Chapter
Chapter 2: Kinetic theories of liquid chromatography
2.2 Macroscopic Kinetic Theories
2.2.1 Lumped Kinetic Model
2.2.1.1 van Deemter plate height equation
2.2.2.1 General rate model for monolith columns
2.2.2.2 General rate model for core-shell particles
2.2.3 Lumped Pore Diffusion Model
2.2.4 Equivalence of the Macroscopic Kinetic Models
2.2.5 Kinetic Theory of Nonlinear Chromatography
2.3 Microscopic Kinetic Theories
2.3.1.1 Stochastic-dispersive model
2.3.2 Giddings Plate Height Equation
2.3.3 Monte Carlo Simulations of Nonlinear Chromatography
2.4 Comparison of the Microscopic and the Macroscopic Kinetic Models
Chapter 3: Column technology in liquid chromatography
3.2 Column Design and Hardware
3.2.1 Column History in Brief
3.2.3 Column Miniaturization
3.3 Column Packing Materials and Stationary Phases
3.3.2 Classification of LC Columns
3.3.3 Packing Materials [21]
3.3.3.1 Particle shape, size, and size distribution
3.3.3.2 Pore structure parameters
3.3.3.3 Surface functionalization of silica—the key to gaining selectivity
3.3.3.4 Surface functionalization of silica—the way to bonded silica columns
3.3.4 Major Synthesis Routes
3.3.4.1 Physicochemical characterization of bonded silica
3.3.4.2 Column packing procedures for analytical columns
3.3.4.3 Examples for selective bonded silica columns
3.3.4.4 The potential of multimodal or multifunctional bonded columns
3.4 Column Systems and Operations
3.4.1 Choice of Average Particle Size and Column Internal Diameter
3.4.3 Choice of Optimum-Flow Conditions
3.4.4 Column Back Pressure
3.4.5 Choice of Column Temperature
3.4.6 Column Capacity and Loadability
3.5 Chromatographic Column Testing and Evaluation
3.5.1 Chromatographic Testing
3.5.1.2 Silanophilic activity
3.5.1.3 Polar selectivity
3.5.1.4 Shape selectivity
3.6 Column Maintenance and Troubleshooting
3.6.1 Silica-Based Columns
3.6.1.1 General guidelines
3.6.3 Mechanical Stability
3.6.4 Mobile Phases (Eluents)
3.6.4.1 Proper storage of HPLC columns
3.6.4.2 Regeneration of a column
3.6.5 Regeneration of RP Packings
3.6.6 Polymer-Based Columns
3.6.6.1 General guidelines
3.6.7 Hydrophobic Unmodified Polystyrene-Divinylbenzene (Ps-Dvb)
3.6.8 Polymer-Based Ion-Exchangers
3.6.9 Regeneration of Polymer Materials
3.7 Today’s Column Market—an Evaluation, Comparison, and Critical Appraisal
3.7.1 Development During 2000–16
3.7.2 A Column Comparison
3.8 Conclusion: Where Do We Go Next? Science vs. Market
Chapter 4: Reversed-phase liquid chromatography
4.2.2 Exothermodynamic Relationships
4.2.3 Thermodynamic Considerations
4.3 System Considerations
4.3.2 Molecular Dynamics Simulations
4.4 Linear Free Energy Relationships
4.4.1 Solvation Parameter Model
4.4.1.1 Analysis of system constants
4.4.1.3 Steric resistance and shape selectivity
4.4.1.4 Electrostatic interactions
4.4.2 Hydrophobic-Subtraction Model
Chapter 5: Secondary chemical equilibria in reversed-phase liquid chromatography
5.2.1 Changes in Retention With pH
5.2.2 Buffers and Measurement of pH
5.3 Ion Interaction Chromatography
5.3.1 Retention Mechanism
5.3.2 Common Reagents and Operational Modes
5.3.3 Separation of Inorganic Anions
