Optimization in HPLC

Concepts and Strategies

Häftad, Engelska, 2021

Av Stavros Kromidas, Ge) Kromidas, Stavros (Novia GmbH, Saarbr¿cken

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Learn to maximize the performance of your HPLC or UHPLC system with this resource from leading experts in the fieldOptimization in HPLC: Concepts and Strategies delivers tried-and-tested strategies for optimizing the performance of HPLC and UHPLC systems for a wide variety of analytical tasks. The book explains how to optimize the different HPLC operation modes for a range of analyses, including small molecules, chiral substances, and biomolecules. It also shows readers when and how computational tools may be used to optimize performance.The practice-oriented text describes common challenges faced by users and developers of HPLC and UHPLC systems, as well as how those challenges can be overcome. Written for first-time and experienced users of HPLC technology and keeping pace with recent developments in HPLC instrumentation and operation modes, this comprehensive guide leaves few questions unanswered.Readers will also benefit from the inclusion of: A thorough introduction to optimization strategies for different modes and uses of HPLC, including working under regulatory constraintsAn exploration of computer aided HPLC optimization, including ChromSwordAuto and Fusion QbDA treatment of current challenges for HPLC users in industry as well as large and small analytical service providersDiscussions of current challenges for HPLC equipment suppliersTailor-made for analytical chemists, chromatographers, pharmacologists, toxicologists, and lab technicians, Optimization in HPLC: Concepts and Strategies will also earn a place on the shelves of analytical laboratories in academia and industry who seek a one-stop reference for optimizing the performance of HPLC systems.

Produktinformation

Utgivningsdatum2021-09-01
Mått170 x 244 x 21 mm
Vikt794 g
FormatHäftad
SpråkEngelska
Antal sidor416
FörlagWiley-VCH Verlag GmbH
ISBN9783527347896

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Stavros Kromidas, PhD, works as an independent consultant for analytical chemistry, based in Blieskastel (Germany). For more than 20 years he has regularly held lectures and training courses on HPLC, and has authored numerous articles and several books on various aspects of chromatography. He is the founder of NOVIA GmbH, a provider of professional training and consulting in analytical chemistry, and served as its CEO until 2001.

Preface xvAbout the Book xviiPart I Optimization Strategies for Different Modes and Uses of HPLC 11.1 2D-HPLC – Method Development for Successful Separations 3Dwight R. Stoll, Ph.D.1.1.1 Motivations for Two-Dimensional Separation 31.1.1.1 Difficult-to-Separate Samples 31.1.1.2 Complex Samples 41.1.1.3 Separation Goals 41.1.2 Choosing a Two-Dimensional Separation Mode 41.1.2.1 Analytical Goals Dictate Choice of Mode 51.1.2.2 Survey of Four 2D Separation Modes 51.1.2.3 Hybrid Modes Provide Flexibility 71.1.3 Choosing Separation Types/Mechanisms 81.1.3.1 Complementarity as a Guiding Principle 81.1.3.2 Pirok Compatibility Table 91.1.3.3 Measuring the Complementarity of Separation Types 91.1.4 Choosing Separation Conditions 111.1.4.1 Starting with Fixed First-Dimension Conditions 111.1.4.2 Starting from Scratch – Flexible First-Dimension Conditions 131.1.4.3 Special Considerations for Comprehensive 2D-LC Methods 131.1.4.4 Rules of Thumb 131.1.5 Method Development Examples 141.1.5.1 Example 1 – Use of LC–LC to Identify an Impurity in a Synthetic Oligonucleotide 141.1.5.2 Example 2 – Comprehensive 2D-LC Separation of Surfactants 141.1.6 Outlook for the Future 17Acknowledgment 18References 