In Vivo NMR Spectroscopy 2nd Edition Principles and Techniques. ROBIN A. DE GRAAF Yale University, Connecticut, USA
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1 In Vivo NMR Spectroscopy 2nd Edition Principles and Techniques ROBIN A. DE GRAAF Yale University, Connecticut, USA
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3 In Vivo NMR Spectroscopy 2nd Edition
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5 In Vivo NMR Spectroscopy 2nd Edition Principles and Techniques ROBIN A. DE GRAAF Yale University, Connecticut, USA
6 Copyright C 2007 John Wiley & Sons Ltd, The Atrium, Southern Gate, Chichester, West Sussex PO19 8SQ, England Telephone (+44) (for orders and customer service enquiries): cs-books@wiley.co.uk Visit our Home Page on or All Rights Reserved. No part of this publication may be reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning or otherwise, except under the terms of the Copyright, Designs and Patents Act 1988 or under the terms of a licence issued by the Copyright Licensing Agency Ltd, 90 Tottenham Court Road, London W1T 4LP, UK, without the permission in writing of the Publisher. Requests to the Publisher should be addressed to the Permissions Department, John Wiley & Sons Ltd, The Atrium, Southern Gate, Chichester, West Sussex PO19 8SQ, England, or ed to permreq@wiley.co.uk, or faxed to (+44) Designations used by companies to distinguish their products are often claimed as trademarks. All brand names and product names used in this book are trade names, service marks, trademarks or registered trademarks of their respective owners. The Publisher is not associated with any product or vendor mentioned in this book. This publication is designed to provide accurate and authoritative information in regard to the subject matter covered. It is sold on the understanding that the Publisher is not engaged in rendering professional services. If professional advice or other expert assistance is required, the services of a competent professional should be sought. The Publisher and the Author make no representations or warranties with respect to the accuracy or completeness of the contents of this work and specifically disclaim all warranties, including without limitation any implied warranties of fitness for a particular purpose. The advice and strategies contained herein may not be suitable for every situation. In view of ongoing research, equipment modifications, changes in governmental regulations, and the constant flow of information relating to the use of experimental reagents, equipment, and devices, the reader is urged to review and evaluate the information provided in the package insert or instructions for each chemical, piece of equipment, reagent, or device for, among other things, any changes in the instructions or indication of usage and for added warnings and precautions. The fact that an organization or Website is referred to in this work as a citation and/or a potential source of further information does not mean that the author or the publisher endorses the information the organization or Website may provide or recommendations it may make. Further, readers should be aware that Internet Websites listed in this work may have changed or disappeared between when this work was written and when it is read. No warranty may be created or extended by any promotional statements for this work. Neither the Publisher nor the Author shall be liable for any damages arising herefrom. Other Wiley Editorial Offices John Wiley & Sons Ltd, 111 River Street, Hoboken, NJ 07030, USA Jossey-Bass, 989 Market Street, San Francisco, CA , USA Wiley-VCH Verlag GmbH, Boschstr. 12, D Weinheim, Germany John Wiley & Sons Australia Ltd, 42 McDougall Street, Milton, Queensland 4064, Australia John Wiley & Sons (Asia) Pte Ltd, 2 Clementi Loop #02-01, Jin Xing Distripark, Singapore John Wiley & Sons Ltd, 6045 Freemont Blvd, Mississauga, Ontario L5R 4J3, Canada Wiley also publishes its books in a variety of electronic formats. Some content that appears in print may not be available in electronic books. Anniversary Logo Design: Richard J. Pacifico Library of Congress Cataloging-in-Publication Data De Graaf, Robin A. In vivo NMR spectroscopy : principles and techniques / Robin de Graaf. 2nd ed. p.;cm. Includes bibliographical references and index. ISBN (cloth : alk. paper) 1. Nuclear magnetic resonance spectroscopy. 2. Magnetic resonance imaging. I. Title. [DNLM: 1. Magnetic Resonance Spectroscopy diagnostic use. 2. Magnetic Resonance Spectroscopy methods. QU 25 D321i 2007] QP519.9.N83D dc British Library Cataloguing in Publication Data A catalogue record for this book is available from the British Library ISBN Typeset in 10/12pt Times by Aptara Inc., New Delhi, India Printed and bound in Great Britain by Antony Rowe Ltd, Chippenham, Wiltshire This book is printed on acid-free paper responsibly manufactured from sustainable forestry in which at least two trees are planted for each one used for paper production.