5.3.4 The Silanol Effect and Its Suppression With Amine Compounds
5.3.5 Use of Perfluorinated Carboxylate Anions and Chaotropic Ions as Additives
5.3.6 Use of ILs as Additives
5.3.7 Measurement of the Enhancement of Column Performance Using Additives
5.4 Micellar Liquid Chromatography
5.4.1 An Additional Secondary Equilibrium in the Mobile Phase
5.4.2 Hybrid Micellar Liquid Chromatography
5.4.3 Microemulsion Liquid Chromatography
5.5.1 Determination of Metal Ions
5.5.2 Determination of Organic Compounds
5.6 Use of Redox Reactions
Chapter 6: Hydrophilic interaction liquid chromatography
6.2.1 Thermodynamics of Adsorption
6.2.2 Adsorption Kinetics
6.3 Stationary and mobile phases commonly employed in HILIC
6.3.1.2 Chemically bonded phases
6.3.1.3 Ion exchange and zwitterionic stationary phase
6.3.1.4 Hydrophilic macromolecules bonded phases
6.3.1.5 Surface-confined ionic liquids stationary phases
Chapter 7: Hydrophobic interaction chromatography*
7.2 Hydrophobic Interactions and Retention Mechanisms in HIC
7.2.1 Hydrophobic Interactions
7.2.2 Retention Mechanisms in HIC
7.3 Parameters That Affect HIC
7.3.2.1 Type and concentration of salt
7.3.3 Biomolecules Hydrophobicity
7.4 Purification Strategies
7.5 Experimental Considerations
7.6 Recent Selected Applications
Chapter 8: Liquid-solid chromatography
8.2 Retention and Separation
8.2.1 The Retention Process (“Mechanism”)
8.2.2 Solute and Solvent Localization
8.3.1 Thin-Layer Chromatography
8.3.2 Selection of the Mobile Phase
8.3.3 Example of Method Development
8.4 Problems in the Use of Normal-Phase Chromatography
Chapter 9: Ion chromatography
9.2 Basic Principles and Separation Modes
9.2.1 Ion-Exchange Chromatography
9.2.2 Ion-Exclusion Chromatography
9.2.3 Chelation Ion Chromatography
9.2.4 Zwitterionic Ion Chromatography
9.2.5.1 Typical eluents for anion exchange
9.2.5.2 Typical eluents for cation exchange
9.3.1.1 Anion-exchange columns
9.3.1.2 Cation-exchange columns
9.3.3.1 Conductimetric detection
Nonsuppressed conductivity
9.3.3.2 Electrochemical detection
9.3.3.3 Spectroscopic detection
Postcolumn reaction detection
9.3.3.4 Mass spectrometry
9.4.1 Industrial Applications
9.4.2 Environmental Applications
Chapter 10: Size-exclusion chromatography
10.2 Historical Background
10.3.1 A Size-Exclusion Process
10.3.2 An Entropy-Controlled Process
10.3.3 An Equilibrium Process
10.4 Band Broadening in SEC
10.4.1 Extra-column effects
10.6 SEC Enters the Modern Era: The Determination of Absolute Molar Mass
10.6.1 Universal Calibration and Online Viscometry
10.7 Multidetector Separations, Physicochemical Characterization, 2D Techniques
Acknowledgment and Disclaimer
Chapter 11: Interaction polymer chromatography
11.2.1 Retention Mechanisms
11.2.2 Thermodynamics of Polymer Chromatography
11.2.3 Modes of Polymer Chromatography
11.2.4 Modeling of the Chromatographic Process
11.3 Individual IPC Techniques
11.3.1 Equipment and Chromatographic Media
11.3.3 Isocratic Techniques
11.3.3.1 Liquid chromatography at critical conditions
11.3.3.2 Barrier techniques
11.3.4 Gradient Techniques
11.3.4.1 Liquid adsorption chromatography
11.3.4.2 Gradient elution at CPA
11.3.4.3 Liquid precipitation chromatography
