myocardial Tissue Contractility 836 Multinuclear MR Spectroscopy 839 VascularMRI 842 Conclusion and Future Perspective 843 Acknowledgements 843 References 844 Application of Pharmacological MRI to Preclinical Drug Discovery and Development 849 Introduction 849 Surrogate Markers of Neuronal Activity 849 Image Acquisition Strategies for Preclinical phMRI 852 Effects of Anesthesia 854 Data Analysis 856 Using Dopamine Receptor Agonists as Prototypical Agents for Animal phMRI 859 The Future of phMRI 867 References 868 Application of MRI to Cell Tracking 873 Introduction 873 Intracellular MRI Contrast Agents 873 Properties of a Good Contrast Agent for CelL Tracking 874 MRI Contrast Agent for Cell Tracking 874 Paramagnetic Agents 874 Superparamagnetic Agents 874 Engineering Delivery Systems for Iran Oxide Contrast Agents 875 Delivery of Contrast Agent with Transfection Agents 875 Delivery of Contrast Agent Using Specifk Targeting 875 Cytotoxicity and Metabolism 877 Conjugation Chemistry: Attaching Contrast Agent to Delivery Ligand 877 MRI Tracking of Stem Cells in the Heart 879 MRI Tracking of Stern CeLLs in the CNS 880 MRI Tracking of Cell-Based Tumor Therapy 882 Acknowledgment 882 References 883 Glossary 885 Introduction 886 Comprehensive Compositional Analysis of Fish Feed by Time Domain NMR 887 Introduction 887 Experimental 887 Results and Discussion 890 Conclusions 892 AcknowLedgments 893 References 893 Low Field NMR Studies of Atlantic Satmon (Salmo salar) 895 Introduction 895 Materials and Methods 896 ResuLts and Oiscussion 899 Conclusion 902 References 902 Water Distribution and Mobility in Fish Products in Relation to Quality 905 Introduction 905 Algorithms 905 Applications 906 References 908 Proton NMR of Fish Oils and Lipids 909 Introduction 909 aH-NMR Spectra of Fish Oils and Lipids Extracted from Fish Musdes 909 Quantitative Determination of n-3 PUFAs 909 Proton NMR and Lipolysis 911 Oxidation Products 912 Application Remarks 913 References 913 Determination of Fatty Arid Composition and Oxidation in Fish Oils by High Resolution Nuclear Magnetic Resonance Spectroscopy 915 Fatty Acid Analysis of Fish Oils 915 The !H NMR Spectra of Fish Oils 915 The 13C NMR Spectra of Fish Oils 915 Fish Oil Oxidation and its Evaluation by NMR 917 Conclusions 91^ Acknowledgments " ° References 920 Resonance Spectroscopy to Study Lipid Oxidation in Fish and Fish Products 923 Electron Spin Resonance Spectroscopy 923 Investiqation of Free Radicals in Marine Lipids 924 NMR. 926 Concluding Remarks 928 Acknowledgements 929 References 930 Omega-3 Fatty Acid Content of Intact Muscle of Farmed Atlantic Salmon (Salmosalar) Examined by JH MAS NMR Spectroscopy 931 Introduction 931 Experimental Procedures 931 Results and Discussion 932 References 935 HR MAS NMR Spectroscopy of Marine Microalgae, Part 1: Classification and Metabolite Composition from HR MAS 1H NMR Spectra and Multivariate Analysis 937 Introduction 937 Results and Discussion 937 Conclusion 940 References 941 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 943 Introduction 943 Results and Discussion 944 Conclusion 946 References 947 Post-mortem Studies of Fish Using Magnetic Resonance Imaging 949 Introduction 949 Materials and Methods 950 Results and Discussion 951 Conclusions 955 Acknowtedgment 956 References 956 Howis the Fish Meat Afferted by Technological Processes? 957 Introduction 957 Study of SaLt Interaction in Smoked Salmon by SQ and DQF MRS 957 MRI Study of Salt and Fat Distribution in Smoked Salmon 958 Conclusion 961 References 961 PART II Foreword 963 Abbreviations 964 Metabolite Abbreviations 965 Glossary of Terms 967 Acquiring Neurospectroscopy in Clinical Practice 971 Part I: Seven Secrets to Successful Spectroscopy 971 Introduction 971 Signal and Homogeneity 971 Acquisition Paradigms 972 Patient Positioning 972 Sequences 974 Echo Time 974 VoxelSize 975 Number of Averages 976 Voxel Position 976 Consistency 978 Multivoxel Spectroscopy 979 Part II: Neurospectroscopy Protocols 980 Protocol 1: Standard Gray Matter (GM) or Posterior Cingulate Gyrus (PCG) 981 Protocol 2: Standard White Matter 983 Protocol 3: Frontal GM 983 Protocol 4: Hippocampus/Temporal Lobe 983 Protocol 5: Multivoxel Neurospectroscopy (For Focal Use Only) 986 Summary 988 Acknowledgments 989 Suggested Reading List for "Clinical Neurospectroscopy Protocols" 989 Application of Magnetic Resonance for the Diagnosis of Infective Brain Lesions 991 Introduction 991 Magnetic Resonance Techniques 991 Contrast Enhancement 993 Conventional MRI of Infective Brain Lesions 993 Other MRI Methods 994 Magnetic Resonance Spectroscopy 995 Data Analysis 996 Summary 997 Glossary of Terms 997 References 997 Application of 2D Magnetic Resonance Spectroscopy to the Study of Human Biopsies 1001 Introduction 1001 Application of 2D NMR Spectroscopy to Cells and Tissues 1002 Data Acquisition 1005 Data Processing 1006 Concluding Remarks 1010 Acknowledgments 1010 References 1010 Correlation of Histopathology with Magnetic Resonance Spectroscopy of Human Biopsies 1013 Introduction 1013 Histopathology—Strengths and Limitations 1013 Collection and Storage of Biopsy Specimens for Analysis 1014 Collection of a FNAB 1015 Preparation of Specimens for MRS 1016 ExperimentalTemperature 1017 Magnetic Field Strength 1017 MR Spectroscopy Methods 1017 After MR Spectroscopy 1018 Assignments and Visual Inspection of the Data 1018 The Complexity of Tumor Development and Progression 1018 Pattern Recognition Methods 1018 Regression Analysis 1021 Future Challenges 1021 Acknowledgments 1021 References 1021 Functional MRI 1023 Principi.es offMRI 1023 Design offMRI Trials 1023 Prindples of ExperimentaL Design 1025 Prinriples of Analysis 1026 Artifactsand Pitfalis 1027 Practicai AppLications 1028 Conclusion 1032 Abbreviations 1035 Further Reading 1035 High Resolution Magic Angle Spinning (HRMAS) Proton MRS of Surgical Sperimens 1037 List of Abbreviations 1037 Introduction 1037 Methodology 1038 HRMAS MRS of Human SurgicaiSpecimens 1040 Future Developments and Conciusions 1048 Giossary of Terms 1048 Acknowledg ments 1049 References 1049 Intraoperative MRI 1051 Historical Miiestones in Neurotogy 1051 Principles of Intraoperative Imaging 1051 Hardware and Configuration 1051 Clinical AppLications of iMRI 1053 Neoplasia 1055 Epilepsy 1055 Vascular disorders 1058 Spine 1059 Future Directions 1059 Bioi nformatics 1061 Acknowledgments 1062 References 1062 In Vivo Magnetic Resonance Spectroscopy in Breast Cancer 1063 Introduction 1063 In vivo Localization in MRS 1063 31P M R Spectroscopy 1064 JH MR Spectroscopy of Breast 1065 Future Directions and Conciusions 1070 Acknowledgments 1071 References 1071 In Vivo Molecular MR Imaging: Potential and Limits 1073 Introduction 1073 Detectability 1073 Cell Labeling 1076 In vivo MRI Experiments 1077 Biological Aspects of Cell Labeling 1078 Summary 1081 Outlook 1081 Acknowledgment 1081 GLossary of Terms 1081 References 1082 In vivo 13C MRS 1085 Introduction 1085 Methods 1085 Pulse Sequences for in vivo 13C MRS 1088 Checking System Performance 1089 Data Processing 1091 Modeling and Determination of Flux Rates 1092 MisceLlaneous 1093 Applications 1093 Hyperpolarized 13C Compounds 1096 Acknowledgments 1096 Glossary 1096 References 1098 Magnetic Resonance Spectroscopy and Spectroscopic Imaging of the Prostate, Breast, and Liver 1099 Introduction 1099 Techniques for Spectroscopy and Spectroscopic Imaging of the Body 1100 Applications in the Prostate, Breast, and Liver 1105 Summary 1107 Acknowledgments 1108 Glossary of Terms 1108 References 1109 MR-Mammography 1113 Introduction 1113 History