7 Contents Preface List of Abbreviations and Symbols xiii xv 1 Basic Principles Introduction Classical Description Quantum Mechanical Description Macroscopic Magnetization Excitation Bloch Equations Fourier Transform NMR Chemical Shift Digital Fourier Transform NMR Multi-scan Principle Time-domain Filtering Analog-To-Digital Conversion Zero Filling Spin spin Coupling Spectral Characteristics T 1 Relaxation T 2 Relaxation and Spin-echoes Exercises 38 References 41 2 In Vivo NMR Spectroscopy Static Aspects Introduction Proton NMR Spectroscopy Acetate (Ace) N-Acetyl Aspartate (NAA) 45
8 vi Contents N-Acetyl Aspartyl Glutamate (NAAG) Adenosine Triphosphate (ATP) Alanine (Ala) γ-aminobutyric Acid (GABA) Ascorbic Acid (Asc) Aspartate (Asp) Choline-containing Compounds (tcho) Creatine (Cr) and Phosphocreatine (PCr) Ethanolamine and Phosphorylethanolamine (PE) Glucose (Glc) Glutamate (Glu) Glutamine (Gln) Glutathione (GSH) Glycerol Glycine Glycogen Histamine Histidine Homocarnosine β-hydroxybutyrate (BHB) Myo-Inositol (mi) and scyllo-inositol (si) Lactate (Lac) Macromolecules Phenylalanine Pyruvate Serine Succinate Taurine (Tau) Threonine (Thr) Tryptophan (Trp) Tyrosine (Tyr) Valine (Val) Water Intra- and Extramyocellular Lipids (IMCL and EMCL) Deoxymyoglobin (DMb) Citric Acid Carnosine Phosphorus-31 NMR Spectroscopy Identification of Resonances Intracellular ph Carbon-13 NMR Spectroscopy Identification of Resonances Sodium-23 and Potassium-39 NMR Spectroscopy Fluorine-19 NMR Spectroscopy Identification of Resonances 89
9 Contents vii Fluorinated Drugs, Anaesthetics, and Fluorodeoxyglucose Metabolism Fluorinated Probes Exercises 93 References 95 3 In Vivo NMR Spectroscopy Dynamic Aspects Introduction Relaxation General Principles of Dipolar Relaxation Nuclear Overhauser Effect Alternative Relaxation Mechanisms In Vivo Relaxation Magnetization Transfer Creatine Kinase Inversion Transfer Saturation Transfer ATpases Fast Magnetization Transfer Methods Off-resonance Magnetization Transfer Chemical Exchange Dependent Saturation Transfer Diffusion Principles of Diffusion Diffusion and NMR Anisotropic Diffusion Restricted Diffusion Dynamic Carbon-13 NMR Spectroscopy General Set-up Metabolic Modeling Substrates Applications Hyperpolarization Brute Force Hyperpolarization Optical Pumping of Noble Gases Para-hydrogen-induced Polarization (PHIP) Dynamic Nuclear Polarization Exercises 179 References Magnetic Resonance Imaging Introduction Magnetic Field Gradients Slice Selection Frequency Encoding Phase Encoding 201
10 viii Contents 4.6 Spatial Frequency Space Fast MRI Sequences Echo-planar Imaging Contrast in MRI T 1 and T 2 Relaxation Mapping Fast T 1 and T 2 Relaxation Mapping Magnetic Field B 0 Mapping Magnetic Field B 1 Mapping Alternative Image Contrast Mechanisms Functional Imaging Parallel MRI Exercises 225 References Radiofrequency Pulses Introduction Square RF Pulses Selective RF Pulses Sinc Pulses Gaussian and Hermitian Pulses Multifrequency RF Pulses Pulse Optimization Shinnar Le Roux Algorithm DANTE RF Pulses Composite RF Pulses Adiabatic RF Pulses Rotating Frames of Reference Adiabatic Half and Full Passage Pulses Plane Rotations and Refocused Component Adiabatic Full Passage Refocusing Adiabatic Plane Rotation Pulses Variable Angle Adiabatic Plane Rotation Pulse, BIR Modulation Functions Offset-independent Adiabaticity Pulse Imperfections and Relaxation Power Deposition Multidimensional RF Pulses Spectral spatial RF Pulses Exercises 290 References Single Volume Localization and Water Suppression Introduction Single Volume Localization Image Selected In Vivo Spectroscopy (ISIS) Chemical Shift Displacement 302