11.3.4.4 Temperature gradient interaction chromatography
Chapter 12: Affinity chromatography
12.2 Basic Components of Affinity Chromatography
12.3 Bioaffinity Chromatography
12.4 Immunoaffinity Chromatography
12.5 Dye-Ligand and Biomimetic Affinity Chromatography
12.6 Immobilized Metal-Ion Affinity Chromatography
12.7 Analytical Affinity Chromatography
12.8 Miscellaneous Methods and Newer Developments
Chapter 13: Solvent selection in liquid chromatography
13.2 Columns and Solvents in RPLC, NPLC, and HILIC
13.3 Assessment of the Elution Strength
13.3.1 The Hildebrand Solubility Parameter and Other Global Polarity Estimators
13.3.2 Global Polarity for Solvent Mixtures
13.3.3 Application Field of the Chromatographic Modes as Deduced From the Schoenmakers’ Rule
13.4 Isoeluotropic Mixtures
13.5 Solvent-Selectivity Triangles
13.5.1 The Snyder’s Solvent-Selectivity Triangle
13.5.2 Prediction of the Character of Solvent Mixtures
13.5.3 A Solvatochromic Solvent-Selectivity Triangle
13.5.4 Other Solvent Descriptors and Alternative Diagrams for Solvent Classification and Comparison
13.6 Practical Guidelines for Optimization of Mobile-Phase Composition
13.6.1 Selection of the Chromatographic Mode
13.6.2 Description of the Retention Using the Modifier Content as a Factor
13.6.3 Systematic Trial-and-Error Mobile-Phase Optimization for Isocratic Elution
13.6.4 Systematic Trial-and-Error Mobile-Phase Optimization for Gradient Elution
13.6.5 Computer-Assisted Interpretive Optimization
13.6.6 Use of Combined Mobile Phases or Gradients to Achieve Full Resolution
13.7 Additional Considerations for Solvent Selection
Chapter 14: Method development in liquid chromatography
14.3 A Structured Approach to Method Development
14.3.1 Column Plate Number, N: Term i of Eq. (14.1)
14.3.2 Retention Factor, k: Term ii of Eq. (14.1)
14.3.3 Selectivity, α: Term iii of Eq. (14.1)
14.4 Method Development in Practice
14.4.1 Resolution-Modeling Software
14.4.2 Priority of Column Screening
Chapter 15: Theory and practice of gradient elution liquid chromatography
15.2 The Effects of Experimental Conditions on Separation
15.2.1 Gradient and Isocratic Separation Compared
15.2.2 The Effect of Gradient Conditions
15.2.3 The Effect of Column Conditions
15.2.4 The Effect of Other Conditions on Selectivity
15.4 Problems Associated With Gradient Elution
Chapter 16: Comprehensive two-dimensional liquid chromatography
16.3 Instrumental Set-Up and Data Analysis
16.4 Novel Stationary Phases
16.5 Conclusions and Future Perspectives
Chapter 17: General instrumentation in HPLC*
17.2.1 Mobile Phase/Solvent Reservoir
17.2.2 Solvent Delivery System
17.2.3 Sample Introduction Device
17.2.5 Post-column Apparatus
17.2.6.1 UV/Vis absorbance detectors
17.2.6.2 Fluorescence detectors
17.2.6.3 Electrochemical detectors
17.2.6.4 Conductivity detectors
17.2.6.6 Mass spectrometry
17.2.7 Data Collection and Output
17.2.8 Post-detection Eluent Processing
17.2.9 Connective Tubing and Fittings
17.3 Related HPLC Techniques
Chapter 18: Advanced spectroscopic detectors for identification and quantification: Mass spectrometry
18.2 Ionization Methods Suitable for LC Coupling
18.2.1 Electrospray Ionization