of MRM 1113 Pathophysiological Background of MRM 1114 Technique 1122 Indications for MRM 1122 Discrepancies and Pitfalls 1123 Future Challenges 1124 References 1125 Internet Resources 1127 Phosphorus Magnetic Resonance Spectroscopy on Biopsy and In Vivo 1129 Features of 31P MRS in Tissues 1129 31P MRS of Tissue Biopsy Samples 1132 31PMRSJf7 Vivo 1137 References 1144 Radio Frequency Coils for Magnetic Resonance Spectroscopy 1149 The Requirements 1149 The Issues 1H9 The Solenoid Coil and Saddle-Shape Coil 1150 SurfaceCoil 1150 Superconducting rf Coils 1152 PhasedArray 1152 ßi Homogeneity Vs. SNR 1152 Transmit-Only and Receive-Only Coils 1153 LocaL rf CoiLs with Improved ßi Homogeneity and SNR 1154 Implanted rf Coils 1154 Microcoils 1154 Dual Frequency rf Coils 1155 Summary 1155 Glossary of Terms 1155 References 1155 Spatially Resolved Two-Dimensional MR Spectroscopy in vivo 1157 Introduction 1157 Single- and Multi-voxel Based 1D aH MR Spectroscopy 1157 Single Volume Localized 2D XH MR Spectroscopy 1159 Artefacts in Localized ZD MRS and SimuLation 1166 Multi-Voxel Based 2D 1H MR Spectroscopy 1166 Summary 1168 Acknowledgment 1168 References 1168 Glossary 1171 Overview of NMR in the Pharmaceutical Sciences 1171 Applications of Cryogenic NMR Probe Technology for the Identification of Low-Level Impurities in Pharmaceuticals 1171 Flow NMR Techniques in the Pharmaceutical Sciences 1171 Developments in NMR Hyphenation for Pharmaceutical Industry 1171 LC-NMR in Dereplication and Stracture Elucidation of Herbai Drugs 1171 New Approaches to NMR Data Acquisition, Assignment and Protein Structure Determination: Potential Impact in Drug Discovery 1171 Transferred Cross-CorreLated Relaxation: Application to Drug/Target Complexes 1172 Novel Uses of Paramagnets to Solve Complex Protein Structures 1172 Fast Assignments of 15N-HSQC Spectra of Proteins by Paramagnetic Labeling 1172 Phospholipid Bicelle Membrane Systems for Studying Drug Molecules 1172 Partial Alignmentfor Structure Determination of Organic Molecules 1172 Measurement of Residual Dipolar Couplings and Applications in Protein NMR 1172 Using Chemical Shift Perturbations to Validate and Refine the Docking of Novel IgE Antagonists to the High-Affinity IgE Receptor 1172 Dual-Region Hadamard-Encoding to Improve Resolution and Save Time 1172 Nonuniform Sampling in Biomolecular NMR 1173 Structural Characterization of Antimicrobial Peptides by NMR Spectroscopy 1173 Pharmaceutical Applications of Ion Channel Blockers: Use of NMR to Determine the Structure of Scorpion Toxins 1173 Structure and Dynamics of Inhibitor and Metal Binding to Metallo-ß-Lactamases 1173 NMR Spectroscopy in the Analysis of Protein-Protein Interactions 1173 Identification and Characterization of Ternary Complexes Using NMR Spectroscopy 1173 The Transferred NOE 1173 NMR Kinetic Measurements in DNA Folding and Drug Binding 1174 The Use of NMR in the Studies of Highly Flexible States of Proteins: Relation to Protein Function and Stability 1174 NMR-based Metabonomics Techniques and Applications 1174 Protein Misfolding Disease: Overview of Liquid and Solid-State High Resolution NMR Studies 1174 19F NMR Spectroscopy for Functional and Binding High-Throughput Screening 1174 Applications of Receptor-Based NMR Screening in Drug Discovery. . . 1174 NMR SHAPES Screening 1175 NMR-Based Screening Applied to Drug Discovery Targets 1175 NMR and Structural Genomics in the Pharmaceutical Sciences 1175 Section Preface 1176 Overview of NMR in the Pharmaceutical Sciences 1177 Introduction 1177 Technical. Developments 1178 Structure-based Design 1179 NMR Screening 1181 Studies of Drug Effects 1182 Future Directions 1182 Acknowledgments 1182 References 1183 Instrumentation 1185 Applications of Cryogenic NMR Probe Technology for the Identification of Low-Level Impurities in Pharmaceuticals 1187 Introduction 1187 Cryogenic NMR Probes 1187 Sample Preparation 1188 Identification of Degradants 1188 Applications of Cryogenic NMR Probe Technology 1189 Condusions 1193 References 1193 Flow NMR Techniques in the Pharmaceutical Sciences 1195 Introduction 1195 LC-NMR 1195 LC-NMR-MS 1196 Other Detectors in LC-NMR 1197 Other Chromatography in LC-NMR 1197 Other Plumbing Schemes: Loop-Collection LC-NMR and Solid-Phase Extraction NMR (SPE-NMR) 1197 Applications of LC-NMR 1197 Limitations of LC-NMR 1197 Flow-Injection Analysis NMR (FIA-NMR) 1197 Direct Injection NMR (DI-NMR) 1198 Complementary Technologies 1199 Condusions 1200 References 1200 Developments in NMR Hyphenation for Pharmaceutical Industry 1203 Introduction 1203 On-Flow LC-NMR 1203 Direct Stop-Flow 1204 Loop Collection 1206 Post-Column Solid Phase Extraction 1206 Cryogenic Probes for LC-NMR 1208 Improvements in the LC Peak Detection by Integrating Mass Spectroscopy into the LC-NMR Setup 1209 Conclusion and Outlook 1209 References 1210 LC-NMR in Dereplication and Structure Elucidation of Herbai Drugs 1211 Introduction 1211 Dereplication of Skullcap Herb 1212 Structure Elucidation of Aloe MetaboLites 1214 References 1217 Techniques 1219 New Approaches to NMR Data Acquisition, Assignment and Protein Structure Determination: Potential Impact in Drug Discovery 1221 Introduction 1221 Fast Multidimensional NMR Spectroscopy 1221 Speeding Up the Assignment Process 1223 Automated Protein Structure Determination 1225 Condusion 1227 References 1227 Transferred Cross-Correlated Relaxation: Application to Drug/Target Complexes 1229 Introduction 1229 Cross-Correlated Relaxation forthe Measurement of Projection Angles between Tensors 1229 Application to the Epothilone/Tubulin Complex 1234 Condusion 1235 References 1235 Novel Uses of Paramagnets to Solve Complex Protein Structures 1237 Introduction 1237 Methods to Bind Paramagnets to Non-Metalloproteins 1237 PCS Assignment and Ilse of PCSs and pmiRDCs as Structural Restraints 1239 New Approaches to Measurement of Small, ParamagneticaLly Induced RDCs 1240 Structural Applications of PCSs and pmiRDCs 1240 Condusion 1242 References 1242 Fast Assignments of 15N-HSQC Spectra of Proteins by Paramagnetic Labeling 1245 Introduction 1245 £186-8 Complex 1245 Paramagnetic Restraints Derived from 15N-HSQC Spectra of Paramagnetic and Diamagnetic E186-8 Complexes 1246 PLATYPUS Algorithm for Resonance Assignments from Paramagnetic Restraints 1247 Results Obtained with Selectively Labeled £186-8 Complexes 1248 Alternative Methods 1249 Outlook 1249 Acknowledgments 1250 References 1250 Phospholipid Bicelle Membrane Systems for Studying Drug Molecules 1253 Introduction 1253 Membrane Systems for NMR Studies 1254 Optimizing Isotropie Bicelles for Drug Conformational Studies 1255 Magnetkally Aligned Bicelles for Studying Drug Orientation 1257 Condusion 1258 References 1258 Partial Alignment for Structure Determination of Organic Molecules 1261 Introduction 1261 Residual Dipolar Couplings 1261 The Alignment Tensor 1261 Alignment Media 1262 RDC Measurement 1263 Applications 1265 Conclusion 1266 References 1266 Measurement of Residual Dipolar Couplings and Applications in Protein NMR 1269 Introduction 1269 Measurement of Backbone Residual Dipolar Couplings in Proteins 1270 AppLications of Residual Dipolar Couplings in Proteins 1271 Discussion 1272 Acknowledgments 1273 References 1273 Using Chemical Shift Perturbations to Validate and Refine the Docking of Novel IgE Antagonists to the High-Affinity IgE Receptor 1275 Hairpin Peptide Structure 1275 Zeta Peptide Structure 1275 Receptor Binding 1276 Conclusion 1280 References 1280 Dual-Region Hadamard-Encoding to Improve Resolution and Save Time 1281 References 1286 Nonuniform Sampling in