Problems in Organic Structure Determination

A Practical Approach to NMR Spectroscopy

Author: Roger G. Linington,Philip G. Williams,John B. MacMillan

Publisher: CRC Press

ISBN: 1498719635

Category: Science

Page: 755

View: 868

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At a point where most introductory organic chemistry texts end, this problems-based workbook picks up the thread to lead students through a graduated set of 120 problems. With extensive detailed spectral data, it contains a variety of problems designed by renowned authors to develop proficiency in organic structure determination. This workbook leads you from basic problems encountered in introductory organic chemistry textbooks to highly complex natural product-based problems. It presents a concept-based learning platform, introducing key concepts sequentially and reinforcing them with problems that exemplify the complexities and underlying principles that govern each concept. The book is organized in such a way that allows you to work through the problems in order or in selections according to your experience and desired area of mastery. It also provides access to raw data files online that can be downloaded and used for data manipulation using freeware or commercial software. With its problem-centered approach, integrated use of online and digital resources, and appendices that include notes and hints, Problems in Organic Structure Determination: A Practical Approach to NMR Spectroscopy is an outstanding resource for training students and professionals in structure determination.

Organic Structure Determination Using 2-D NMR Spectroscopy

A Problem-based Approach

Author: Jeffrey H. Simpson

Publisher: Academic Press

ISBN: 0123849705

Category: Science

Page: 574

View: 4691

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"The second edition of this book comes with a number of new figures, passages, and problems. Increasing the number of figures from 290 to 448 has necessarily added considerable length, weight, and, expense. It is my hope that the book has not lost any of its readability and accessibility. I firmly believe that most of the concepts needed to learn organic structure determination using nuclear magnetic resonance spectroscopy do not require an extensive mathematical background. It is my hope that the manner in which the material contained in this book is presented both reflects and validates this belief"--

NMR - From Spectra to Structures

An Experimental Approach

Author: Terence N. Mitchell,Burkhard Costisella

Publisher: Springer Science & Business Media

ISBN: 3540721967

Category: Science

Page: 207

View: 9197

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This practice-oriented textbook shows how to utilize the huge variety of NMR experiments available today in addition to standard experiments. Intended as a practical guide for students and laboratory personnel, it treats theoretical aspects only to the extent necessary to understand the experiments and to interpret the results. The book is significantly revised and expanded for the 2nd edition, and now includes the nuclei 1H/2H, 13C, 31P, 17O, 15N, 19F, 29Si, 77Se, 113Cd, 117Sn/119Sn, 195Pt, 207Pb and a new chapter on solid state NMR. An expanded set of 50 graded problems offers invaluable help for students, practitioners and laboratory personnel alike.

