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Chemical Analysis: A Series of Monographs on Analytical Chem #177: Hydrophilic Interaction Chromatography: A Guide for Practitioners

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Chemical Analysis: A Series of Monographs on Analytical Chem #177: Hydrophilic Interaction Chromatography: A Guide for Practitioners Cover

 

Synopses & Reviews

Publisher Comments:

Discover how to use HILIC to analyze and better understand polar compounds

An increasingly popular analytical method, hydrophilic interaction chromatography (HILIC) has the ability to retain and separate polar compounds that are often difficult to analyze by reversed-phase high-performance liquid chromatography (HPLC) or other analytical methods. Offering a comprehensive review, this book enables readers to develop a fundamental understanding of how HILIC works and then apply that knowledge to develop and implement a variety of practical applications.

Hydrophilic Interaction Chromatography begins with discussions of HILIC retention mechanisms, stationary phases, and general method development. This sets the foundation for the book's extensive coverage of applications. The authors address unique separation challenges for bioanalytical, environmental, pharmaceutical, and biochemical applications. Moreover, there is a thorough discussion of HILIC in two-dimensional chromatography.

With contributions from leading analytical scientists who have extensive experience in HILIC as well as HPLC, Hydrophilic Interaction Chromatography serves as a practical guide for researchers, featuring:

  • Detailed examples of HILIC methods and development approaches
  • Thorough explanations of retention mechanisms and the impact of stationary phase and mobile phase properties on separations
  • Step-by-step guidance for developing efficient, sensitive, and robust HILIC methods
  • References to the primary literature at the end of each chapter

Hydrophilic Interaction Chromatography is written for scientists who use or develop analytical methods for the separation of polar compounds. In particular, these researchers will discover how HILIC can be used to analyze and better understand the composition of pharmaceutical, bioanalytical, biochemical, chemical, food, and environmental samples.

Synopsis:

This book provides background information, guidance for method development, and a discussion of applications in the field of hydrophilic interaction chromatography (HILIC.) The book serves as a valuable reference tool for scientists confronted with an analysis problem involving polar compounds to determine if HILIC would be a good choice to pursue and helps them in choosing initial experimental conditions.  The book gives a detailed description of the HILIC retention mechanisms and specific information regarding application areas spanning a wide range of industries.

Topics include: HILIC retention mechanisms, Stationary Phases for HILIC, HILIC Method Development, Pharmaceutical and Other Applications of HILIC, HILIC for Drug Discovery, HILIC in Two-Dimensional Separations

About the Author

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.

Table of Contents

Chapter 1.  Separation Mechanisms in Hydrophilic Interaction Chromatography

1.1  Introduction

1.2  Historical Background. Recognition of the contribution of partition, ion exchange and reversed-phase interactions to the retention process