Biomolecular NMR 1287 MaxEnt Reconstruction 1288 Nonuniform Sampling 1289 Example Applications 1289 Concluding Remarks 1293 Acknowledgments 1293 References 1293 Applications 1295 Structural Characterization of Antimicrobial Peptides by NMR Spectroscopy 1297 Introduction 1297 Solution Structures of Antimicrobial Peptides 1297 Solid-State NMR Experiments: Peptide Orientation in Bilayers 1302 Conclusions and Future Directions 1303 Acknowledgments 1303 References 1303 Pharmaceutical Applications of Ion Channel Blockers: Use of NMR to Determine the Structure of Scorpion Toxins 1307 Introduction 1307 Use of NMR to Determine the Structure of Rare Components 1307 NMR Structures of Toxins Active on Sodium Channels 1309 NMR Structures of Toxins Active on Potassium Channels 1309 Conclusion 1311 References 1311 Structure and Dynamics of Inhibitor and Metal Binding to Metallo-ß-Lactamases 1313 Introduction 1313 Effect of Inhibitor Binding on the ßackbone Amide Resonances 1314 Effect of Inhibitor Binding on the Imidazole Resonances of the Metal Ligands 1314 Direct Observation of the Active-Site Metals 1316 Effects of Thiomandelate Binding on the 113Cd Spectrum 1317 Conclusion 1318 References 1318 NMR Spectroscopy in the Analysis of Protein-Protein Interactions 1321 Introduction 1321 Tackling the Size Issue for Larger Protein Complexes 1321 Reducing Complexity: Differential Isotope Labeling 1322 Obtaining Long-Range Structural Information 1323 Mapping Protein-Protein Interfaces 1324 Protein-Protein Interactions and Chemical Exchange 1325 Stitching Up Proteins for Improved Stability 1326 Docking Protein Complexes 1326 Summary 1327 References 1327 Identification and Characterization of Ternary Complexes Using NMR Spectroscopy 1329 Introduction 1329 Borate Complexes and Their Study by NMR Spectroscopy 1329 Ternary Complexes Involving Organic Molecules 1332 ILOE Observations—Type II Dihydrofolate Reductase 1336 Summary 1338 References 1338 The Transferred NOE 1339 Affinities and Timescales 1339 The NOE 1340 Spin Diffusion 1341 The Transferred NOE 1341 Related Experiments 1344 References 1344 NMR Kinetic Measurements in DNA Folding and Drug Binding 1345 Drug-Quadruplex Interactions Studied by NMR 1345 Exchange Rates for Drug Binding to Quadruplex DNA 1345 DNA Hairpin Folding and Slow Exchange Equilibria 1346 Slow Exchange Between Two Conformers 1346 DNA Hairpin Folding Kinetics by Magnetization Transfer 1348 Acknowledgments 1348 References 1348 The Use of NMR in the Studies of Highly Flexible States of Proteins: Relation to Protein Function and Stability 1351 Introduction 1351 Insulin Flexibility and Activity 1352 The Acid State of Human Growth Hormone 1354 Acknowledgement 1357 References 1357 NMR-based Metabonomics Techniques and Applications 1359 Introduction 1359 Metabonomics Analytical Technologies 1359 Selected Applications of Metabonomics 1363 Conclusions 1366 References 1367 Protein Misfolding Disease: Overview of Liquid and Solid-State High Resolution NMR Studies 1369 Protein Misfolding Diseases 1369 Natively Unfolded Proteins Involved in Protein Misfolding Diseases 1369 Brief Background in NMR Parameters 1369 Proteins Involved in Misfolding Diseases Studied by NMR 1370 Amyloid Precursor Protein 1371 Prion Protein 1371 ot-Synudein 1371 Cu-Zn-Superoxide Dismutase 1372 Transthyretin 1372 References 1372 19F NMR Spectroscopy for Functional and Binding High-Throughput Screening 1375 FAXS 1375 3-FABS 1378 Conclusion 1380 References 1381 Applications of Receptor-Based NMR Screening in Drug Discovery 1383 Introduction 1383 Fragment-Based Screening: Identifying "Hot Spots" on Protein Surfaces 1383 Receptor-Based NMR Screening 1384 Utilization of Fragment Leads in Drug Design 1385 Core Replacement 1385 High-Throughput Core Elaboration 1386 Fragment Linking 1387 Receptor-Based Methods for Lead Validation and Characterization 1387 Summary 1388 References 1388 NMR SHAPES Screening 1391 Introduction 1391 Principles of SHAPES Screening 1391 Design of the SHAPES Compound Library 1391 NMR Methods for Screening Compound Libraries 1392 Implementation of SHAPES Screening 1394 Pre-HTS Screening 1394 Post-HTS Screening 1396 Lead Optimization 1396 Conclusion 1397 References 1398 NMR-Based Screening Applied to Drug Discovery Targets 1401 NMR for Lead Discovery 1401 NMR-Based Screening Techniques 1401 NMR-Based Screening Applied to Drug Targets 1405 Condusion 1407 References 1409 NMR and Structural Genomics in the Pharmaceutfcal Sdences 111 Introduction 1411 Strategies and Targets in Structural Genomics 1411 Advantages and Disadvantages of NMR for Structural Genomics 1411 Advances in NMR Instrumentation and Methodology 1415 Outlook and Conclusions 1416 References 1416 PART III Introduction 1417 References 1418 Acoustically Stimulated NMR Relaxometry: Application to the Study of Molecular Dynamics in Liquid Crystalline Materials 1419 Introduction 1419 Why Field-Cycling Experiments in Liquid Crystals? 1419 Relevant Properties of Liquid Crystals 1419 Order Director Fluctuations 1420 Seif Diffusion 1421 Molecular Reorientations 1421 Proton FC Relaxometry in Liquid Crystals 1421 Ultrasound Induced Relaxometry 1422 Outlook 1423 Acknowledgment 1424 References 1424 Characterization of Elastomers Based on Monitoring Ultraslow Dipolar CorreUtions by NMR 1425 Introduction 1425 Background of the Dipolar Correlation Effect 1426 The DCEin Elastomers 1427 Imaging on the Basis of the DCE 1431 Concluding Remarks 1432 References 1432 Correlating Molecular and Macroscopic Properties of Elastomers by NMR Relaxometry and Multi-pulse NMR Techniques 1435 Introduction 1435 Theoretical Background 1435 Relaxometry Experiments 1436 Double Quantum Experiments 1439 Summary 1440 Acknowledgments 1441 References 1441 Determining Structural and Dynamic Distribution Functions from Inhomogeneously Broadened NMR Spectra: The Conjugate Orthogonal Functions Approach 1443 Introduction 1443 Conjugate Orthogonal Functions 1443 Orientational Order 1445 Conclusions 1449 Acknowledgments 1449 References 1449 Fluid Diffusion in Partially Filled Nanoscopic and Microscopic Porous Materials 1451 Introduction 1451 The Two-Phase Exchange Model in NMR Diffusometry 1451 Experi mental 1454 Discussion and ConcLusions 1456 Acknowledg ments 1456 References 1457 Gas Adsorption on Carbon Nanotubes 1459 Introduction 1459 NMR Spectroscopy of CNTs 1459 ESR Spectroscopy of CNTs 1460 Gas Adsorption on MWNTs 1460 Gas Adsorption on SWNTs 1463 Summary 1463 Acknowledg ments 1464 References 1464 Magnetic Resonance Studies of the Heterogeneous Rotational and Translational dynamics in Disordered Materials 1467 Introduction 1467 Rotational Dynamics Near the Vitrification Transition 1468 Freezing in GLassy Crystals 1468 Heterogeneous Transport in Ionic Conductors 1469 Probing Secondary Relaxations 1470 Single-Molecule Spectroscopy 1471 Conclusion 1471 References 1471 Nuclear Magnetic Resonance in Ferromagnetic Multilayers and Nanocomposites: Investigations of Their Structural and Magnetic Properties 1473 Introduction 1473 NMR and Atomic Structure 1473 Local Magnetic Moments—Hyperfine Field and Magnetization Profiles 1474 Zero-Field NMR—Local Restoring Field and Magnetic Stiffness 1474 Magnetic Phase Separation 1476 In Field NMR—Local Magnetic Anisotropy 1477 Conclusions 1477 References 1478 1H Solid-State NMR of Supramolecular Systems 1479 Introduction 1479 High Resolution Solid-State NMR 1479 Applications to Supramolecular Structures 1482 References 1486 Quadrupolar NMR of Inorganic Materials: The Multiple-Quantum Magic Angle Spinning Experiment 1487 Introduction 1487 Multiple-Quantum MAS 