11 Contents ix Stimulated Echo Acquisition Mode (STEAM) Point Resolved Spectroscopy (PRESS) Signal Dephasing with Magnetic Field Gradients Effects of Imperfect RF Pulses Localization by Adiabatic Selective Refocusing (LASER) Chemical Shift Displacement Scalar-coupled Spins Water Suppression Binomial and Related Pulse Sequences Frequency Selective Excitation Frequency Selective Refocusing Relaxation Based Methods Non-water-suppressed NMR Spectroscopy Exercises 341 References Spectroscopic Imaging and Multivolume Localization Introduction Principles of Spectroscopic Imaging Spatial Resolution in MRSI Temporal Resolution in MRSI Conventional Methods Methods Based on Fast MRI Sequences Methods Based on Prior Knowledge Lipid Suppression Relaxation Based Methods Outer Volume Suppression and Volume Pre-localization Methods Utilizing Spatial Prior Knowledge Spectroscopic Imaging Processing and Display Multivolume Localization Hadamard Localization Sequential Multivolume Localization Exercises 382 References Spectral Editing and Two-dimensional NMR Introduction Scalar Evolution J-difference Editing Practical Considerations of J-difference Editing Multiple Quantum Coherence Editing Heteronuclear Spectral Editing Polarization Transfer INEPT and DEPT Sensitivity Broadband Decoupling 416
12 x Contents 8.10 Two-dimensional NMR Spectroscopy Correlation Spectroscopy (COSY) Spin-echo or J-resolved NMR Two-dimensional Exchange Spectroscopy Exercises 438 References Spectral Quantification Introduction Data Acquisition Data Pre-processing Phasing and Frequency Alignment Lineshape Correction Removal of Residual Water Baseline Correction Data Quantification Time- and Frequency-domain Parameters Prior Knowledge Spectral Fitting Algorithms Error Estimation Data Calibration Internal Concentration Reference External Concentration Reference Phantom Replacement External Concentration Reference Exercises 473 References Hardware Introduction Magnets Magnetic Field Homogeneity Origins and Effects of Magnetic Field Inhomogeneity In Vivo Active Shimming Shimming Hardware Manual Shimming Magnetic Field Map Based Shimming Projection Based Shimming Dynamic Shim Updating (DSU) Passive Shimming Magnetic Field Gradients Eddy Currents Pre-Emphasis Active Shielding 512
13 Contents xi 10.5 Radiofrequency Coils Resonant LCR Circuits RF Coil Performance Spatial Field Properties Principle of Reciprocity I Principle of Reciprocity II Radiofrequency Coil Types Combined Transmit and Receive RF Coils Phased-array Coils H-[ 13 C] and 13 C-[ 1 H] RF Coils Cooled (Superconducting) RF Coils Complete MR System RF Transmission Signal Reception Quadrature Detection Dynamic Range Gradient and Shim Systems Exercises 542 References 545 Appendix 549 A1 Matrix Calculations 549 A2 Trigonometric Equations 551 A3 Fourier Transformation 551 A3.1 Introduction 552 A3.2 Properties 553 A3.3 Discrete Fourier Transformation 554 A4 Product Operator Formalism 554 A4.1 Cartesian Product Operators 555 A4.2 Spherical Tensor Product Operators 556 References 559 Further Reading 560 Index 563
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15 Preface Since the first edition of this textbook, published in 1998, the field of in vivo NMR spectroscopy has seen continued development of new techniques and applications, while at the same time some of the older techniques have become obsolete. One of the driving forces to write a second edition was to review some of these novel developments, such as hyperpolarized NMR, dynamic 13 C NMR, automated shimming and parallel acquisitions. To maintain the flow of the book, several of the older techniques that have limited merits in modern in vivo NMR were removed. A second driving force was provided by the need for a textbook to be used in conjunction with a teaching course on in vivo NMR. In order to pursue this objective, most techniques are described from an educational point of view, without losing the practical aspects appreciated by experimental NMR spectroscopists. Furthermore, each chapter is concluded with a number of exercises designed to review, but often also to extend, the presented NMR principles and techniques. Many of the ideas and changes that formed the basis for this second edition came from numerous discussions with colleagues. I would like to thank Douglas Rothman, Terry Nixon, Graeme Mason, Kevin Behar, Peter Brown and Kevin Koch for many fruitful discussions. Special thanks go to Christoph Juchem for his many insightful comments and careful reading of all chapters. Finally, I would like to acknowledge the contributions of original data from Dan Green and Simon Pittard (Magnex Scientific), Andrew Maudsley (University of Miami), Gerald Shulman (Yale University) and Graeme Mason (Yale University). Companion website URL: Robin A. de Graaf New Haven, USA January, 2007
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