1.3  Recent studies on the contributory mechanisms to HILIC retention

1.3.1 Overview

1.3.2 Contribution of adsorption and partition to HILIC separations

1.3.3 Further studies on the contribution of ionic retention in HILIC

1.3.3.1 Introduction

1.3.3.2 Mobile phase considerations for the separation of ionogenic compounds

1.3.3.3. Ionisation state of the column as a function of pH

1.3.3.4 Quantitation of ionic retention effects on different columns

1.3.4 Reversed-phase retention on bare silica

1.3.5 Electrostatic Repulsion Hydrophilic Interaction Chromatography (ERLIC)- a new separation mode in HILIC.

1.4 Conclusions

Chapter 2.  Stationary Phases for HILIC

2.1 Introduction

2.2 HILIC stationary phases

2.2.1 Underivatized silica

2.2.1.1 Totally porous silica particles 

2.2.1.2 Superficially porous (core shell) silica particles

2.2.1.3 Monolithic silica

2.2.1.4 Ethylene Bridged Hybrids (BEH)

2.2.2 Derivatized silica

2.2.2.1 Neutral derivatized silica

2.2.2.2 Zwitterionic derivatized silica

2.2.2.3 Positively charged derivatized silica

2.2.2.4 Negatively charged derivatized silica

2.2.3 Non-silica phases

2.2.3.1 Amino phases

2.2.3.2 Sulfonated S-DVB phases

2.3 Commercial HILIC phases

2.3.1 Efficiency comparison

2.3.2 Retention and selectivity comparisons

2.4 Conclusions

Chapter 3.  HILIC Method Development

3.1 Introduction

3.2 General method development considerations

3.2.1 Method objectives

3.2.2 Sample consideration

3.2.3 Systematic method development

3.3 Method development strategies

3.3.1 Systematic approach to column screening

3.3.2 Optimization of method parameters

3.3.2.1 Final column selection

3.3.2.2 Organic solvents

3.3.2.3 Mobile phase pH

3.3.2.4 Buffer types and concentration

3.3.2.5 Column temperature

3.3.2.6 Sample solvents

3.4 Detection for HILIC methods

3.4.1 Mass Spectrometry detector (MS)

3.4.2 Charged aerosol detector (CAD)

3.5 Conclusions

Chapter 4.  Pharmaceutical Applications of Hydrophilic Interaction Chromatography

4.1 Introduction

4.1.1 Definition of the problem

4.1.2 Selection of conditions

4.1.3 Validation of the method

4.1.4 General references

4.2 Determination of Counterions

4.2.1 Salt selection and options for counterion determination

4.2.2 Specific counterion analysis

4.2.3 Counterion screening with gradient elution

4.2.4 Suitable reference standards for counterion analysis

4.3 Main Component Methods

4.3.1 Potency/assay methods

4.3.2  Equipment cleaning verification assays

4.3.3 Dissolution methods

4.4 Determination of Impurities

4.4.1 Impurity screening and orthogonal separations

4.4.2 Impurity identification

4.4.3 Specific impurity determination

4.4.3.1 Pyrimidines, purines, nucleosides

4.4.3.2 Hydrazines with ethanol as weak solvent

4.4.3.3 Neutral and charged polar impurities in a drug substance

4.4.3.4 Polar basic compounds and impurities

4.4.4 Statistical design of experiments (DOE) for optimization

4.5 Excipients

4.5.1 Parenteral and solution formulations

4.5.2 Tablets, capsules and inhalation products

4.5.3 Sugars

4.5.4 Stabilizers and antioxidants

4.6 Chiral Applications

4.6.1 Chiral selectors and HILIC

4.6.1.1 Cyclodextrins

4.6.1.2 Macrocyclic antibiotics

4.6.1.3 Chiral crown ethers

4.6.1.4 Cyclofructans

4.6.2 Conclusions for chiral separations

4.7 Conclusions

Chapter 5.  Hydrophilic Interaction Chromatography (HILIC) for Drug Discovery

5.1 Drug Discovery Model

5.2 HILIC Applications for in vitro Biology

5.2.1 Biological screening and hit finding

5.2.1.1 Target selection and assay validation

5.2.1.2 High-throughput screening

5.2.2 New drug discovery strategies

5.3 HILIC Applications and Advances for Discovery Chemistry

5.3.1 Lead identification

5.3.2 Lead optimization

5.3.2.1 ADME profile

5.3.2.2 Biopharmaceutics

5.3.2.3   Chiral purity

5.3.3 Candidate selection

5.4 Practical Considerations

5.5 Conclusions

Chapter 6.  Advances in Hydrophilic Interaction Chromatography (HILIC) for Biochemical Applications