1487 Pulse Sequencesfor MQMAS 1489 Spectral Analysis 1491 Application to Disordered and Amorphous SoLids 1492 Summary 1^94 Acknowledgments 1494 References 1494 Rheo-NMR Spectroscopy 1495 Introduction 1495 Experimental Aspects 1495 Nematic Liquid CrystaLs 1496 Hexagonal and Lamellar Lyomesophases 1498 Shear-Induced Phase Transitions 1500 Conclusions 1500 References 1500 Advances in Single-Sided NMR 1503 Introduction 1503 Material Characterization via Relaxometry by the NMR-MOUSE 1503 3D Imaging with a Single-Sided Sensor 1504 Flow Characterization with a Single-Sided Sensor 1505 Conclusions and Remarks 1506 References 1506 Site-specific Characterization of Structure and Dynamics of Complex Materials by EPRSpin Probes 1509 Introduction 1509 Addressing Specific Sites by Spin Probes and Spin Labels 1509 Oetecting Supramolecular Interactions by Changes in Probe Dynamics 1510 Characterization of Broad Distance Distributions 1510 Concatenated Macrocycles in Frozen Solution 1511 Polyelectrolytes: Probing Polyion-Counterion Interaction in Fluid and Frozen Solution 1514 References 1516 NMR of Organic Semiconductors 1519 Introduction 1519 Ligand Dynamics in ALq3 1520 Characterizing the Isomers of Alq3 1522 Variable Deposition Rate Studies 1523 Conclusions 1525 Acknowledgments 1525 References 1525 Solid State NMR of Xerogels 1527 Acknowledgments 1530 References 1530 Solid-State 17O NMR Spectroscopy of High-Pressure Silicates 1531 Introduction 1531 Oxygen NMR 1531 Sample Preparation 1532 MQMAS NMR of Upper Mantle Silicates 1532 STMAS NMR of Dense Silicate Phases 1536 NMR of Hydrous Magnesium Silicates: Humite Minerals 1536 Discussion and Conclusions 1539 Acknowledgments 1540 References 1540 The Structure of Oxide Glasses: Insights frotn 170 NMR 1543 References 1547 Studies of the Local Structure of Silk Using Solid-State NMR 1549 Introduction 1549 The NMR Measurements of Torsion Angles 1549 Geometrical Information on the Molecular-to-Nanometer Scale 1550 Conclusions 1554 Acknowledgments 1556 References 1557 Velocity Imaging of Granulär Materials 1561 Introduction 1561 NMR of Transport in Granulär Media—an Overview 1561 Gas-Fluidized Bed 1562 Rotating Drum 1565 Summary 1566 Acknowledgments 1567 References 1567 Glossary 1569 Introduction 1571 References 1571 High Resolution Solution State Methods 1573 Characterization of the Chemical Composition of Beverages by NMR Spectroscopy 1575 Introduction 1575 Alcoholic Beverages 1575 Nonalcoholic Beverages 1578 References 1580 High Resolution NMR of Carrageenans 1583 Carrageenan Structure 1583 Experimental Setup 1583 Analysis of the Major Carrageenan Types 1584 Analysis of Minor Components 1585 References 1587 Flavor-Food Compound Interactions by NMR Spectroscopy 1589 References 1593 High-Resolution Nuclear Magnetic Resonance Spectroscopy of Fruit Juices 1595 References 1598 High-Resolution NMR Spectroscopy in Human Metabolism and Metabonomics 1601 Introduction 1601 Water Suppression 1602 Assignments of the Metabolite Resonances 1603 Spectral Editing in Biologkai NMR Spectroscopy 1603 Other Useful Techniques 1604 NMR-Based Metabonomics Techniques 1605 Future Perspectives 1606 References 1606 High-Resolution NMR of Milk and Milk Proteins 1609 GeneraL Remarks 1609 NMRSpectra of Milk 1609 NMR Studies of Milk Proteins 1611 References 1613 High-Resolution 13C Nuclear Magnetic Resonance in the Study of Oils 1615 Introduction 1615 Quantitative Determination of the Oils Major Components 1615 Minor Oil Components 1619 13C NMR Spectroscopy As a Discriminating forthe Varietal, Geographical, and Botanical Origin of Vegetable Oils 1620 13C NMR of Olive OiL Minor Compounds to Oetermine Oil Authenticity 1620 References 1621 High-Resolution 1H Nuclear Magnetic Resonance in the Study of Oils 1623 Introduction 1623 Triglycerides 1623 Minor Compounds 1625 Use of :H NMR Spectroscopy to Characterize Olive Oil Geographical Origin 1627 References 1628 SNIF-NMR—Part 1: Prinriples 1629 Introduction 1629 Isotopic Abundances and Isotopic Ratios 1629 Isotopic Fractionation 1630 Quantitative Deuterium-NMR 1631 Referencing of Isotopic Parameters 1632 Carbon SNIF-NMR 1635 References 1636 SNIF-NMR—Part 2: Isotope Ratios as Tracers of Chemical and Biochemical Mechanistic Pathways 1637 Introduction 1637 Influence of Phase Transitions and Transport Phenomena on the Isotopic Parameters 1637 Simultaneous Determination of Site-Specific Thermodynamic Isotope Effects 1638 Determination of Kinetic Isotope Effects 1639 Sperific Connections Between SNIF Parameters of Reactants and Products 1640 Elaboration of SNIF-NMR Probes: From Carbohydrates to Ethanol and Glycerol 1642 Access to Mechanistic Information on Enantiotopic Hydrogen Sites 1643 References 1644 SNIF-NMR—Part 3: From Mechanistic Affiliation to Origin Inference 1647 Introduction 1647 SNIF Parameters as Witnesses of Individual Mechanistic Routes of Atoms 1647 Identification of Starting Materials: The Nature Laboratory 1651 Experimental Strategies for Origin Inference of Products 1651 Natural or Synthetic Origin of Products 1652 Characterization of Chemical Processes 1653 Identification of Plant Precursors 1654 Climatic Effects and Geographicat Origin 1655 References 1657 SNIF-NMR—Part 4: Applications in an Economic Context: The Example of Wines, Spirits, and Juices 1659 Introduction 1659 Current Regulations About Wines and Juices 1659 Ethanol: A Reliable Isotopic NMR Probe for Characterizing Wines, Spirits, and Juices in an Industrial Context 1660 Origin Authentication and Data Banks 1661 NMR Methodologies in an OfficiaL and Economic Context 1662 Determination of Illegal Enrichments 1662 Isotopic Characterization of Concentrated Juices 1663 Multi-component and Multi-isotope Strategies in the Detection of Adulterations 1663 Detection of Exogeneous Minor Components 1664 References 1664 High-ResoLution Nuclear Magnetic Resonance Spectroscopy of Wine, Beer, and Spirits 1667 References 1670 Relaxation Time Methods 1673 NMR Relaxation of Dairy Products 1675 Introduction 1675 Water Relaxation 1675 Water Retention 1676 Water Diffusion 1677 Fat Relaxation 1677 Conclusion 1678 References 1678 Characterization of Molecular Mobility in Carbohydrate Food Systems byNMR 1681 Introduction 1681 Water Molecular Mobility by NMR 1681 NMR to Determine Various Populations of Water 1682 T2 Distribution of Water in Starch 1683 Solid-State Nuclear Magnetic Resonance 1683 Solid Mobility by Cross Relaxation 1686 NMR Mobility and Microbial Activity 1687 Concluding Remarks 1688 References 1689 Diffusion and Relaxation in Gels 1691 Introduction 1691 Diffusion 1691 Relaxation 1693 References 1696 NMR Relaxation and Diffusion Studies of Horticultural Products 1699 Introduction 1699 NMR Relaxation and Water Compartmentation 1699 NMR Diffusometry and Water Compartmentation 1700 Fruit and Vegetable Quality 1701 Conclusions 1703 Acknowledgment 1703 References 1703 Proton NMR Relaxometry in Meat Science 1707 Introduction 1707 Determination of Fat Content in Meat and Meat Products Using NMR Relaxometry 1707 T2 Relaxation in Meat 1707 Water-Holding Capacity 1708 Relaxometry Studies During Conversion of Muscle to Meat 1708 Relaxometry Applied During Meat Processing 1710 Conclusions 1710 References 1710 Time-Domain NMR in Quality Control: More Advanced Methods 1713 Introduction 1713 Gradient Experiments 1713 Combined Relaxation Analysis in Foods with High Water Content 1714 Conclusion 1716 Acknowledgements 1716 References 1716 Time-Domain NMR in Quality Control: Standard Applications in Food 1717 Introduction 1717 Time-Domain NMR (TD-NMR) 1717 A. Determination of the SFC in Fat Compositions 1717 B. Simultaneous Oil and Moisture Determination in Food (Moisture Content Below Approx. 