Sample Preparation in LC-MS Bioanalysis

Description

Content: Intro -- Title Page -- Copyright Page -- Contents -- List of Contributors -- Preface -- List of Abbreviations -- Part I Current Sample Preparation Techniques in LC-MS Bioanalysis -- Chapter 1 Basic Sample Preparation Techniques in LC-MS Bioanalysis: Protein Precipitation, Liquid-Liquid Extraction, and Solid-Phase Extraction -- 1.1 Introduction -- 1.2 Physicochemical Properties of Drugs and Their Metabolites -- 1.2.1 Hydrophilicity vs. Lipophilicity of Analyte(s) -- 1.2.2 Protolytic Properties of Analyte(s) -- 1.3 Pre-analytical Variables of Analyte(s) of Interest in Biological Matrix -- 1.3.1 Stability -- 1.3.2 Nonspecific Binding -- 1.3.3 Protein Binding -- 1.3.4 Blood-to-plasma Ratio and Red Blood Cell Partition -- 1.4 Most Commonly Used Sample Preparation Methods in LC-MS Bioanalysis -- 1.4.1 Protein Precipitation (PPT) -- 1.4.1.1 Water-miscible Organic Solvents -- 1.4.1.2 Acids -- 1.4.2 Liquid-Liquid Extraction (LLE) -- 1.4.2.1 Mechanism of LLE and Extraction Recovery -- 1.4.2.2 Solvent in LLE -- 1.4.2.3 General Procedures in LLE -- 1.4.2.4 Application of LLE in LC-MS Bioanalysis -- 1.4.2.5 Other Formats of LLE -- 1.4.3 Solid-phase Extraction (SPE) -- 1.4.3.1 SPE Stationary Phases (Sorbents) -- 1.4.3.2 Common SPE Platforms in LC-MS Bioanalysis -- 1.4.3.3 General SPE Workflows -- 1.4.3.4 Other Formats of SPE -- 1.4.4 Combination of PPT, LLE, and/or SPE in LC-MS Bioanalysis -- 1.4.4.1 Combination of PPT and LLE -- 1.4.4.2 Combination of PPT and SPE -- 1.4.4.3 Combination of LLE and SPE -- 1.4.5 Summary -- References -- Chapter 2 Online Extraction and Column Switching Techniques in LC-MS Bioanalysis -- 2.1 Introduction -- 2.2 System Configuration -- 2.2.1 Single-column System -- 2.2.2 Dual-column System -- 2.2.3 Staggered Parallel Online Extraction Systems -- 2.3 Commonly Used Online Extraction Techniques. 2.3.1 Turbulent/High Flow Chromatography -- 2.3.2 Restricted Access Media -- 2.3.3 Monolithic Materials -- 2.3.4 Hydrophilic Interaction Liquid Chromatography -- 2.3.5 Immunoaffinity Extraction -- 2.3.6 Disposable Extraction Cartridges -- Online SPE -- 2.3.7 Online Extraction of Dried Blood Spot (DBS) Samples -- 2.3.8 SPE-MS -- 2.4 Considerations for Utilizing Online Extraction Techniques -- 2.4.1 Advantages and Limitations -- 2.4.2 Strategies for Online Extraction Method Development -- 2.5 Summary -- References -- Chapter 3 Equilibrium Dialysis, Ultracentrifugation, and Ultrafiltration in LC-MS Bioanalysis -- 3.1 Introduction -- 3.2 Challenges and Considerations -- 3.3 Experimental Procedures -- 3.3.1 Equilibrium Dialysis -- 3.3.2 Ultrafiltration -- 3.3.3 Ultracentrifugation -- 3.4 Summary -- References -- Chapter 4 Phospholipid Depletion Techniques in LC-MS Bioanalysis -- 4.1 Introduction -- 4.2 Impact of Phospholipids on Bioanalytical Methods -- 4.3 Investigating Matrix Effects Associated with Phospholipids -- 4.4 Minimizing Matrix Effects Associated with Phospholipids -- 4.4.1 Sample Dilution -- 4.4.2 Column Manipulations -- 4.4.3 Internal Standards -- 4.4.4 Ionization Choice -- 4.4.5 