181.2 Do you HILIC? With Mass Spectrometry? Then do it Systematically 23Thomas Letzel1.2.1 Initial Situation and Optimal Use of Stationary HILIC Phases 251.2.2 Initial Situation and Optimal Use of the “Mobile” HILIC Phase 281.2.2.1 Organic Solvent 281.2.2.2 Salts 311.2.2.3 pH Value 331.2.3 Further Settings and Conditions Specific to Mass Spectrometric Detection 351.2.4 Short Summary on Method Optimization in HILIC 36References 361.3 Optimization Strategies in LC–MS Method Development 39Markus M. Martin1.3.1 Introduction 391.3.2 Developing New Methods for HPLC–MS Separations 391.3.2.1 Optimizing the LC Separation 401.3.2.1.1 Optimizing for Sensitivity and Limit of Detection – Which Column to Take? 401.3.2.1.2 Optimizing Resolution vs. Sample Throughput 411.3.2.1.3 MS-Compatible Eluent Compositions and Additives 431.3.2.2 Optimizing Ion Source Conditions 441.3.2.3 Optimizing MS Detection 471.3.2.4 Verifying the Hyphenated Method 481.3.2.5 Method Development Supported by Software-based Parameter Variation 491.3.3 Transferring Established HPLC Methods to Mass spectrometry 501.3.3.1 Transfer of an Entire HPLC Method to a Mass Spectrometer 511.3.3.2 Selected Analysis of an Unknown Impurity – Solvent Change by Single-/Multi-Heartcut Techniques 52Abbreviations 54References 551.4 Chromatographic Strategies for the Successful Characterization of Protein Biopharmaceuticals 57Szabolcs Fekete, Valentina D’Atri, and Davy Guillarme1.4.1 Introduction to Protein Biopharmaceuticals 571.4.2 From Standard to High-Performance Chromatography of Protein Biopharmaceuticals 581.4.3 Online Coupling of Nondenaturing LC Modes with MS 621.4.4 Multidimensional LC Approaches for Protein Biopharmaceuticals 641.4.5 Conclusion and Future Trends in Protein Biopharmaceuticals Analysis 66References 671.5 Optimization Strategies in HPLC for the Separation of Biomolecules 73Lisa Strasser, Florian Füssl, and Jonathan Bones1.5.1 Optimizing a Chromatographic Separation 731.5.2 Optimizing the Speed of an HPLC Method 771.5.3 Optimizing the Sensitivity of an HPLC Method 791.5.4 Multidimensional Separations (See also Chapter 1.1) 801.5.5 Considerations for MS Detection (See also Chapter 1.3) 811.5.6 Conclusions and Future Prospects 83References 841.6 Optimization Strategies in Packed-Column Supercritical Fluid Chromatography (SFC) 87Caroline West1.6.1 Selecting a Stationary Phase Allowing for Adequate Retention and Desired Selectivity 881.6.1.1 Selecting a Stationary Phase for Chiral Separations 881.6.1.2 Selecting a Stationary Phase for Achiral Separations 901.6.2 Optimizing Mobile Phase to Elute all Analytes 931.6.2.1 Nature of the Cosolvent 931.6.2.2 Proportion of Cosolvent 941.6.2.3 Use of Additives 961.6.2.4 Sample Diluent 971.6.3 Optimizing Temperature, Pressure, and Flow Rate 971.6.3.1 Understanding the Effects of Temperature, Pressure, and Flow Rate on your Chromatograms 971.6.3.2 Optimizing Temperature, Pressure, and Flow Rate Concomitantly 991.6.4 Considerations on SFC–MS Coupling 1001.6.5 Summary of Method Optimization 1011.6.6 SFC as a Second Dimension in Two-Dimensional Chromatography 1021.6.7 Further Reading 102References 1031.7 Strategies for Enantioselective (Chiral) Separations 107Markus Juza1.7.1 How to Start? 1081.7.2 Particle Size 1091.7.3 Chiral Polysaccharide Stationary Phases as First Choice 1101.7.4 Screening Coated and Immobilized Polysaccharide CSPs in Normal-Phase and Polar Organic Mode 1131.7.5 Screening Coated and Immobilized Polysaccharide CSPs in Reversed-Phase Mode 1161.7.6 Screening Immobilized Polysaccharide CSPs in Medium-Polarity Mode 1191.7.7 Screening Coated and Immobilized Polysaccharide CSPs under Polar Organic Supercritical Fluid Chromatography Conditions 1201.7.8 Screening Immobilized Polysaccharide CSPs in Medium-Polarity Supercritical Fluid Chromatography Conditions 1251.7.9 SFC First? 