Organic Structure Analysis

Author: Phillip Crews,Jaime Rodríguez,Marcel Jaspars

Publisher: Oxford University Press, USA

ISBN: 9780195336047

Category: Medical

Page: 636

View: 9018

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The most up-to-date integrated spectroscopy text available, Organic Structure Analysis, Second Edition, is the only text that teaches students how to solve structures as they are solved in actual practice. Ideal for advanced undergraduate and graduate courses in organic structure analysis, organic structure identification, and organic spectroscopy, it emphasizes real applications--integrating theory as needed--and introduces students to the latest spectroscopic methods. An Instructor's Resource CD-ROM, which includes all of the figures from the text in electronic format and the solutions to all of the exercises and problems from the text (in an editable Word file format), is also available for adopting professors. Please contact your publisher sales representative. FEATURES * Focus on Structure: Opens with structural elements and then considers the characteristics, advantages, and disadvantages of spectroscopic methods. Includes coverage of the steps used in determining a molecular structure, the limitations to organic structure determination by spectroscopic methods, and an "Organic Structure Analyses Gone Bad" table (all unique to this text) * Practical Organization: Presents the most commonly used methods first, beginning with an overview of strategies, followed by the use of NMR, and then moving on to mass spectrometry, infrared, and ultraviolet * Innovative Real-World Problem-Solving Approach: Follows the actual information flow used by chemists to solve molecular structures, as opposed to the standard methods-based approach of other texts * Unique Chapter (12) Featuring 51 Structure-Solving Problems: Each problem emphasizes a different method; the problems increase in difficulty throughout the chapter, successively building on students' knowledge and requiring them to integrate multiple methods to identify molecules. NEW TO THE SECOND EDITION * Coverage of the Latest Instrumental and Computational Advances: Examines the use of modern instruments, data processing, and computer-assisted structure elucidation techniques * Updated and Expanded Treatment of NMR (Chapters 2-5): An extensively revised Chapter 5 discusses multi-pulse 1D and 2D NMR methods, 1D TOCSY and 1D NOESY sequences, and using NOESY and ROESY in determining relative stereochemistry and solution conformation. * Additional Coverage of Mass Spectrometry: A new chapter (7) expands the discussion of mass spectrometry to three chapters (6-8). Topics include cutting-edge MS instrumentation and new information on tandem MS techniques, combining NMR with MS, large-molecule MS, chemo-informatics, and more. * More Exercises and Improved Spectra: The second edition includes 25% more problems than the previous edition (279 total). In addition, many of the spectra, including all of those presented in Chapters 11 and 12, have been reprocessed or reacquired for greater clarity.

Nuclear Magnetic Resonance Spectroscopy

An Introduction to Principles, Applications, and Experimental Methods

Author: Joseph B. Lambert,Eugene P. Mazzola

Publisher: Prentice Hall

ISBN: 9780130890665

Category: Science

Page: 341

View: 3542

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This book offers complete coverage of classic (one-dimensional) NMR as well as up-to-date coverage of two-dimensional NMR and other modern methods. This book focuses on all aspects of NMR including classic methods, modern techniques, practical advice for execution of the NMR experiment, theory, and more. For practicing NMR spectroscopists who want a better understanding of their subject, professors who want a wider knowledge of NMR, preparative (synthetic) organic chemists in industry who want to have more information about how to prove the structures of the compounds they make, and analytical chemists in industry who actually carry out the experiments and want a better understanding of what they are doing.

Tables of Spectral Data for Structure Determination of Organic Compounds

Author: Ernö Pretsch,T. Clerc,J. Seibl,W. Simon

Publisher: Springer Science & Business Media

ISBN: 3662224550

Category: Science

Page: 318

View: 5004

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Although numerical data are, in principle, universal, the compilations presented in this book are extensively annotated and interleaved with text. This translation of the second German edition has been prepared to facilitate the use of this work, with all its valuable detail, by the large community of English-speaking scientists. Translation has also provided an opportunity to correct and revise the text, and to update the nomenclature. Fortunately, spectroscopic data and their relationship with structure do not change much with time so one can predict that this book will, for a long period of time, continue to be very useful to organic chemists involved in the identification of organic compounds or the elucidation of their structure. Klaus Biemann Cambridge, MA, April 1983 Preface to the First German Edition Making use of the information provided by various spectroscopic tech niques has become a matter of routine for the analytically oriented organic chemist. Those who have graduated recently received extensive training in these techniques as part of the curriculum while their older colleagues learned to use these methods by necessity. One can, therefore, assume that chemists are well versed in the proper choice of the methods suitable for the solution of a particular problem and to translate the experimental data into structural information.