6.1  Introduction

6.2 Carbohydrates

6.2.1 Mono- and disaccharides

6.2.2  Oligosaccharides and polysaccharides

6.2.3  Glycans

6.2.3.1 Glycan and glycopeptide analysis

6.2.3.2 HILIC for sample enrichment

6.3 Nucleobases and Nucleosides

6.4 Oligonucleotides

6.5 Amino Acids and Peptides

6.6 Proteins

6.7 Phospholipids

6.8 Conclusions

Chapter 7.  HILIC-MS for Targeted Metabolomics and Small Molecule Bioanalysis

7.1 Introduction

7.2 The role of HILIC-MS in targeted metabolomics versus other LC modes

7.3 Strategies for method development based on retention behavior of targeted metabolites on HILIC stationary phases

7.3.1 Retention behavior of metabolites on HILIC stationary phases

7.3.2 Robustness, mobile phase compositions, and matrix effects

7.4 Summary

Chapter 8.  HILIC for Food, Environmental, and Other Applications

8.1 Introduction

8.2 Food applications for HILIC

8.2.1 Review of  HILIC analytical methods for food analysis

8.2.1.1 Sample preparation in HILIC methods applied to food matrices

8.2.1.2 HILIC methods applied to food matrices: chromatographic parameters and detection

8.2.2 Selected detailed examples of HILIC applications in food analysis

8.2.2.1 Melamine (MEL) and cyanuric acid (CYA)

8.2.2.2 Water soluble vitamins

8.2.2.3 Seafood and other toxins

8.3 Environmental and other applications of HILIC

8.3.1 Review of environmental applications based on the stages of method development

8.3.2 Selected detailed examples of environmental and other HILIC applications

8.3.2.1 Metals and their related organic compounds

8.3.2.2 Pharmaceutical compounds in aqueous environmental samples

8.3.2.3 Other applications

8.4 Conclusions

Chapter 9.  Theory and Practice of Two-Dimensional Liquid Chromatography Separations Involving the HILIC Mode of Separation

9.1 Fundamentals of multi-dimensional liquid chromatography

9.1.1 Scope

9.1.2 Potential advantages of two-dimensional separations over conventional separations

9.1.3 Modes of 2D separation

9.1.3.1 Offline fraction transfer

9.1.3.2 Online fraction transfer

9.1.3.3 Conceptual comparison of different 2D separation modes

9.1.4 Undersampling

9.1.5 Orthogonality

9.2 Complementarity of HILIC selectivity to other separation modes

9.3 Instrumentation and Experimental Considerations

9.3.1 Online versus offline 2DLC

9.3.1.1 Offline 2DLC

9.3.1.2 Online 2DLC

9.3.2 Dealing with solvent incompatibility

9.3.2.1 Partial mobile phase evaporation

9.3.2.2 Consideration of fraction transfer volume relative to the second dimension column volume

9.3.2.3 On-column focusing

9.3.3 Fast Separations

9.3.3.1 General considerations for fast LC separations

9.3.3.2 Fast HILIC separations

9.4 Applications

9.5 The future of HILIC separations in 2DLC

Product Details

ISBN:
9781118054178
Author:
Olsen, Bernard A.
Publisher:
Wiley
Author:
Pack, Brian W.
Subject:
Chemistry - Analytic
Subject:
Chromatography / Separation Techniques
Subject:
p
Subject:
HILIC, hydrophilic interaction chromatography, polar compound analysis, bioanalytical, pharmaceutical analysis, glycans, glycomics, metabolomics, food analysis, environmental analysis, multidimensional chromatography, HPLC
Subject:
HILIC, hydrophilic interaction chromatography, polar compound analysis, bioanalytical, pharmaceutical analysis, glycans, glycomics, metabolomics, food analysis, environmental analysis, multid
Subject:
imensional chromatography, HPLC
Copyright:
Edition Description:
WOL online Book (not BRO)
Series:
Chemical Analysis: A Series of Monographs on Analytical Chemistry and Its Applications
Series Volume:
177
Publication Date:
20130226
Binding:
HARDCOVER
Language:
English
Pages:
336
Dimensions:
226 x 173 x 24.9 mm 20.896 oz

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Chemical Analysis: A Series of Monographs on Analytical Chem #177: Hydrophilic Interaction Chromatography: A Guide for Practitioners New Hardcover
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Product details 336 pages John Wiley & Sons - English 9781118054178 Reviews:
"Synopsis" by , This book provides background information, guidance for method development, and a discussion of applications in the field of hydrophilic interaction chromatography (HILIC.) The book serves as a valuable reference tool for scientists confronted with an analysis problem involving polar compounds to determine if HILIC would be a good choice to pursue and helps them in choosing initial experimental conditions.  The book gives a detailed description of the HILIC retention mechanisms and specific information regarding application areas spanning a wide range of industries.

Topics include: HILIC retention mechanisms, Stationary Phases for HILIC, HILIC Method Development, Pharmaceutical and Other Applications of HILIC, HILIC for Drug Discovery, HILIC in Two-Dimensional Separations

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