18.2.2 Atmospheric-Pressure Chemical Ionization
18.2.3 Atmospheric Pressure Photonization
18.3 How to Increase Specificity of MS Data
18.3.1 Accurate Mass Measurements
18.4 Micro- and Nano-LC-MS
18.4.1 Classical Approach
18.4.2 Microfluidic Devices
18.5 Capillary Electrochromatography
18.5.1 Interfacing With MS
Chapter 19: Advanced IR and Raman detectors for identification and quantification
19.2 Off-Line Hyphenation
Chapter 20: Advanced spectroscopic detectors for identification and quantification: Nuclear magnetic resonance
20.2 Hyphenation of NMR with HPLC
20.3 Advances in NMR Sensitivity
20.3.5 High-Temperature Superconducting Coils
20.3.6 Sample Amounts Typically Analyzable According to the Probes and the Magnet Field
20.3.7 Strategies for Obtaining NMR Information from a Given LC Peak
20.4 Direct LC-NMR Hyphenation (On-flow/Stop-flow LC-NMR)
20.4.1 Direct LC-NMR Hyphenation (On-flow/Stop-flow LC-NMR)
20.4.2 Indirect LC-NMR Hyphenation (LC-SPE-NMR)
20.4.3 Microfractionation and At-line MicroNMR Analysis
20.4.4 Practical Considerations for NMR Detection on Microgram Amounts of Sample
20.5 Integration with a Multiple Detection System (LC-NMR-MS)
20.6 Quantification Capabilities
20.6.1 General Considerations on Quantitative NMR
20.6.2 Methods for Quantification in On-line and At-line LC-NMR
20.7 Fields of Application
20.7.1 Dereplication and Rapid De novo Identification of NPs in Complex Extracts
20.7.2 Analysis of Unstable Compounds
20.7.3 Metabolite Identification in Metabolomics
20.7.4 Metabolite Identification in Body Fluids
20.7.5 Identification of Pharmaceutical Impurities
Chapter 21: Data analysis
21.2 Univariate Detection and Zeroth-Order Calibration
21.3 Preprocessing: Baseline Correction, Peak Shift Alignment, Warping, and Normalization
21.3.1 Baseline Correction
21.3.2 Peak Alignment and Warping Methods
21.4 Univariate Detection and First-Order Calibration
21.5 Multivariate Detection and Second-Order Calibration
21.5.1 Why Second-Order Calibration?
21.5.2 Data and Algorithms
21.5.3 Recent Applications
21.6 Multivariate Detection and Third-Order Calibration
21.6.1 Third-Order Chromatographic Data Generation
21.6.2 Data and Algorithms
Chapter 22: Validation of liquid chromatographic methods
22.1.1 Traditional Method Validation
22.1.2 Enhanced Approaches
22.1.2.2 Technique selection and method development
22.1.2.3 Analytical method risk assessment
22.1.2.4 Develop understanding and identify operating conditions
22.1.2.5 Method validation
22.1.2.6 Method control strategy
22.1.2.7 Lifecycle management
Chapter 23: Quantitative structure property (retention) relationships in liquid chromatography
23.2 Methodology and Goals of QSRR Studies
23.2.1 Structural Descriptors
23.2.2 Retention Prediction
23.3 Applications of QSRR in Proteomics
23.4 Characterization of Stationary Phases
23.5 QSRR and Assessment of Lipophilicity of Xenobiotics
23.6 QSRR Analysis of Retention Data Determined on Immobilized-Biomacromolecule Stationary Phases
23.7 Quantitative Retention-(Biological) Activity Relationships
23.8 Chemometrically Processed Multivariate Chromatographic Data in Relation to Pharmacological Properties of Drugs and ...