Organic Structures from Spectra

Author: L. D. Field,S. Sternhell,J. R. Kalman

Publisher: John Wiley & Sons

ISBN: 1118325486

Category: Science

Page: 512

View: 1685

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The derivation of structural information from spectroscopic data is now an integral part of organic chemistry courses at all Universities. A critical part of any such course is a suitable set of problems to develop the student’s understanding of how structures are determined from spectra. Organic Structures from Spectra, Fifth Edition is a carefully chosen set of more than 280 structural problems employing the major modern spectroscopic techniques, a selection of 27 problems using 2D-NMR spectroscopy, more than 20 problems specifically dealing with the interpretation of spin-spin coupling in proton NMR spectra and 8 problems based on the quantitative analysis of mixtures using proton and carbon NMR spectroscopy. All of the problems are graded to develop and consolidate the student’s understanding of organic spectroscopy. The accompanying text is descriptive and only explains the underlying theory at a level which is sufficient to tackle the problems. The text includes condensed tables of characteristic spectral properties covering the frequently encountered functional groups. The examples themselves have been selected to include all important common structural features found in organic compounds and to emphasise connectivity arguments. Many of the compounds were synthesised specifically for this purpose. There are many more easy problems, to build confidence and demonstrate basic principles, than in other collections. The fifth edition of this popular textbook: • includes more than 250 new spectra and more than 25 completely new problems; • now incorporates an expanded suite of new problems dealing with the analysis of 2D NMR spectra (COSY, C H Correlation spectroscopy, HMBC, NOESY and TOCSY); • has been expanded and updated to reflect the new developments in NMR and to retire older techniques that are no longer in common use; • provides a set of problems dealing specifically with the quantitative analysis of mixtures using NMR spectroscopy; • features proton NMR spectra obtained at 200, 400 and 600 MHz and 13C NMR spectra include DEPT experiments as well as proton-coupled experiments; • contains 6 problems in the style of the experimental section of a research paper and two examples of fully worked solutions. Organic Structures from Spectra, Fifth Edition will prove invaluable for students of Chemistry, Pharmacy and Biochemistry taking a first course in Organic Chemistry. Contents Preface Introduction Ultraviolet Spectroscopy Infrared Spectroscopy Mass Spectrometry Nuclear Magnetic Resonance Spectroscopy 2DNMR Problems Index Reviews from earlier editions “Your book is becoming one of the “go to” books for teaching structure determination here in the States. Great work!” “…I would definitely state that this book is the most useful aid to basic organic spectroscopy teaching in existence and I would strongly recommend every instructor in this area to use it either as a source of examples or as a class textbook”. Magnetic Resonance in Chemistry “Over the past year I have trained many students using problems in your book - they initially find it as a task. But after doing 3-4 problems with all their brains activities... working out the rest of the problems become a mania. They get addicted to the problem solving and every time they solve a problem by themselves, their confident level also increases.” “I am teaching the fundamentals of Molecular Spectroscopy and your books represent excellent sources of spectroscopic problems for students.”

NMR Spectroscopy Explained

Simplified Theory, Applications and Examples for Organic Chemistry and Structural Biology

Author: Neil E. Jacobsen

Publisher: John Wiley & Sons

ISBN: 9780470173343

Category: Science

Page: 640

View: 7941

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NMR Spectroscopy Explained : Simplified Theory, Applications and Examples for Organic Chemistry and Structural Biology provides a fresh, practical guide to NMR for both students and practitioners, in a clearly written and non-mathematical format. It gives the reader an intermediate level theoretical basis for understanding laboratory applications, developing concepts gradually within the context of examples and useful experiments. Introduces students to modern NMR as applied to analysis of organic compounds. Presents material in a clear, conversational style that is appealing to students. Contains comprehensive coverage of how NMR experiments actually work. Combines basic ideas with practical implementation of the spectrometer. Provides an intermediate level theoretical basis for understanding laboratory experiments. Develops concepts gradually within the context of examples and useful experiments. Introduces the product operator formalism after introducing the simpler (but limited) vector model.