Other Experimental Modifications -- 4.5 Removing Phospholipids Prior to LC-MS Analysis -- 4.5.1 Protein Precipitations -- 4.5.2 Liquid-Liquid Extraction and Supported Liquid Membranes -- 4.5.3 Supported Liquid Extraction -- 4.5.4 Electrostatic Removal -- 4.5.5 Solid-Phase Extraction -- 4.6 Example Methods that Demonstrate Successful Phospholipid Removal -- 4.7 Conclusions -- Acknowledgement -- References -- Chapter 5 Salting-out Assisted Liquid-Liquid Extraction (SALLE) in LC-MS Bioanalysis -- 5.1 Introduction -- 5.2 Considerations in Developing a SALLE Method -- 5.2.1 Salts -- 5.2.2 Water-Miscible Solvent -- 5.2.3 pH. 5.3 Combination of SALLE with Other Extraction Techniques -- 5.4 Matrix Effect in SALLE -- 5.5 Miniaturization and Automatization -- 5.6 Summary -- References -- Chapter 6 Supported Liquid Extraction (SLE) in LC-MS Bioanalysis -- 6.1 Introduction -- 6.2 Principle of SLE -- 6.3 Advantages and Limitation of SLE in Quantitative LC-MS Bioanalysis -- 6.3.1 Advantages -- 6.3.2 Limitation -- 6.4 Key Consideration in Developing Robust SLE-LC-MS Bioanalytical Method -- 6.5 Representative Protocols -- 6.5.1 Material, Supplies, and Equipment -- 6.5.2 Protocols for SLE Cartridge and Plate Processing -- 6.6 Summary -- References -- Chapter 7 Immunocapture in LC-MS Bioanalysis -- 7.1 Introduction -- 7.2 Experimental Workflow and Optimization -- 7.3 Considerations on the Selection of Capture Reagents and the Limitations -- 7.4 Platforms for Immunocapture -- 7.5 Internal Standard Selection -- 7.6 Performance Evaluation -- 7.7 Applications and Representative Protocols -- 7.7.1 Endogenous Peptides/Proteins -- 7.7.2 Protein-based Biotherapeutics -- 7.7.3 Immunogenicity -- 7.8 Validation Criteria and Regulatory Considerations -- 7.9 Summary -- References -- Chapter 8 Microextraction Techniques in LC-MS Bioanalysis -- 8.1 Introduction -- 8.2 Solid-Phase Microextraction -- 8.2.1 Conventional Fiber SPME -- 8.2.2 Stir-Bar Sorptive Extraction -- 8.2.3 Thin-Film Microextraction -- 8.2.4 In-Tube SPME -- 8.2.5 In-Needle SPME -- 8.2.5.1 Solid-Phase Dynamic Extraction -- 8.2.5.2 Microextraction by Packed Sorbent -- 8.2.5.3 Fiber-Packed Needle Microextraction -- 8.2.6 In-Tip SPME -- 8.2.7 New Sorbents for SPME -- 8.2.7.1 Monolithic Sorbent -- 8.2.7.2 Carbon Nanotubes -- 8.3 Liquid-Phase Microextraction -- 8.3.1 Single-Drop Microextraction -- 8.3.2 Hollow Fiber Liquid-Phase Microextraction -- 8.3.3 Dispersive Liquid-Liquid Microextraction. 8.3.4 Influence Factors on LPME Efficiency -- 8.4 Summary -- Acknowledgements -- References -- Chapter 9 Microsampling Applications with LC-MS Bioanalysis -- 9.1 Introduction -- 9.2 Plasma Microsampling Considerations -- 9.2.1 Sample Collection -- 9.2.2 Interaction with Thixotropic Gel -- 9.2.3 Sample Manipulation -- 9.2.4 Extraction, LC-MS/MS Analysis, and Detection -- 9.3 Dried Blood (Matrix) Spot (DBS) Considerations -- 9.3.1 Sample Collection -- 9.3.2 Sample Manipulation -- 9.3.3 Extraction, LC-MS/MS Analysis, and Detection -- 9.4 Volumetric Absorptive Microsampling (VAMS) -- 9.4.1 Sample Collection -- 9.4.2 Sample Manipulation -- 