[...]... Historical Development of LC-NMR, 904 20.3 LC-NMR, 905 20.3.1 Introduction, 905 20.3.2 Modes of Operation for LC-NMR, 908 20.3.3 Other Analytical Separation Techniques Hyphenated with NMR, 914 20.3.4 Applications of LC-NMR, 916 20.4 LC-MS-NMR (or LC-NMR-MS or LC-NMR/MS), 916 20.4.1 Introduction, 916 20.4.2 Modes of Operation for LC-MS-NMR, 917 20.4.3 Applications of LC-MS-NMR, 926 20.5 Conclusions,... high performance liquid chromatography (HPLC) , fast HPLC, automated method development, HPLC- MS (mass spectrometry), HPLC- NMR (nuclear magnetic resonance) and high-throughput purification methods This book is unique in the sense that it elucidates the role of HPLC throughout the entire drug development process from drug candidate inception to marketed drug product It is written in a manner that scientists. .. approaches for implementing HPLC, fast HPLC, and hyphenated HPLC techniques towards pharmaceutical analysis are discussed This book has the potential to serve as a useful resource for the chromatographic community It can be used as a handbook for the novice as well as the more experienced pharmaceutical chemist who utilizes HPLC as an analytical tool to solve challenging problems regularly in the pharmaceutical. .. Glycosylation and Phosphorylation, 860 19.3.3 Microwave-Assisted Methods for Proteins/Peptides, 871 19.3.4 Drug–Protein Interaction by Affinity-Based HPLC/ MS, 877 19.3.5 Multidimensional HPLC in Proteomics, 879 19.3.6 Characterization of Adenovirus Structural Proteins for Gene Therapy, 884 19.4 Conclusions, 890 Acknowledgment, 890 References, 890 20 LC-NMR Overview and Pharmaceutical Applications 901 Maria Victoria... of HPLC Methods, 507 10.3.1 Off-Line Optimization, 507 10.3.2 On-Line Optimization, 510 10.3.3 Method Screening, 511 10.3.4 Method Optimization, 512 10.4 Structure-Based Tools, 517 10.4.1 Knowledge Management, 517 10.4.2 Applications Databases, 519 10.4.3 Structure-Based Prediction, 521 10.5 Conclusion, 528 References, 529 PART II HPLC IN THE PHARMACEUTICAL INDUSTRY 533 11 The Expanding Role of HPLC. .. development is of HPLC for Pharmaceutical Scientists, Edited by Yuri Kazakevich and Rosario LoBrutto Copyright © 2007 by John Wiley & Sons, Inc 3 4 INTRODUCTION paramount importance throughout this drug development life cycle This requires a thorough understanding of HPLC principles and theory which lay a solid foundation for appreciating the many variables that are optimized during fast and effective HPLC method... [11] This was the origin of high-performance liquid chromatography (HPLC) , and the actual name for this separation method was introduced by Prof Horvath in 1970 at the Twenty-first Pittsburgh Conference in Cleveland, where he gave this title 8 INTRODUCTION Figure 1-3 Components of performance as defined by C Horvath (Reprinted from reference 12, with permission.) Figure 1-4 Separation of fatty acids on... Ruggedness/Robustness, 486 9.4.8 Specificity, 490 9.4.9 Forced Degradation Studies (Solid State and Solution)— Drug Substance and Drug Product, 491 9.5 Distinguishing Drug-Related and Non-Drug-Related Degradation Products, 495 9.5.1 Drug Product Stress, 497 9.6 Concluding Remarks, 499 References, 499 10 Computer-Assisted HPLC and Knowledge Management Yuri Kazakevich, Michael McBrien, and Rosario LoBrutto... Pharmaceuticals Corporation, East Hanover, NJ 07936 Anant Vailaya, Analytical Research, Merck Research Laboratories, Rahway, NJ 07065 Richard V Vivilecchia, Novartis Pharmaceuticals Corporation, East Hanover, NJ 07936 Li-Kang Zhang, Schering-Plough Research Institute, Kenilworth, NJ 07033 PART I HPLC THEORY AND PRACTICE 1 INTRODUCTION Yuri Kazakevich and Rosario LoBrutto 1.1 CHROMATOGRAPHY IN THE PHARMACEUTICAL. .. 542 11.6.1 Purity Assessment of Compound Libraries, 544 11.7 Purification Technologies for Drug Discovery, 547 11.7.1 UV-Directed Purification, 548 11.7.2 Mass-Directed Preparative Purification, 549 11.8 Higher-Throughput Purification Strategies, 552 11.8.1 Fluorous Split-Mix Library Synthesis and Prepartive LC/MS De-Mixing, 552 11.8.2 Parallel Analysis and Parallel Purification, 553 11.8.3 Streamlining . Cataloging-in-Publication Data: HPLC for pharmaceutical scientists / edited by Yuri Kazakevich, Rosario LoBrutto. p. cm. Includes bibliographical references and index. ISBN-13: 97 8-0 -4 7 1-6 816 2-5 (cloth) ISBN-10:. Applications of LC-NMR, 916 20.4 LC-MS-NMR (or LC-NMR-MS or LC-NMR/MS), 916 20.4.1 Introduction, 916 20.4.2 Modes of Operation for LC-MS-NMR, 917 20.4.3 Applications of LC-MS-NMR, 926 20.5 Conclusions,. 8 1.5.1 Modern HPLC Column, 9 1.5.2 HPLC System, 9 1.6 Types of HPLC, 10 1.6.1 Normal-Phase Chromatography (NP HPLC) , 10 1.6.2 Reversed-Phase HPLC (RP HPLC or RPLC), 11 1.6.3 Ion-Exchange Chromatography