Understanding NMR Spectroscopy

Author: James Keeler

Publisher: John Wiley & Sons

ISBN: 1119964938

Category: Science

Page: 526

View: 4655

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This text is aimed at people who have some familiarity with high-resolution NMR and who wish to deepen their understanding of how NMR experiments actually ‘work’. This revised and updated edition takes the same approach as the highly-acclaimed first edition. The text concentrates on the description of commonly-used experiments and explains in detail the theory behind how such experiments work. The quantum mechanical tools needed to analyse pulse sequences are introduced set by step, but the approach is relatively informal with the emphasis on obtaining a good understanding of how the experiments actually work. The use of two-colour printing and a new larger format improves the readability of the text. In addition, a number of new topics have been introduced: How product operators can be extended to describe experiments in AX2 and AX3 spin systems, thus making it possible to discuss the important APT, INEPT and DEPT experiments often used in carbon-13 NMR. Spin system analysis i.e. how shifts and couplings can be extracted from strongly-coupled (second-order) spectra. How the presence of chemically equivalent spins leads to spectral features which are somewhat unusual and possibly misleading, even at high magnetic fields. A discussion of chemical exchange effects has been introduced in order to help with the explanation of transverse relaxation. The double-quantum spectroscopy of a three-spin system is now considered in more detail. Reviews of the First Edition “For anyone wishing to know what really goes on in their NMR experiments, I would highly recommend this book” – Chemistry World “…I warmly recommend for budding NMR spectroscopists, or others who wish to deepen their understanding of elementary NMR theory or theoretical tools” – Magnetic Resonance in Chemistry

Anthropic Awareness

The Human Aspects of Scientific Thinking in NMR Spectroscopy and Mass Spectrometry

Author: Csaba Szantay, Jr.

Publisher: Elsevier

ISBN: 0124199798

Category: Science

Page: 464

View: 7735

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Anthropic Awareness: The Human Aspects of Scientific Thinking in NMR Spectroscopy and Mass Spectrometry blends psychology, philosophy, physics, mathematics, and chemistry, describing a human-centered philosophy of the essence of scientific thinking in the natural sciences and in everyday life. It addresses the reasons why we are prone to make errors in our conclusions and how to avoid such mistakes, also exploring a number of the "mental traps" that can lead to both individual mistakes and mass misconceptions. The book advocates that by understanding the nature of these mental traps we can adopt tactics to safely evade them. It includes Illustrative examples of common scientific misunderstandings and mental traps in both the theory and real-life application of NMR spectroscopy and mass spectrometry. Provides strategies on how to deal with molecular challenges and instrument limitations Presents multiple applications of small molecule structure elucidation using NMR, MS, IR, and UV Explores critical topics, including anthropic awareness (AA), NMR Spectroscopy, mass spectrometry, scientific thinking, and more Includes tactics on how to Improve quality control and data interpretation skills while minimizing data analysis time and increasing confidence in results Presents coverage on tactics to optimize experimental NMR parameters and enhance NMR vocabulary

NMR Spectroscopy in Liquids and Solids

Author: Vladimir I. Bakhmutov

Publisher: CRC Press

ISBN: 148226272X

Category: Medical

Page: 360

View: 374

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NMR Spectroscopy in Liquids and Solids provides an introduction of the general concepts behind Nuclear Magnetic Resonance (NMR) and its applications, including how to perform adequate NMR experiments and interpret data collected in liquids and solids to characterize molecule systems in terms of their structure and dynamics. The book is composed of ten chapters. The first three chapters consider the theoretical basis of NMR spectroscopy, the theory of NMR relaxation, and the practice of relaxation measurements. The middle chapters discuss the general aspects of molecular dynamics and their relationships to NMR, NMR spectroscopy and relaxation studies in solutions, and special issues related to NMR in solutions. The remaining chapters introduce general principles and strategies involved in solid-state NMR studies, provide examples of applications of relaxation for the determination of molecular dynamics in diamagnetic solids, and discuss special issues related to solid state NMR— including NMR relaxation in paramagnetic solids. All chapters are accompanied by references and recommended literature for further reading. Many practical examples of multinuclear NMR and relaxation experiments and their interpretations are also presented. The book is ideal for scientists new to NMR, students, and investigators working in the areas of chemistry, biochemistry, biology, pharmaceutical sciences, or materials science.