Chapter 24: Modeling of preparative liquid chromatography
24.2.1 The Equilibrium-Dispersive Model
24.3.1 Band Shape Dependence on Adsorption
24.3.2 Adsorption Isotherms
24.3.2.1 The Langmuir adsorption isotherm
24.3.3 Determination of Adsorption Data
24.3.3.1 Frontal analysis
24.4 Process Optimization of Preparative Chromatography
24.4.1 Empirical Optimization
24.4.2 Numerical Optimization
24.4.2.1 General procedures
24.4.2.2 Numerical injection-volume optimization
24.4.2.3 Numerical full optimization
24.4.3 Important Operational Conditions
24.4.3.2 Injection profiles
24.4.3.3 Modeling additives
24.4.3.4 Modeling gradient elution
Chapter 25: Process concepts in preparative chromatography
25.2 Classical Isocratic Discontinuous Elution Chromatography
25.2.1 Mathematical Modeling and Typical Effects
25.3 Other Discontinuous Operating Concepts
25.3.1 Gradient Chromatography
25.3.2 Recycling Techniques
25.3.2.1 Closed-loop recycling chromatography
25.3.2.2 Steady-state recycling chromatography
25.4 Continuous Concepts of Preparative Chromatography
25.4.1 Multicolumn Countercurrent Concepts: SMB Chromatography
25.4.1.1 Improved operating concepts
25.4.2 Annular Chromatography
25.5 Optimization and Concept Comparison
Chapter 26: Miniaturization and microfluidics
26.2 Microfluidic Systems for Separations
26.2.1 Microfabrication Technologies
26.2.1.1 Photolithography and etching
26.2.1.2 Casting, molding, and hot embossing
26.2.1.3 Microcontact printing—stamping
26.2.1.4 Other techniques
26.2.1.5 Paper-based microfluidics
26.2.2 Miniaturization of HPLC Systems
26.3 Commercial Instrumentation
26.3.1 Electrophoretic Systems
Chapter 27: Nano-liquid chromatography
27.2 Features of Microfluidic Analytical Techniques
27.2.1 Improving Sensitivity Reducing the Chromatographic Dilution
27.2.2 Efficiency and Extra Column Band Broadening
27.3 SPS and Column Preparation
27.3.1 SPs Used in Nano-LC
27.3.2 Capillary Columns' Preparation
27.4.1 Microfluidic Pump Systems
27.4.2 Nano-volumes' Injection
27.4.4 Hyphenation of Nano-LC With Mass Spectrometry
27.5 Some Selected Applications
27.5.1 Proteins and Peptides Analysis
27.5.3 Environmental Analysis
27.5.4 Pharmaceutical Analysis
27.5.5 Clinical, Legal, and Forensic Analysis
Chapter 28: Capillary electrochromatography
28.2 Principles of Capillary Electrochromatography
28.3.2.1 Packed columns: particle-packed columns
28.3.2.2 Packed columns: in situ formed monolithic columns
28.3.2.3 Open-tubular columns
28.3.3.1 Mass spectrometry
28.4 Miniaturized Systems
Chapter 29: Ultra-high performance liquid chromatography
29.2.1 Chromatographic Performance
29.2.2 Frictional Heating
29.2.3 Method Translation From HPLC to UHPLC
29.3 Instrumentation for UHPLC
29.3.1 Instrumental Challenges
29.3.1.1 System pressure limit
29.3.1.2 Extra-column band broadening
29.3.1.3 System dwell volume
29.3.1.4 Detection in UHPLC
29.3.2 Coupling of UHPLC with spectrometric detectors
29.3.3 Coupling of UHPLC with mass spectrometers
29.4 Stationary Phases for UHPLC
29.4.1 Stationary Phases Based on Fully Porous Particles
29.4.1.1 Silica-based stationary phases
29.4.1.2 Metal oxide stationary phases
29.4.1.3 Hybrid stationary phases
29.4.1.4 Polymer stationary phases
29.4.2 Stationary Phases Based on Core-Shell Particles
29.5 Applications of UHPLC
29.5.1 Pharmaceutical Analysis
29.5.3 Food and Feed Analysis
29.5.4 Environmental Analysis
Liquid Chromatography
：Fundamentals and Instrumentation
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