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. The much-anticipated second edition 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. This edition features
methods to quantify concentration and assess purity of isolated
metabolites on the micro scale and incorporates computational
approaches to accelerate the structure elucidation process. The
author also includes implementation and application of qNMR and
automated and practical use of computational chemistry combined
with QM and DFT to predict highly accurate NMR chemical shifts. 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 structural characterization 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.
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