Structure Elucidation in Organic Chemistry

The Search for the Right Tools

Author: Maria-Magdalena Cid,Jorge Bravo

Publisher: John Wiley & Sons

ISBN: 3527664637

Category: Science

Page: 552

View: 2687

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Intended for advanced readers, this is a review of all relevant techniques for structure analysis in one handy volume. As such, it provides the latest knowledge on spectroscopic and related techniques for chemical structure analysis, such as NMR, optical spectroscopy, mass spectrometry and X-ray crystallography, including the scope and limitation of each method. As a result, readers not only become acquainted with the techniques, but also the advantages of the synergy between them. This enables them to choose the correct analytical method for each problem, saving both time and resources. Special emphasis is placed on NMR and its application to absolute configuration determination and the analysis of molecular interactions. Adopting a practical point of view, the author team from academia and industry guarantees both solid methodology and applications essential for structure determination, equipping experts as well as newcomers with the tools to solve any structural problem.

High-resolution NMR Techniques in Organic Chemistry

Author: Timothy D. W. Claridge

Publisher: Newnes

ISBN: 0080546285

Category: Mathematics

Page: 383

View: 1631

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"Nuclear Magnetic Resonance (NMR) Spectroscopy remains the foremost analytical technique for the structure elucidation of organic molecules and an indispensable tool for the synthetic, medicinal and natural product chemist. New techniques continue to emerge and the application of NMR methods continues to expand. High-Resolution NMR Techniques in Organic Chemistry is designed for use in academic and industrial NMR facilities, as a text for graduate-level NMR courses, and as an accessible reference for the chemist's or spectroscopist's desk." --Book Jacket.

Basic One- and Two-Dimensional NMR Spectroscopy

Author: Horst Friebolin

Publisher: Wiley-VCH

ISBN: 9783527327829

Category: Science

Page: 442

View: 4659

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This is the fifth edition of the highly successful, classic textbook for bachelor and master courses, with over 20 % new material and the contents completely revised and updated. Using a minimum of mathematics, it explains the underlying theory of this most important spectroscopic technique in a thorough, yet readily understandable way, covering instrumentation and interpretation of the spectra. It presents all students need to know about 1D, 2D-NMR, solid state and dynamic NMR spectroscopy, as well as NMR imaging, all illustrated by examples for maximum clarity. All the sections include sub-chapters that focus on applications taken from organic, macromolecular, polymer and biochemistry. A must for students and lecturers in chemistry, biochemistry, pharmacy, and life sciences, as well as for spectroscopists.

Solving Problems with NMR Spectroscopy

Author: Atta-ur-Rahman,Muhammad Iqbal Choudhary,Atia-tul- Wahab

Publisher: Academic Press

ISBN: 0124116132

Category: Science

Page: 534

View: 5838

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Solving Problems with NMR Spectroscopy, Second Edition, is a fully updated and revised version of the best-selling book. This new edition still clearly presents the basic principles and applications of NMR spectroscopy with only as much math as is necessary. It shows how to solve chemical structures with NMR by giving many new, clear examples for readers to understand and try, with new solutions provided in the text. It also explains new developments and concepts in NMR spectroscopy, including sensitivity problems (hardware and software solutions) and an extension of the multidimensional coverage to 3D NMR. The book also includes a series of applications showing how NMR is used in real life to solve advanced problems beyond simple small-molecule chemical analysis. This new text enables organic chemistry students to choose the most appropriate NMR techniques to solve specific structures. The problems provided by the authors help readers understand the discussion more clearly and the solution and interpretation of spectra help readers become proficient in the application of important, modern 1D, 2D, and 3D NMR techniques to structural studies. Explains and presents the most important NMR techniques used for structural determinations Offers a unique problem-solving approach for readers to understand how to solve structure problems Uses questions and problems, including discussions of their solutions and interpretations, to help readers understand the fundamentals and applications of NMR Avoids use of extensive mathematical formulas and clearly explains how to implement NMR structure analysis Foreword by Nobel Prize winner Richard R. Ernst New to This Edition Key developments in the field of NMR spectroscopy since the First Edition in 1996 New chapter on sensitivity enhancement, a key driver of development in NMR spectroscopy New concepts such as Pulse Field Gradients, shaped pulses, and DOSY (Diffusion Order Spectroscopy) in relevant chapters More emphasis on practical aspects of NMR spectroscopy, such as the use of Shigemi tubes and various types of cryogenic probes Over 100 new problems and questions addressing the key concepts in NMR spectroscopy Improved figures and diagrams More than 180 example problems to solve, with detailed solutions provided at the end of each chapter