15%) 1720 C. Oil Content Determination in Pre-Dried Olives 1721 Conclusion 1721 Acknowledgment 1721 References 1721 Nuclear Magnetic Relaxation in Starch Systems 1723 Introduction 1723 General Considerations for NMR of Starch Systems 1724 Solid Starch Systems 1726 Proton Spin-Spin Relaxation and Second Moment of Solid Starch Polysaccharides 1726 Water in Starch Systems 1729 Future Perspective 1730 References 1730 High Resolution Solid State Methods 1733 Magic Angle Spinning NMR of Flours and Doughs 1735 Introduction 1735 "CCross Polarization MAS NMR of Flours 1735 1H High Resolution MAS NMR of Flours 1735 1H and 13C MAS NMR of Doughs 1736 References 1741 High-Resolution Magic Angle Spinning NMR Spectroscopy of Fruits and Vegetables 1743 References 1746 High-Resolution Solid-State NMR of Gluten and Dough 1747 Introduction 1747 Gluten 1748 Flour and Dough 1750 References 1754 High-Resolution Solid-State NMR as an Analytical Tool to Study Plant Seeds 1755 Introduction 1755 Spectral Edition Inside the Seeds 1755 Assignments of the NMR Signals 1756 Solid-State Proton NMR 1757 Conclusion and Prospects 1757 References 1759 High-Resolution Solid-State NMR Spectroscopy of Starch Polysaccharides 1761 Introduction 1761 NMR Techniques 1763 Spectral Editing Techniques 1766 Future Perspectives 1767 References 1768 Imaging and Related Techniques 1771 NMR Imaging of Bread and Biscuit 1773 Introduction 1773 Monitoring the Baking Process 1773 Monitoring the Post-Chilling and Freezing Steps 1775 Assessing the Bread Crumb Structure 1776 References 1777 NMR Imaging of Oairy Products 1779 Introduction 1779 Waterand Fat Content and Distribution 1779 Macrostructure Information 1780 Temperature and Flow 1782 Conclusion 1783 References 1783 NMR Imaging of Dough 1785 Introduction 1785 Assessment of Ice Fraction Cartographies During Freezing, Storage, and Thawing of Raw Dough 1785 Assessment of Porosity During the Proving Process 1787 References 1789 MRI in Food Process Engineering 1791 Introduction 1791 Structure and Changes 1791 References 1794 Rheo-NMR: Applications to Food 1797 Introduction 1797 Applications of Rheo-NMR 1798 Relevance of NMR for Process Engineering 1800 References 18°1 Temperature Measurements by Magnetic Resonance 1803 Introduction 1803 7i and Tz Relaxation Times 1803 Diffusion Coefficient 1803 Chemical Shift 1804 Summary 1807 References 1807 Statistical Methods 1809 Chemometric Analysis of NMR Data 1811 Introduction 1811 Unsupervised Data Exploration by PCA 1814 Supervised Data Exploration 1814 Conclusion 1821 References 1821 Direct Exponential Curve Resolution by Slicing 1823 Tri-Linear Models 1825 Data Slicing 1825 NMR Relaxometry: An Example 1827 Conclusion 1828 References '. 1830 ESR Methods 1831 ESR as a Technique for Food Irradiation Detection 1833 Introduction 1833 Definition of the Absorbed Dose (kGy) 1833 LabeLing 1833 Interactions of Radiation with Matter 1833 Food Irradiation Detection 1834 Conclusion 1837 References 1837 ESR Spectroscopy for the Study of Oxidative Processes in Food and Beverages 1839 Introduction 1839 ESR Detection of Radicals in Foods 1839 Spin Trapping 1840 Prediction of Oxidative Stability of Foods 1840 Other Uses of ESR for Studies of Food Oxidation 1842 Perspective and Future Developments 1842 References 1843 Applications to Food Systems 1845 Magnetic Resonance Studies of Food Freezing 1847 Introduction 1847 Spin Relaxometry 1847 PFGSE Diffusion Measurements 1851 Magnetic Resonance Imaging 1851 Liquid Phase Chemical Spectroscopy 1853 Solid-State NMR 1853 Conclusion 1854 References 1854 Nuclear Magnetic Resonance Studies on the Glass Transition and Crystallization in Low Moisture Sugars 1857 Introduction 1857 Line Width and Shape Studies 1857 Deuterium Line Shape Studies 1859 Relaxation Studies 1859 High-Resolution Solid-State 13C NMR 1862 CPMAS NMR and CrystalLization 1864 Other NMR Techniques As Monitors of the Glass Transition 1865 Imaging in the Study of Glasses 1866 References 1866 Probing the Sensory Properties of Food Materials with Nuclear Magnetic Resonance Spectroscopy and Imaging 1867 Introduction 1867 Texture 1868 Taste 1870 Summary and Future Applications 1871 References 1871 Single-Sided NMR in Foods 1873 Introduction 1873 The Bruker Single-Sided NMR Device 1873 Experimental Approaches in Fat and Water Determination 1873 Conclusion 1875 Acknowledgment 1875 References 1875 Applications of NMR in the Studies of Starch Systems 1877 Introduction 1877 NMR Studies of Starch Systems 1878 Conclusion 1883 References 1883 Index 1887 List of Tables Part 1: Applications in Chemistry, Biological and Marine Sciences Kinetics of Amyloid Fibril Formation of Human Calcitonin Table 1 Kinetic parameters for the fibril formation of hCTs in various pH solution 11 NMR Chemical Shift Map Table 1 Calculated 13C chemical shifts (ppm) of L-aLanine residue Ca- and Cp-carbons by the 4-31G-GIA0-CHF method 36 Table 2 Observed 13C chemical shifts of L-alanine residue Ca- and Cß-carbons for peptides including L-alanine residues in the solid state, as determined by 13C CP-MAS NMR, and their geometrical parameters 36 NMR Chemical Shifts Based on Band Theory Table 1 Observed and calculated 13C chemical shifts and shieldings of an isolated polyglycine chain 42 Table 2 Calculated 15N shieldings and band gaps for aromatic and quinoid polypyrrole modeis using INDO/S TB MO 44 Table 3 Total energies, band gaps, and NMR chemical shieldings for a Single chain of os- and tram-polyacetylenes and for a 30 crystal of eis- and trans-polyacetylenes as calculated by ob initio TB MO method within the framework of ST0-3G minimal basis set 46 Modeling NMR Chemical Shifts Table 1 Comparison of the calculated chemical shieldings using the KT1, KT2, and KT3 exchange-correlation functionals with those from other electronic strueture methods. The calculations were performed using the experimental geometries of the compounds. Data from references [46-49] in ppm, referenced to the bare nucleus (i.e. absolute shieldings) 51 Table 2 Parameters defining the linear correlation between calculated 1H chemical shieldings and measured chemicaL shifts in selected molecules from the G2 and G3 sets 53 Table 3 Parameters defining the linear correlation between calculated 13C chemical shieldings and measured chemical shifts in selected molecules from the G2 and G3 sets 54 Table 4 Parameters defining the linear correlation between calculated 15N chemical shieldings and measured chemical shifts in selected molecules from the G2 and G3 sets 55 Table 5 Parameters defining the linear correlation between calculated 15N chemical shieldings and measured chemical shifts in selected molecules from the G2 and G3 sets 56 Crystal Strueture Refinement Using Chemical Shifts Table 1 Energy contributions and chemical shift differences of the original and chemical shift refined cellulose Ia struetures 72 Industrial Application of In situ NMR Imaging Experiments to Steel-Making Process Table 1 The quantitative analysis of these chemical struetures between sample 1 and 3 after drying obtained by CRAMPS and MQMAS spectra 164 NMR Imaging: Monitoring of Sweüing of Environmental Sensitive Hydrogels Table 1 Water diffusion coefficientinside PVMEgelswith differentcross-linking densities (irradiation doses). A calibration of the signal (Figure 9) is necessary to calculate absolute values of D. This was done by means of measurements with pure water at different temperatures 188 Solid State NMR Characterization of Solid Surface of