Hydrophilic Interaction Chromatography

BERNARD A. OLSEN, PhD, has close to three decades of experience at Eli Lilly and Company in chemistry, manufacturing, and control of drug substances and drug products. He contributed to the development and support of more than twenty-five commercialized drugs as well as numerous developmental drugs. A Fellow of the American Association of Pharmaceutical Scientists, Dr. Olsen currently provides consulting and training services to the pharmaceutical industry and serves as Chair of the USP Expert Committee on Monograph Development: Small Molecules 3.BRIAN W. PACK, PhD, is a Research Advisor in Analytical Sciences R&D at Eli Lilly and Company, where he has contributed to the development of many solid oral and parenteral dosage forms. He is recognized for his contributions to HPLC method development, raw material control strategies, genotoxic impurities, cleaning validation, and colorimetry. Dr. Pack has published on the topics of HILIC applications, Raman spectroscopy, mass spectrometry, dissolution, and cleaning verification.

• PREFACE xiiiCONTRIBUTORS xvCHAPTER 1 SEPARATION MECHANISMS IN HYDROPHILIC INTERACTION CHROMATOGRAPHY 1David V. McCalley1.1 Introduction 11.2 Historical Background: Recognition of the Contribution of Partition, Ion Exchange, and RP Interactions to the Retention Process 31.3 Recent Studies on the Contributory Mechanisms to HILIC Retention 71.4 Conclusions 38References 38CHAPTER 2 STATIONARY PHASES FOR HILIC 43Mohammed E.A. Ibrahim and Charles A. Lucy2.1 Introduction 432.2 HILIC Stationary Phases 442.3 Commercial HILIC Phases 612.4 Conclusions 77Acknowledgments 77References 77CHAPTER 3 HILIC METHOD DEVELOPMENT 87Yong Guo and Xiande Wang3.1 Introduction 873.2 General Method Development Considerations 883.3 HILIC Method Development 933.4 Detection for HILIC Methods 1043.5 Conclusions 107References 108CHAPTER 4 PHARMACEUTICAL APPLICATIONS OF HYDROPHILIC INTERACTION CHROMATOGRAPHY 111Bernard A. Olsen, Donald S. Risley, V. Scott Sharp, Brian W. Pack, and Michelle L. Lytle4.1 Introduction 1124.2 Determination of Counterions 1174.3 Main Component Methods 1294.4 Determination of Impurities 1354.5 Excipients 1464.6 Chiral Applications 1524.7 Conclusions 161References 161CHAPTER 5 HYDROPHILIC INTERACTION CHROMATOGRAPHY (HILIC) FOR DRUG DISCOVERY 169Alfonso Espada and Mark Strege5.1 Drug Discovery Model 1695.2 HILIC Applications for In Vitro Biology 1705.4 Practical Considerations 1865.5 Conclusions 187References 188CHAPTER 6 ADVANCES IN HYDROPHILIC INTERACTION CHROMATOGRAPHY (HILIC) FOR BIOCHEMICAL APPLICATIONS 195Fred Rabel and Bernard A. Olsen6.1 Introduction 1956.2 Carbohydrates 1966.2.1 Mono- and Disaccharides 1966.3 Nucleobases and Nucleosides 2036.4 Oligonucleotides 2056.5 Amino Acids and Peptides 2066.6 Proteins 2096.7 Phospholipids 2096.8 Conclusions 211References 212CHAPTER 7 HILIC-MS FOR TARGETED METABOLOMICS AND SMALL MOLECULE BIOANALYSIS 219Hien P. Nguyen, Heather D. Tippens, and Kevin A. Schug7.1 Introduction 2197.2 The Role of HILIC-MS in Targeted Metabolomics versus Other LC Modes 2217.3 Strategies for Method Development Based on Retention Behavior of Targeted Metabolites on HILIC Stationary Phases 2237.4 Summary 231Acknowledgments 232References 232CHAPTER 8 HILIC FOR FOOD, ENVIRONMENTAL, AND OTHER APPLICATIONS 239Michael A. Koupparis, Nikolaos C. Megoulas, and Aikaterini M. Gremilogianni8.1 Introduction 2398.2 Food Applications for HILIC 2408.3 Environmental and Other Applications of HILIC 2548.4 Conclusions 257References 259CHAPTER 9 THEORY AND PRACTICE OF TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY SEPARATIONS INVOLVING THE HILIC MODE OF SEPARATION 265Stephen R. Groskreutz and Dwight R. Stoll9.1 Fundamentals of Multidimensional Liquid Chromatography 2659.2 Complementarity of HILIC Selectivity to Other Separation Modes 2789.3 Instrumentation and Experimental Considerations 2789.4 Applications 2919.5 The Future of HILIC Separations in 2DLC 298References 298INDEX 307

“The well-balanced mixture with updated HILIC theory and detailed practical descriptions makes it a useful resource for scientists working in analytical chemistry, biochemistry, biotechnology, and bioinformatics, and a valuable resource for people in the analytical column industry.”  (Analytical and Bioanalytical Chemistry, 22 September 2013)