NMR Spectroscopy of the Non-Metallic Elements

Author: Stefan Berger,Siegmar Braun,Hans-Otto Kalinowski

Publisher: Wiley

ISBN: N.A

Category: Science

Page: 1098

View: 1960

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NMR Spectroscopy of the Non-Metallic Elements Stefan Berger Philipps-Universität, Marburg, Germany Siegmar Braun Technische Hochschule Darmstadt, Germany Hans-Otto Kalinowski Justus-Liebig-Universität, Gießen, Germany In recent years, the technique of Nuclear Magnetic Resonance (NMR) Spectroscopy has rapidly gained in importance outside its traditional areas of proton NMR and carbon-13 NMR. In particular, it has become much more applicable to compounds containing elements such as phosphorus, nitrogen and fluorine. NMR Spectroscopy of the Non-Metallic Elements gathers together a wealth of NMR data for the most important non-metallic elements, namely nitrogen, oxygen, fluorine, phosphorus, sulphur and xenon. For each element, the data for the simpler compounds and their derivatives (both organic and inorganic) are gathered together in as complete a form as possible, and the regularities that emerge are discussed in detail in relation to structural variations. This allows the reader to interpret the structure of more complex structures. The chapters containing the NMR data for the elements are preceded by a practical introduction to the basic theory and experimental techniques of the NMR parameters, especially the chemical shift and indirect spin-spin coupling. This material will help the reader both in finding practical solutions to problems of structure determination, and in critically evaluating the spectra obtained. NMR Spectroscopy of the Non-Metallic Elements is an invaluable reference source for all laboratories where NMR is used. It will also be widely used by organic and inorganic chemists, especially those working on nitrogen, fluorine and phosphorus compounds.

Nuclear Magnetic Resonance Spectroscopy

Author: Frank A. Bovey,Peter A. Mirau,H. S. Gutowsky

Publisher: Elsevier

ISBN: 0080916996

Category: Science

Page: 653

View: 4179

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Nuclear Magnetic Resonance Spectroscopy, Second Edition focuses on two-dimensional nuclear magnetic resonance (NMR) spectroscopy, high resolution NMR of solids, water suppression, multiple quantum spectroscopy, and NMR imaging. The selection first takes a look at the fundamental principles and experimental methods. Discussions focus on the NMR phenomenon, dipolar broadening and spin-spin relaxation, nuclear electric quadrupole relaxation, saturation, magnetic shielding and chemical shift, magnetic field, transitions between the nuclear energy levels, and resolution and sensitivity considerations. The manuscript then ponders on chemical shift, coupling of nuclear spins, and nuclear relaxation and chemical rate processes. Topics include spin lattice relaxation, spin-spin relaxation, spin decoupling and associated techniques, and description and analysis of spin systems. The text examines two-dimensional NMR spectroscopy, macromolecules, and NMR of solids, including magic angle spinning, cross polarization, proton dipolar broadening, biopolymers, and chain motion in macromolecules. The selection is a valuable source of data for readers interested in nuclear magnetic resonance spectroscopy.