Heterogeneous Catalysts TabLe 1 13C MAS NMR isotopic chemical shift (in ppm) of carbonyl carbon of 2-13C-acetone on (or in) different solid (or liquid) acids 203 Solid State 19F-NMR Analysis of Oriented Biomembranes Table 1 CSA parameters of 19F-labeled amino acids used for structure analysis Two different sets of results are separated by a slash, namely of the polycrystalline amino acids (U. Dürr, PhD thesis, in preparation) and when they are incorporated into a lyophilized peptide 260 Site-Directed NMR Studies on Membrane Proteins Table 1 Conformation-dependent 13C chemical shifts of Ala residues (ppm from TMS) 288 3H NMR and Its Application Table 1 Important properties of tritium and its non-radioactive isotopes 392 On-line SEC-NMR Table 1 Effects of flow rate on the^ NMR signal of CHÜ3 in CDCl3 (5/95 v/v) measured at 750 MHz using an LONMR probe with a 60 ^ flow cell 396 Separated Detection of H-Transfer Motions in Multi-H-Bonded Systems Studied by Combined H NMR and 35Cl NQR Measurements Table 1 Theoretical values of quadrupole coupling constants (e2Qq), asymmetry parameters of electric field gradients (/j) and resonance frequencies (v) calcuLated for a neutral chloranilic acid molecule, and monovalent and divalent chloranilate ions in isolated states 429 EPR: Prinriples Table 1 Equations for the g matrix for the four possibLe cases using the d±\ and dxy basis functions for tz 438 Crystalline Structure of Ethylene Copolymers and Its Relation to the Comonomer Content Table 1 Specifications of EDAM and EMA copolymers 543 Two-Dimensional NMR Analysis of Stereoregularity of Polymers Table 1 Assignments of the methylene carbon resonances of methyl acrylate (A)/methyl methacrylate (B) copolymers from the HSQC spectrum 556 Table 2 1H-1H cross-correlations between non-equivalent geminal protons of methylene and between methine protons and methylene protons in methyl acrylate (A)/methyl methacrylate (B) copolymers observed from the TOCSY spectra 556 Table 3 Couplings of carbonyl carbon with cc-methyl protons («-CH3 and methylene protons observed from the 2D HMBC spectra 558 Polymer Microstructure: The Conformational Connection to NMR Table 1 Nonequivalent 13C NMR chemical shifts of the isopropyl methyl carbons in branched alkanes . 565 Table 2 13C spin-lattice relaxation times, 7"i(s), for the crystalline carbons in s-PS polymorphs 569 H CRAMPS NMR of Polypeptides in the Solid State Table 1 H and 13C chemical shifts and characteristics of polypeptides and cyclic dipeptides 589 Table 2 1H and 13C chemical shifts, and conformational characteristics of silk fibroin and its model polypeptide sample 597 Table 3 JH chemical shifts and conformational characteristics of polypeptides 598 Quantum Information Processing as Studied by Molecule-Based Pulsed ENDOR Spectroscopy Table 1 ENDOR Systems regarding the satisfactions of the DiVincenzo criteria 645 Table 2 The spin Hamiltonian parameters of the malonyl radical 646 Table 3 The unitary Operation and corresponding pulse sequences for encoding 647 Table 4 Detection through angular dependence of the intensities of the electron spin echo 649 Refinement of Nucleic Acid Structures with Residual Dipolar Coupling Restraints in Cartesian Coordinate Space Table 1 Bond angles (degrees) involving hydrogen atoms in sugar-phosphate moieties 664 Two-Dimensional 17O Multiple-Quantum Magic-Angle Spinning NMR of Organic Solids Table 1 A summary of organic compounds studied by 170 MQMAS NMR 693 Rotational-Echo, Double-Resonance NMR Table 1 Phases of the xy-4 cycle and its supercycles 711 Table 2 Dipolar dephasing functions 713 Optimization of MRI Contrast for Pre-Clinical Studies at High Magnetic Field Table 1 Standard scan parameters 756 Table 2 T\ and Tz values for mouse and human tissue at different field strengths 757 The Application of In Vivo MRI and MRS in Phenomic Studies of Murine Models of Disease Table 1 In vivo MRI measurement of brain morphology 768 Application of MRS in Cancer in Pre-clinical Models Table 1 In vitro 1H NMR measurement of metabolites in wild-type (Hepa WT) and HIF-lß deficient (Hepa c4) tumor extracts (n = 4) 822 Experimental Cardiovascular MR in Small Animals Table 1 Relevant cardiac functional parameters 834 Comprehensive Compositional Analysis of Fish Feed by Time Domain NMR Table 1 StatisticaL analysis of the agreement between the NMR and the reference chemical methods . 891 Table 2 Repeatability of the NMR measurements on a dry mixture sample 892 Water Distribution and Mobility in Fish Products in Relation to Quality TabLe 1 Application examples 907 Proton NMR of Fish Oils and Lipids Table 1 Assignment of the Signals of the 1H NMR spectra of anchovies lipids 910 Determination of Fatty Acid Composition and Oxidation in Fish Oils by High Resolution Nuclear Magnetic Resonance Spectroscopy Table 1 Fatty acid composition of depot fats from selected fishes 916 Resonance Spectroscopy to Study Lipid Oxidation in Fish and Fish Products Table 1 Relative intensity (ratio between the Signal amplitude and the reference sample (Manganese)) of spin adducts in cod liver oil added PBN as spin trap. The oil were pre-oxidised at 40 °C in 0, 1, 2, 3, and 4 weeks before addition of spin trap. Spectra were recorded after 0, 1, 2, 3, 4, 5, and 24, 48, 72, and 96 h of further oxidation at 40 C. Instrumental settings: sww 5mT, swT 2 min, Mod width 0.2 mT, cf 335.6 mT, timec ls (Jeol X-band). Unpublished data 928 Table 2 Chemical shift assignments of components in the !H NMR spectra associated with changes during lipid oxidation 929 Omega-3 Fatty Acid Content of Intact Muscle of Farmed Atlantic Salmon (Salmo salar) Examined by 1H MAS NMR Spectroscopy Table 1 Omega-3 fatty acid, DHA (C22:6 n-3) and cholesterol content (moL %) of white muscle of farmed AtLantic salmon examined by high-resolution 1H NMR spectroscopy 934 Table 2 Omega-3 fatty acid content (mol %) of white muscle of farmed Atlantic salmon measured on intact muscle and the lipid extracted from the corresponding muscle examined by 1H MAS NMR (200 MHz) and high-resolution :H NMR (500 MHz), respectively 934 HR MAS NMR Spectroscopy of Marine Microalgae, Part 1: CLassification and Metabolite Composition from HR MAS *H NMR Spectra and Multivariate Analysis Table 1 Tentative chemical shift assignment in 1H HR MAS spectra of whole cells of Thatassiosira pseudonana (Bacillariophyceae), referenced to TSP. Literature references: (1) Nicholson and Foxall; (2) Sitter et al. (2002); (3) Willker and Leibfritz (1998); (4) Lindon et ai; (5) Wardetal 939 HR MAS NMR Spectroscopy of Marine Microalgae, Part 2: 13C and 13C HR MAS NMR Analysis Used to Study Fatty Add Composition and Polysaccharide Structure Table 1 Assignments of fatty acid resonances from the 13C HR MAS NMR spectrum of C. miiUeri. Literature u^ed for the assignments 945 Table 2 Assignments of the carbohydrate resonances in the 13C NMR and HETCORR spectra 946 Table 3 Assignments of peaks in Figure 2 947 Post-mortem Studies of Fish Using Magnetic Resonance Imaging Table 1 Mean water and salt content in cod fillet pieces caLculated from the three MR slices images (see Fig. 3 and 4). The corresponding Variation ranges (minimal and maximal Contents) are given in the parentheses 954 Part 2: Applications in Medical and Pharmaceutical Sciences Acquiring Neurospectroscopy in Clinical Practice Table 1 Clinical protocoL decision matrix 981 Application of Magnetic Resonance for the Diagnosis of Infective Brain Lesions Table 1 Choline to creatine ratio determined by Integration of the resonances at 3.2 and 3.0 ppm, respectively. Ratios were determined for