1271.7.10 Are There Rules for Predicting Which CSP Is Suited for My Separation Problem? 1271.7.11 Which Are the Most Promising Polysaccharide CSPs? 1271.7.12 Are some CSPs Comparable? 1291.7.13 “No-Go’s,” Pitfalls, and Peculiarities in Chiral HPLC and SFC 1321.7.14 Gradients in Chiral Chromatography 1331.7.15 Alternative Strategies to Chiral HPLC and SFC on Polysaccharide CSPs 1331.7.16 How Can I Solve Enantiomer Separation Problems Without Going to the Laboratory? 1351.7.17 The Future of Chiral Separations – Fast Chiral Separations (cUHPLC and cSFC)? 136References 1381.8 Optimization Strategies Based on the Structure of the Analytes 141Christoph A. Fleckenstein1.8.1 Introduction 1411.8.2 The Impact of Functional Moieties 1421.8.3 Hydrogen Bonds 1431.8.4 Influence ofWater Solubility by Hydrate Formation of Aldehydes and Ketones 1461.8.5 Does “Polar” Equal “Hydrophilic”? 1481.8.6 Peroxide Formation of Ethers 1501.8.7 The pH Value in HPLC 1511.8.7.1 Acidic Functional Groups 1521.8.7.2 Basic Functional Groups 1531.8.8 General Assessment and Estimation of Solubility of Complex Molecules 1551.8.9 Octanol–Water Coefficient 1571.8.10 Hansen Solubility Parameters 1601.8.11 Conclusion and Outlook 162Acknowledgments 163References 1631.9 Optimization Opportunities in a Regulated Environment 165Stavros Kromidas1.9.1 Introduction 1651.9.2 Preliminary Remark 1651.9.3 Resolution 1671.9.3.1 Hardware Changes 1671.9.3.1.1 Preliminary Remark 1671.9.3.1.2 UHPLC Systems 1681.9.3.1.3 Column Oven 1681.9.3.2 Improving the Peak Shape 1691.9.4 Peak-to-Noise Ratio 1711.9.4.1 Noise Reduction 1711.9.5 Coefficient of Variation, VC (Relative Standard Deviation, RSD) 171References 176Part II Computer-aided Optimization 1772.1 Strategy for Automated Development of Reversed-Phase HPLC Methods for Domain-Specific Characterization of Monoclonal Antibodies 179Jennifer La, Mark Condina, Leexin Chong, Craig Kyngdon, Matthias Zimmermann, and Sergey Galushko2.1.1 Introduction 1792.1.2 Interaction with Instruments 1812.1.3 Columns 1822.1.4 Sample Preparation and HPLC Analysis 1832.1.5 Automated Method Development 1842.1.5.1 Columns Screening 1852.1.5.2 Rapid Optimization 1862.1.5.3 Fine Optimization and Sample Profiling 1882.1.6 Robustness Tests 1882.1.6.1 Selection of the Variables 1892.1.6.2 Selection of the experimental design 1902.1.6.3 Definition of the Different Levels for the Factors 1912.1.6.4 Creation of the Experimental Set-up 1912.1.6.5 Execution of Experiments 1922.1.6.6 Calculation of Effects and Response and Numerical and Graphical Analysis of the Effects 1922.1.6.7 Improving the Performance of the Method 1942.1.7 Conclusions 196References 1962.2 Fusion QbD® Software Implementation of APLM Best Practices for Analytical Method Development, Validation, and Transfer 199Richard Verseput2.2.1 Introduction 1992.2.1.1 Application to Chromatographic Separation Modes 2002.2.1.2 Small- and Large-Molecule Applications 2002.2.1.3 Use for Non-LC Method Development Procedures 2002.2.2 Overview – Experimental Design and Data Modeling in Fusion QbD 2012.2.3 Analytical Target Profile 2012.2.4 APLM Stage 1 – Procedure Design and Development 2022.2.4.1 Initial SampleWorkup 2022.2.5 Chemistry System Screening 2042.2.5.1 Starting Points Based on Molecular Structure and Chemistry Considerations 2052.2.5.2 Trend Responses and Data Modeling 2052.2.6 Method Optimization 2072.2.6.1 Optimizing Mean Performance 2072.2.6.2 Optimizing Robustness In Silico – Monte Carlo Simulation 2102.2.6.3 A FewWords About Segmented (Multistep) Gradients and Robustness 2132.2.7 APLM Stage 2 – Procedure Performance Verification 