9.4.3 Extraction, LC-MS/MS Analysis, and Detection -- 9.5 Emerging Techniques -- 9.6 Summary -- Acknowledgements -- References -- Chapter 10 Nanomaterials for Sample Preparation in LC-MS Bioanalysis -- 10.1 Introduction -- 10.2 Carbon Nanomaterials -- 10.3 Metallic NPs -- 10.3.1 Metal Nanoparticles -- 10.3.2 Metal Oxide Nanoparticles -- 10.4 Nanoporous Materials -- 10.4.1 Polymeric Nanomaterials -- 10.4.2 Mesoporous Materials -- 10.4.3 Molecular Imprinted Polymers (MIPs) -- 10.5 Future Perspectives -- Acknowledgements -- References -- Chapter 11 Sample Preparation via Molecularly Imprinted Polymers (MIPs) in LC-MS Bioanalysis -- 11.1 Introduction -- 11.2 Preparation of MIPs -- 11.2.1 Template and Monomer(s) -- 11.2.2 Cross-linker -- 11.2.3 Porogen -- 11.3 MIPs for Sample Preparation in Bioanalysis -- 11.3.1 Molecularly Imprinted Solid-phase Extraction (MISPE) -- 11.3.1.1 Off-line Protocols -- 11.3.1.2 Online Protocols -- 11.3.1.3 In-line Protocols -- 11.3.1.4 Other Protocols -- 11.3.2 MIPs in Other Sample Preparation Techniques -- 11.4 Fragment Imprinting -- 11.5 Summary -- References -- Chapter 12 Stir-bar Sorptive Extraction for Sample Preparation in LC-MS Bioanalysis -- 12.1 Introduction -- 12.2 SBSE Principle. 12.3 SBSE Steps -- 12.3.1 Extraction Procedure -- 12.3.2 Desorption -- 12.3.2.1 Thermal Desorption -- 12.3.2.2 Liquid Desorption -- 12.4 Derivatization -- 12.4.1 In Situ Derivatization -- 12.4.2 On-Stir-Bar Derivatization -- 12.4.3 Post-Extraction Mode -- 12.5 Coating Materials -- 12.6 Applications -- 12.7 Summary -- References -- Chapter 13 Monolithic Spin Column Extraction in LC-MS Bioanalysis -- 13.1 Introduction -- 13.2 History of Monoliths -- 13.3 The Use of Monolith as Sorbent in Solid-Phase Extraction -- 13.4 Monolithic Spin Column for Sample Preparation -- 13.4.1 Extraction Procedure -- 13.4.2 Extraction Mechanism -- 13.4.3 Advantages and Limitations -- 13.4.3.1 Zero Dead Volume -- 13.4.3.2 No Channeling -- 13.4.3.3 Ease of Operation -- 13.4.3.4 Ease of Shape Modification -- 13.4.3.5 Loading Sample Volume -- 13.4.3.6 High Viscosity Sample -- 13.4.3.7 Commercial Suppliers -- 13.4.4 Applications -- References -- Chapter 14 Aptamer-based Sample Preparation in LC-MS Bioanalysis -- 14.1 Introduction -- 14.2 Aptamer-based Sample Preparation -- 14.2.1 Aptamer-based Solid-phase Extraction -- 14.2.1.1 Aptamer-based Affinity Columns for SPE -- 14.2.1.2 Aptamer-based Magnetic SPE -- 14.2.1.3 Aptamer-based Surface Affinity SPE -- 14.2.1.4 Aptamer-functionalized Materials for Other SPE Format -- 14.2.2 Aptamer-based Solid-phase Microextraction -- 14.2.3 Aptamer-based Microfluidic Sample Preparation -- 14.3 Representative Protocols -- 14.4 Summary -- Acknowledgements -- References -- Chapter 15 Sample Extraction via Electromembrane in LC-MS Bioanalysis -- 15.1 Introduction -- 15.2 Factors Affecting the Extraction Efficiency of EME -- 15.2.1 Composition of Supported Liquid Membrane and Nature of the Supports -- 15.2.2 Composition of Acceptor and Donor (Sample) Phase -- 15.2.2.1 For Extraction of Basic Drugs -- 15.2.2.2 For Extraction of Acidic Drugs.