cystic GBMs, abscesses with growth of Streptococcus aureus and sterile abscesses 996 Application of 2D Magnetic Resonance Spectroscopy to the Study of Human Biopsies Table 1 Assignment of major cross peaks in 2D 1H-1H COSY MR spectra of thyroid biopsy tissue 1003 Correlation of Histopathology with Magnetic Resonance Spectroscopy of Human Biopsies Table 1 Resonances in one-dimensional JH MR spectra 1015 Table 2 Summary of classifiers and spectral regions using SCS 1016 High Resolution Magic Angle Spinning (HRMAS) Proton MRS of Surgical Spenmens Table 1 Matrix of selected brain metabolite concentrations measured with HRMAS MRS for differentiation between different pathological specimens NAA, in the table, includes both measured resonances of NAA at 2.01ppm and acetate at 1.92 ppm (see text for details); Numbers in parentheses represent resonance chemical shift in ppm. The resonance at 3.93 is tentatively assigned to the Cr metabolite. As an example of the use of this matrix, the Chol resonance can be used to differentiate low-grade/anaplastic astrocytomas from GBMs with a significance of / 0.05. Similarly, the glycine resonance (Gly) can be used to distinguish GBMs from Schwannomas with ap 0.005 1044 Intraoperative MRI Table 1 iMRI Systems with main advantage and disadvantage 1052 TabLe 2 Patient characteristics grouped by pathoLogical finding 1054 Table 3 Number and type of intraoperative MR imaging sequences 1055 In Vivo Magnetic Resonance Spectroscopy in Breast Cancer Table 1 Summary of experimental details used in various :H MRS studies 1066 In vivo 13C MRS Table 1 Equipment needed for 13C MRS beyond that required for Standard MR imaging 1086 Phosphorus Magnetic Resonance Spectroscopy on Biopsy and In Vivo Table 1 Summary of main metabolites detected by 31P MRS in vivo 1130 Table 2 Some measured concentrations of metabolites detected by 31P MRS in different human tissues (units of mM) 1133 Table 3A Published values of h relaxation times in different human tissues 1134 Table 3B Published values of Tz relaxation times in different human tissues 1135 Table 4 Relative merits of tissue extracts and in vivo 31P MRS measurements 1137 Table 5 A summary of the relative merits of STEAM, PRESS, and ISIS for singLe voxel acquisition of 31P MR spectroscopy data 1140 Table 6 Comparison of CSI and Single voxel techniques 1141 Table 7 Features of double resonance techniques 1141 Spatially Resolved Two-Dimensional MR Spectroscopy in vivo Table 1 Experimental parameters for 2D MRS 1164 Overview of NMR in the Pharmaceutical Sciences Table 1 NMR technologies used for structural characterization of receptors, ligands, and ligand-receptor complexes 1179 Table 2 NMR technologies used for high-throughput screening of ligand-receptor complexes 1181 Novel Uses of Paramagnets to Solve Complex Protein Structures Table 1 Magnitudes of pmiRDCs observed for various protein-metal complexes 1239 Measurement of Residual Di polar Couplings and Applications in Protein NMR Table 1 Modulation of the coupling Jmx evolution and 15N chemical shift frequency o n to the raw and manipulated FIDs in the 2D series for values of n from 1 to TDj/2 1271 Structural Characterization of Antimicrobial Peptides by NMR Spectroscopy Table 1 Examples of NMR derived high-resolution solution structures of antimicrobial peptides 1298 Protein Misfolding Disease: Overview of Liquid and Solid-State High Resolution NMR Studies Table 1 Overview of NMR parameters and their conformational dependence 1370 Applications of Receptor-Based NMR Screening in Drug Discovery Table 1 Published examples of receptor-based fragment approaches in the design of novel drug leads 1386 Table 2 Examples of receptor-based NMR methods for the validation of leads derived from HTS, affinity screening, and Virtual ligand screening campaigns 1388 NMR-Based Screening Applied to Drug Discovery Targets Table 1 NMR-based screening applied to drug discovery targets 1405 NMR and Structural Genomics in the Pharmaceutical Sciences Table 1 Summary of global structural genomics initiatives 1412 Part 3: Applications in Materials Science and Food Science Characterization of Elastomers Based on Monitoring Ultraslow Dipolar Correlations by NMR Table 1 Parameters of the Equations (11, 8) fitted to the experimental attenuation curves in dry and swollen samples of NR 1429 Fluid Diffusion in Partially Fitled Nanoscopic and Microscopic Porous Materials Tabte 1 The physical parameters of water and cyclohexane used in the fits of the theory to our experimental data 1455 Gas Adsorption on Carbon Nanotubes Table 1 Sample characteristics 1460 NMR of Organic Semiconductors Table 1 Rate constants determined by least- Squares fitting of the experimental H2 and H3 peak intensities. Error margins represent individual 95% confidence intervaLs 1522 Table 2 Activation parameters obtained from Eyring analysis of the rate constants given in Table 1 Standard errors of regression are indicated 1522 Solid-State 17O NMR Spectroscopy of High-Pressure Silicates Table 1 170 isotropic chemical shifts ( 5cs), quadrupolar products (Pq), quadrupolar coupling constants (Cq), asymmetries (?)), relative populations, and tentative assignments of the oxygen species a variety of silicate minerals 1534 High Resolution NMR of Carrageenans Table 1 Chemical shifts (ppm) of the a-anomeric protons of carrageenans referred to DSS as internal Standard at 0 ppma 1584 Table 2 13C NMR chemical shifts for the most common carrageenan structural unitsa 1586 Table 3 NMR chemical shifts for minor components and additives observed in carrageenan samples . 1586 High-Resolution 13C Nuclear Magnetic Resonance in the Study of Oils Table 1 Quantitative 13C NMR determinations on oils 1616 High-Resolution 1H Nuclear Magnetic Resonance in the Study of Oils Table 1 Calculations of fatty arid composition of oils by signal intensities in the aH NMR spectrum . 1624 Table 2 Chemical shift assignment of the selected resonances used for geographical origin discrimination of olive oils according to Ref. [31] 1628 SNIF-NMR—Part 2: Isotope Ratios as Tracers of Chemical and Biochemical Mechanistic Pathways Table 1 Site-specific unit fractionation factors, a, and thermodynamic isotope effects, ae, for liquid-vapor phase transition of methanol and ethanoL The 13C parameters are determined by isotope ratio mass spectrometry (IRMS) on the same distillate samples as those used in the hydrogen SNIF-NMR measurements 1638 Table 2 Isotopic redistribution coefficients, O/,, relating reactants (water, W, and sites 1-6 of glucose) and products (water, W, and sites I—methyl and II—methylene of ethanoL) in a fermentation reaction carried out with maize glucose and tap water [43]. The coefficients °I3/ °I4/ °B °m. "112/ Oii3/ °H5z and aus are close to zero and a small connection between site II of ethanol and site 4 of glucose is detected. Slightly different values have been measured in other series of experiments 1643 SNIF-NMR—Part 3: From Mechanistic Affiliation to Origin Inference Table 1 Site-specific hydrogen isotope ratios, (O/W), in ppm, of geraniol and ct-pinene 1648 SNIF-NMR—Part 4: Applications in an Economic Context: The Example of Wines, Spirits, and Juices TabLe 1 Conditions limiting the enrichment of musts in different regions A, B, and C. f% and c% are expressed in v/v of ethanol in wine and values into brackets correspond to red wines. For exampLe, zone A includes the 15 State Members but France, Greece, Portugal, and Spain, zone B is composed of the Northern and Central France, Austria, and the Baden region in Germany, and zones C include Southern