2142.2.7.1 Replication Strategy 2142.2.8 The USP <1210> Tolerance Interval in Support of Method Transfer 2142.2.9 What is Coming – Expectations for 2021 and Beyond 216References 217Part III Current Challenges for HPLC Users in Industry 2193.1 Modern HPLC Method Development 221Stefan Lamotte3.1.1 Robust Approaches to Practice 2223.1.1.1 Generic Systems for all Tasks 2223.1.2 The Classic Reverse-phase System 2253.1.3 A System that Primarily Separates According to π–π Interactions 2273.1.4 A system that Primarily Separates According to Cation Exchange and Hydrogen Bridge Bonding Selectivity 2273.1.5 System for Nonpolar Analytes 2283.1.6 System for Polar Analytes 2283.1.7 Conclusion 2303.1.8 The Maximum Peak Capacity 2303.1.9 Outlook 231References 2313.2 Optimization Strategies in HPLC from the Perspective of an Industrial Service Provider 233Juri Leonhardt and Michael Haustein3.2.1 Introduction 2333.2.2 Research and Development 2333.2.3 Quality Control 2343.2.4 Process Control Analytics 2353.2.5 Decision Tree for the Optimization Strategy Depending on the Final Application Field 2373.3 Optimization Strategies in HPLC from the Perspective of a Service Provider – The UNTIE® Process of the CUP Laboratories 239Dirk Freitag-Stechl and Melanie Janich3.3.1 Common Challenges for a Service Provider 2393.3.2 A Typical, Lengthy Project – How it Usually Goes and How it Should not be Done! 2393.3.3 How DoWe Make It Better? - The UNTIE® Process of the CUP Laboratories 2413.3.4 Understanding Customer Needs 2413.3.5 The Test of an Existing Method 2423.3.6 Method Development and Optimization 2433.3.7 Execution of the Validation 2453.3.8 Summary 248Acknowledgments 249References 2493.4 Optimization Strategies in HPLC 251Bernard Burn3.4.1 Definition of the Task 2523.4.2 Relevant Data for the HPLC Analysis of a Substance (see also Chapter 1.8) 2523.4.2.1 Solubility 2523.4.2.2 Acidity Constants (pKa) 2573.4.2.2.1 Polarity of Acidic or Alkaline Substances (see also Chapter 1.8) 2573.4.2.2.2 UV Spectra 2593.4.2.2.3 Influence on the Peak Shape 2593.4.2.2.4 Acid Constant Estimation 2633.4.2.3 Octanol–Water Partition Coefficient 2633.4.2.4 UV Absorption 2703.4.2.5 Stability of the Dissolved Analyte 2723.4.3 Generic Methods 2783.4.3.1 General Method for the Analysis of Active Pharmaceutical Ingredients 2783.4.3.2 Extensions of the Range of Application 2793.4.3.3 Limits of this General Method 2793.4.3.4 Example, Determination of Butamirate Dihydrogen Citrate in a Cough Syrup 2793.4.3.4.1 Basic Data 2793.4.3.4.2 Expected Difficulties 2793.4.3.4.3 HPLC Method 2793.4.3.4.4 Example Chromatogram 2793.4.4 General Tips for Optimizing HPLC Methods 2793.4.4.1 Production of Mobile Phases 2843.4.4.1.1 Reagents 2843.4.4.1.2 Vessels and Bottles 2853.4.4.1.3 Measurement of Reagents and Solvent 2853.4.4.1.4 Preparation of Buffer Solutions 2863.4.4.1.5 Filtration of Solvents and Buffer 2863.4.4.1.6 Degassing of Mobile Phases 2873.4.4.2 Blank Samples 2873.4.4.3 Defining MeasurementWavelengths for UV Detection 2883.4.4.4 UV Detection at LowWavelengths 2883.4.4.4.1 Solvents 2913.4.4.4.2 Acids and Buffer Additives 2923.4.4.4.3 Drift at Solvent Gradients 2943.4.4.5 Avoidance of Peak Tailing 2953.4.4.6 Measurement Uncertainty and Method Design 3023.4.4.6.1 Weighing in or Measuring 3023.4.4.6.2 Dilutions 3033.4.4.6.3 HPLC Analysis 3043.4.4.6.4 Internal Standards 3053.4.4.7 Column Dimension and Particle Sizes 305Reference 309Part IV Current Challenges for HPLC Equipment Suppliers 3114.1 Optimization Strategies with your HPLC – Agilent Technologies 313Jens Trafkowski4.1.1 Increase the Absolute Separation Performance: Zero Dead-Volume Fittings 3144.1.2 Separation Performance: Minimizing the Dispersion 3144.1.3 Increasing the Throughput – DifferentWays to Lower the Turnaround Time 3164.1.4 Minimum Carryover for Trace Analysis: Multiwash 3174.1.5 Increase the Performance of What you have got – Modular or Stepwise Upgrade of Existing Systems 3184.1.6 Increase Automation, Ease of Use, and Reproducibility with the Features of a High-End Quaternary UHPLC Pump 3194.1.7 Increase Automation: Let your Autosampler do the Job 3214.1.8 Use Your System for Multiple Purposes: Multimethod and Method Development Systems 3214.1.9 Combine Sample Preparation with LC Analysis: Online SPE 3224.1.10 Boost Performance with a Second Chromatographic Dimension: 2D-LC (see also Chapter 1.1) 3234.1.11 Think Different,Work with Supercritical CO2 as Eluent: SFC – Supercritical Fluid Chromatography (see also Chapter 1.6) 3244.1.12 Determine Different Concentration Ranges in One System: High-Definition Range (HDR) HPLC 3254.1.13 Automize Even Your Method Transfer from other LC Systems: Intelligent System Emulation Technology (ISET) 3264.1.14 Conclusion 327References 3284.2 To Empower the Customer – Optimization Through Individualization 329Kristin Folmert and Kathryn Monks4.2.1 Introduction 3294.2.2 Define Your Own Requirements 3294.2.2.1 Specification Sheet, Timetable, or Catalogue of Measures 3294.2.2.2 Personnel Optimization Helps to make Better Use of HPLC 3314.2.2.3 Mastering Time-Consuming Method Optimizations in a Planned Manner 3324.2.2.4 Optimizations at Device Level do not Always have to Mean an Investment 3324.2.3 An Assistant Opens Up Many New Possibilities 3334.2.3.1 If the HPLC System must Simply be able to do more in the Future 3334.2.3.2 Individual Optimizations with an Assistant 3334.2.3.3 Automatic Method Optimization and Column Screening 3344.2.3.4 A New Perspective at Fractionation, Sample Preparation, and Peak Recycling 3354.2.3.5 Continuous Chromatography, a New Level of Purification 3364.2.4 The Used Materials in the Focus of the Optimization 3374.2.4.1 Wetted vs. Dry Components of the HPLC 3374.2.4.2 Chemical Resistance ofWetted Components 3384.2.4.3 Bioinert Components 3404.2.4.3.1 Material Certification 3404.2.5 Software Optimization Requires Open-Mindedness 3404.2.6 Outlook 3414.3 (U)HPLC Basics and Beyond 343Gesa Schad, Brigitte Bollig, and Kyoko Watanabe4.3.1 An Evaluation of (U)HPLC-operating Parameters and their Effect on Chromatographic Performance 3434.3.1.1 Compressibility Settings 3434.3.1.2 Solvent Composition and Injection Volume 3464.3.1.3 Photodiode Array Detector: Slit Width 3484.3.2 “Analytical Intelligence” – AI, M2M, IoT – How Modern Technology can Simplify the Lab Routine 3494.3.2.1 Auto-Diagnostics and Auto-Recovery to Maximize Reliability and Uptime 3494.3.2.2 Advanced Peak Processing to Improve Resolution 3504.3.2.3 Predictive Maintenance to Minimize System Downtime 353References 3544.4 Addressing Analytical Challenges in a Modern HPLC Laboratory 355Frank Steiner and Soo Hyun Park4.4.1 Vanquish Core, Flex, and Horizon – Three Different Tiers, all Dedicated to Specific Requirements 3564.4.2 Intelligent and Self-Contained HPLC Devices 3624.4.3 2D-LC for Analyzing Complex Samples and Further Automation Capabilities (see also Chapter 1.1) 3634.4.3.1 Loop-based Single-Heart-Cut 2D-LC 3644.4.3.2 Loop-based Multi-Heart-Cut 2D-LC 3644.4.3.3 Trap-based Single-Heart-Cut 2D-LC for Eluent Strength Reduction 3664.4.3.4 Trap-based Single-Heart-Cut 2D LC–MS Using Vanquish Dual Split Sampler 3674.4.4 Software-Assisted Automated Method Development 368Abbreviations 374References 3744.5 Systematic Method Development with an Analytical Quality-by-Design Approach Supported by Fusion QbD and UPLC–MS 375Falk-Thilo Ferse, Detlev Kurth, Tran N. Pham, Fadi L. Alkhateeb, and Paul RainvilleReferences 384Index 385