Lc-nmr: Expanding The Limits Of Structure Elucidation by Nina C. GonnellaLc-nmr: Expanding The Limits Of Structure Elucidation by Nina C. Gonnella

Lc-nmr: Expanding The Limits Of Structure Elucidation

byNina C. GonnellaEditorNina C. Gonnella

Hardcover | March 15, 2013

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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 Elucidationpresents 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.

Nina C. Gonnella, Ph.D., is a senior research fellow at Boehringer Ingelheim. She heads the NMR group (consisting of solution, solid-state, and LC-NMR capability) and shares co-responsibility for the single-crystal x-ray facility. She also manages the open-access NMR facility for all of the chemical development, providing training and ...
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Title:Lc-nmr: Expanding The Limits Of Structure ElucidationFormat:HardcoverDimensions:301 pages, 9.25 × 6.14 × 0.98 inPublished:March 15, 2013Publisher:Crc Press LlcLanguage:English

The following ISBNs are associated with this title:

ISBN - 10:1439875065

ISBN - 13:9781439875063

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Table of Contents

Introduction to LC-NMR
Historical Review
Flow and NMR
Setting Up the LC-NMR System
Solvent Requirements in LC-NMR
Solvent Suppression and Referencing
The Deuterium Lock
The Solvent-Gradient Ramp
Diffusion
Shimming
Acquisition Parameters
Chemical-Shift Tracking
Other Considerations
Sources of Error
Summary
References

NMR Theory
Magnetic Properties of Nuclei
Data Acquisition
Relaxation of Nuclei
The Chemical Shift
Spin Coupling
Nuclear Overhauser Effect (NOE)
Coupling of HPLC with NMR
References

Separation Methods
Modes of Separation
General Method Development Strategies
Column Packing Types
Detector Selection
RPC Method Development and Compatibility with NMR
Integration of CE and NMR
Transitioning from Analytical to Preparative Chromatography
General Considerations
References

NMR Instrumentation and Probe Technologies
Instrumentation Configuration
The Magnet
Room Temperature Flow Probe
Microcapillary Probes (Room Temperature)
Cryogenically Cooled Probes
Probe Coil Geometries
Probe Sensitivity Comparison
References

NMR-Associated Isolation Technologies
Stopped Flow
Loop Collector
Solid-Phase Extraction (SPE)
Nonchromatographic Flow NMR
Direct-Injection NMR (DI-NMR)
Capillary Electrophoresis and NMR
References

NMR Experiments
Solvent Suppression
Structure Elucidation Experiments
NOE Experiments
References

Applications
Degradation Products
Impurities
Trace Analysis
Analysis of Mixtures
Tautomer Kinetics
Unstable Products
Metabolites
CE Isolates
Natural Products
Proteins/Peptides
References

Other Specialized-Flow NMR
NMR and Parallel Detection
Data Processing and Deconvolution of Parallel Data
Parallel Probe Construction
Microprobes
Advancements in Multiple-Coil Probe Design
Biological Screening and Flow NMR
NMR and Microreactors
Signal-to-Noise Ratio (Microcoils)
Microprobe Design (Microcoil/Microslot/Microstrip)
Future Directions
Summary
References

Glossary

Index

Editorial Reviews

"In a very practical way, the book describes the fundamentals and applications of LC-NMR hyphenation ¿ the book also paves the way for relative novices to gain experience, as it provides very practical tips about using different methods such as continuous flow, stopped flow, and storage modes. Choosing the right solvent, solvent requirements, diffusion effects, shimming issues, chemical shift variations in LC-NMR, and many other effects are discussed and solutions to such problems are given."¿U. Holzgrabe, Institut f¿r Pharmazie und Lebensmittelchemie, Universit¿W¿rzburg, Germany in Analytical and Bioanalytical Chemistry