France, Greece, Portugal, and Spain 1660 Table 2 Ranges of mean values exhibited by the isotopic ratios of ethanol samples obtained by fermenting different plant sugars, including grape, beet, and cane sugars. The carbon-13 deviation, S13C (%) (Part 1, Equation 5) has been measured by IRMS. (D/H)i (in ppm) is the isotope ratio of the methyl site of ethanol 1661 NMR Relaxation and Diffusion Studies of Horticultural Products Table 1 Comparison of theoretical and experimentalp, and o, in Equation (1) for apple parenchyma tissue 1701 Table 2 Summary of references to NMR studies of quality factors in the major types of fruit and vegetables 1702 Time-Domain NMR in Quality Control: Standard Applications in Food Table 1 Applications of TD-NMR for determination of moisture and oil 1720 Nuclear Magnetic Relaxation in Staren Systems Table 1 Proton relaxation data for D2O exchanged and saturated starch granules 1726 Magic Angle Spinning NMR of Flours and Doughs Table 1 Proton assignment of durum wheat flour lipid moieties (From ref. [6]) 1737 High-Resolution Solid-State NMR of Gluten and Dough Table 1 Resonances commonly resolved in proton MAS spectra of gluten, flour, and dough 1751 High-Resolution Solid-State NMR as an Analytical Tool to Study Plant Seeds Table 1 Assignment of 13C NMR SP/MAS spectrum of Pisum sativum 1758 Table 2 Assignment of 13C CP/MAS spectrum of Pisum sativum 1758 High-Resolution Solid-State NMR Spectroscopy of Starch Polysaccharides Table 1 Nuclear-spin interactions for 1H and 13C in a 9.4 T magnetic field 1763 Temperature Measurements by Magnetic Resonance Table 1 Sensitivity and aecuraey of the MRI parameters of water used to measure temperature in real and modelfood Systems (Taken from 2D slice images unless otherwise stated) 1804 ESR Spectroscopy for the Study of Oxidative Processes in Food and Beverages Table 1 ESR detection of radicals in dry foods 1841 Nuclear Magnetic Resonance Studies on the Glass Transition and Crystallization in Low Moisture Sugars Table 1 The frequency of perturbation associated with each experiment 1863 Table 2 Relaxation times for different carbons in the sucrose molecule, crystal (anhydrous) and glass (1-2% moisture), at ambient temperature (295-305 K). Anomeric data are for the F2 carbon of sucrose with no attached protons. The Gi anomeric carbon, having one attached proton, exhibits ring values. Typical or averaged values are shown where several carbons belong to one class. T{s in seconds, T\p's in milliseconds, Tc-h in microseconds 1865
any_adam_object	1
any_adam_object_boolean	1
building	Verbundindex
bvnumber	BV021482926
ctrlnum	(OCoLC)635043310 (DE-599)BVBBV021482926
format	Book
fullrecord	<?xml version="1.0" encoding="UTF-8"?><collection xmlns="http://www.loc.gov/MARC21/slim"><record><leader>01069nam a2200277 cc4500</leader><controlfield tag="001">BV021482926</controlfield><controlfield tag="003">DE-604</controlfield><controlfield tag="005">20070116 </controlfield><controlfield tag="007">t</controlfield><controlfield tag="008">060221s2006 gw ad\|\| \|\|\|\| 00\|\|\| eng d</controlfield><datafield tag="035" ind1=" " ind2=" "><subfield code="a">(OCoLC)635043310</subfield></datafield><datafield tag="035" ind1=" " ind2=" "><subfield code="a">(DE-599)BVBBV021482926</subfield></datafield><datafield tag="040" ind1=" " ind2=" "><subfield code="a">DE-604</subfield><subfield code="b">ger</subfield><subfield code="e">rakwb</subfield></datafield><datafield tag="041" ind1="0" ind2=" "><subfield code="a">eng</subfield></datafield><datafield tag="044" ind1=" " ind2=" "><subfield code="a">gw</subfield><subfield code="c">XA-DE-BE</subfield></datafield><datafield tag="049" ind1=" " ind2=" "><subfield code="a">DE-29</subfield><subfield code="a">DE-355</subfield><subfield code="a">DE-91G</subfield><subfield code="a">DE-19</subfield><subfield code="a">DE-11</subfield></datafield><datafield tag="245" ind1="1" ind2="0"><subfield code="a">Modern magnetic resonance</subfield><subfield code="n">3</subfield><subfield code="p">Applications in materials science and food science</subfield><subfield code="c">Graham A. Webb (ed.)</subfield></datafield><datafield tag="264" ind1=" " ind2="1"><subfield code="a">Berlin</subfield><subfield code="b">Springer</subfield><subfield code="c">2006</subfield></datafield><datafield tag="300" ind1=" " ind2=" "><subfield code="a">LV, LXXII, S. 1417 - 1927</subfield><subfield code="b">Ill., graph. Darst.</subfield></datafield><datafield tag="336" ind1=" " ind2=" "><subfield code="b">txt</subfield><subfield code="2">rdacontent</subfield></datafield><datafield tag="337" ind1=" " ind2=" "><subfield code="b">n</subfield><subfield code="2">rdamedia</subfield></datafield><datafield tag="338" ind1=" " ind2=" "><subfield code="b">nc</subfield><subfield code="2">rdacarrier</subfield></datafield><datafield tag="700" ind1="1" ind2=" "><subfield code="a">Webb, Graham A.</subfield><subfield code="e">Sonstige</subfield><subfield code="4">oth</subfield></datafield><datafield tag="773" ind1="0" ind2="8"><subfield code="w">(DE-604)BV021482869</subfield><subfield code="g">3</subfield></datafield><datafield tag="856" ind1="4" ind2="2"><subfield code="m">HBZ Datenaustausch</subfield><subfield code="q">application/pdf</subfield><subfield code="u">http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=014665296&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA</subfield><subfield code="3">Inhaltsverzeichnis</subfield></datafield><datafield tag="999" ind1=" " ind2=" "><subfield code="a">oai:aleph.bib-bvb.de:BVB01-014665296</subfield></datafield></record></collection>
id	DE-604.BV021482926
illustrated	Illustrated
index_date	2024-07-02T14:05:05Z
indexdate	2024-07-09T20:36:09Z
institution	BVB
language	English
oai_aleph_id	oai:aleph.bib-bvb.de:BVB01-014665296
oclc_num	635043310
open_access_boolean
owner	DE-29 DE-355 DE-BY-UBR DE-91G DE-BY-TUM DE-19 DE-BY-UBM DE-11
owner_facet	DE-29 DE-355 DE-BY-UBR DE-91G DE-BY-TUM DE-19 DE-BY-UBM DE-11
physical	LV, LXXII, S. 1417 - 1927 Ill., graph. Darst.
publishDate	2006
publishDateSearch	2006
publishDateSort	2006
publisher	Springer
record_format	marc
spelling	Modern magnetic resonance 3 Applications in materials science and food science Graham A. Webb (ed.) Berlin Springer 2006 LV, LXXII, S. 1417 - 1927 Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Webb, Graham A. Sonstige oth (DE-604)BV021482869 3 HBZ Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=014665296&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis
spellingShingle	Modern magnetic resonance
title	Modern magnetic resonance
title_auth	Modern magnetic resonance
title_exact_search	Modern magnetic resonance
title_exact_search_txtP	Modern magnetic resonance
title_full	Modern magnetic resonance 3 Applications in materials science and food science Graham A. Webb (ed.)
title_fullStr	Modern magnetic resonance 3 Applications in materials science and food science Graham A. Webb (ed.)
title_full_unstemmed	Modern magnetic resonance 3 Applications in materials science and food science Graham A. Webb (ed.)
title_short	Modern magnetic resonance
title_sort	modern magnetic resonance applications in materials science and food science
url	http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=014665296&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA
volume_link	(DE-604)BV021482869
work_keys_str_mv	AT webbgrahama modernmagneticresonance3

Verfügbarkeit

Es ist kein Print-Exemplar vorhanden.

Fernleihe Bestellen Achtung: Nicht im THWS-Bestand! Inhaltsverzeichnis

MARC

Datensatz im Suchindex

Es ist kein Print-Exemplar vorhanden.

Ähnliche Einträge