NMR of Macromolecules

A Practical Approach

Author: Gordon C. K. Roberts

Publisher: Oxford University Press

ISBN: 0199632243

Category: Political Science

Page: 399

View: 9936

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The last 10-15 years have seen an enormous upsurge in the use of nuclear magnetic resonance (NMR) to study the conformation and interactions of biological macromolecules. NMR is now second in importance only to x-ray crystallography in structural molecular biology. As a result, more and more biologists are seeking to use NMR to solve their structural problems. There are several very good books which give an introduction to the theory of modern NMR spectroscopy, but much less is available on the practical side which is specifically tailored to the special technique required. The aim of this book is to provide the newcomer to these applications of NMR, whether a graduate student or a more senior biologist who wishes to apply NMR to his or her favourite protein, with practical guidance on how to choose the right experiment to obtain the desired information, how to carry out the experiment, and how to analyse the resulting spectra. Those who are familar with chemical applications of NMR but not those to biological macromolecules will also find this book helpful in describing the special requirements of NMR studies of these large molecules. One of the consequences of the considerable proliferation of papers describing the application of NMR to biological macromolecules has been the increasing reluctance of journals to provide space for a detailed description of the methods involved in, for example, resonance assignment or the analysis of NOEs for structure determination. This book will fill this gap, so as to allow the reader both to understand what is involved in the experiments described in the literature and to embark on the application of these powerful methods to his or her own system.

NMR Spectroscopy in Pharmaceutical Analysis

Author: Iwona Wawer,Bernd Diehl

Publisher: Elsevier

ISBN: 008095152X

Category: Science

Page: 528

View: 6177

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For almost a decade, quantitative NMR spectroscopy (qNMR) has been established as valuable tool in drug analysis. In all disciplines, i. e. drug identification, impurity profiling and assay, qNMR can be utilized. Separation techniques such as high performance liquid chromatography, gas chromatography, super fluid chromatography and capillary electrophoresis techniques, govern the purity evaluation of drugs. However, these techniques are not always able to solve the analytical problems often resulting in insufficient methods. Nevertheless such methods find their way into international pharmacopoeias. Thus, the aim of the book is to describe the possibilities of qNMR in pharmaceutical analysis. Beside the introduction to the physical fundamentals and techniques the principles of the application in drug analysis are described: quality evaluation of drugs, polymer characterization, natural products and corresponding reference compounds, metabolism, and solid phase NMR spectroscopy for the characterization drug substances, e.g. the water content, polymorphism, and drug formulations, e.g. tablets, powders. This part is accompanied by more special chapters dealing with representative examples. They give more detailed information by means of concrete examples. Combines theory, techniques, and concrete applications—all of which closely resemble the laboratory experience Considers international pharmacopoeias, addressing the concern for licensing Features the work of academics and researchers, appealing to a broad readership

LC-NMR

Expanding the Limits of Structure Elucidation

Author: Nina C. Gonnella

Publisher: CRC Press

ISBN: 1439875073

Category: Science

Page: 301

View: 7065

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The isolation and structural characterization of substances present at very low concentrations, as is necessary to satisfy regulatory requirements for pharmaceutical drug degradants and impurities, can present scientific challenges. The coupling of HPLC with NMR spectroscopy has been at the forefront of cutting-edge technologies to address these issues. LC-NMR: Expanding the Limits of Structure Elucidation presents a comprehensive overview of key concepts in HPLC and NMR that are required to achieve definitive structure elucidation with very low levels of analytes. Because skill sets from both of these highly established disciplines are involved in LC-NMR, the author provides introductory background to facilitate readers’ proficiency in both areas, including an entire chapter on NMR theory. This book provides guidance in setting up LC-NMR systems, discussion of LC methods that are compatible with NMR, and an update on recent hardware and software advances for system performance, such as improvements in magnet design, probe technology, and solvent suppression techniques that enable unprecedented mass sensitivity in NMR. It also describes numerous NMR collection strategies, including continuous flow, stop flow, solid phase extraction (SPE), loop collection, and capillary electrophoresis. In addition, the author presents an overview of NMR experiments and techniques used in structure elucidation. The text focuses on current developments in chromatographic-NMR integration, with particular emphasis on utility in the pharmaceutical industry. Applications include trace analysis, analysis of mixtures, and detection of degradation products, impurities, metabolites, peptides, and more. The text discusses novel uses and emerging technologies that challenge detection limits as well future directions for this important technique. This book is a practical primary resource for NMR structure determination—including theory and application—that guides the reader through the steps required for isolation and NMR structure elucidation on the micro scale.