Filling the gap for an expert text dealing exclusively with the practical aspects of HPLC-MS coupling, this concise, compact, and clear book provides detailed information to enable users to employ the method most efficiently.

Following an overview of the current state of HPLC-MS and its instrumentation, the text goes on to discuss all relevant aspects of method development. A chapter on tips and tricks is followed by user reports on the advantages - and pitfalls - of applying the method in real-life scenarios. The whole is rounded off by a look at future developments by renowned manufacturers.

1;Cover;1 2;Main title;5 3;Copyright page;6 4;Contents;7 5;Preface;13 6;The Structure of HPLC-MS for Practitioners;15 7;List of Contributors;17 8;Part I Overview, Pitfalls, Hardware-Requirements;19 8.1;1 State of the Art in the LC/MS;21 8.1.1;1.1 Introduction;21 8.1.2;1.2 Ionization Methods at Atmospheric Pressure;23 8.1.2.1;1.2.1 Overview of API Methods;24 8.1.2.2;1.2.2 ESI;24 8.1.2.3;1.2.3 APCI;26 8.1.2.4;1.2.4 APPI;27 8.1.2.5;1.2.5 APLI;28 8.1.2.6;1.2.6 Determination of Ion Suppression;29 8.1.2.7;1.2.7 Best Ionization for Each Question;29 8.1.3;1.3 Mass Analyzer;30 8.1.4;1.4 Future Developments;31 8.1.5;1.5 What Should You Look for When Buying a Mass Spectrometer?;32 8.1.6;References;32 8.2;2 Technical Aspects and Pitfalls of LC/MS Hyphenation;37 8.2.1;2.1 Instrumental Requirements for LC/MS Analysis - Configuring the Right System for Your Analytical Challenge;38 8.2.1.1;2.1.1 (U)HPLC and Mass Spectrometry - Not Just a Mere Front-End;38 8.2.1.2;2.1.2 UHPLC System Optimization - Gradient Delay and Extra-column Volumes;39 8.2.1.3;2.1.3 Does Your Mass Spectrometer Fit Your Purpose?;51 8.2.1.4;2.1.4 Data Rates and Cycle Times of Modern Mass Spectrometers;56 8.2.1.5;2.1.5 Complementary Information by Additional Detectors or Mass Spectrometry Won't Save the World;57 8.2.2;2.2 LC/MS Method Development and HPLC Method Adaptation - How to Make My LC Fit for MS?;61 8.2.2.1;2.2.1 Method Development LC/MS - LC Fits the MS Purposes;62 8.2.2.2;2.2.2 Converting Classical HPLC Methods into LC/MS;71 8.2.3;2.3 Pitfalls and Error Sources - Sometimes Things Do Go Wrong;72 8.2.3.1;2.3.1 No Signal at All;72 8.2.3.2;2.3.2 Inappropriate Ion Source Settings and Their Impact on the Chromatogram;74 8.2.3.3;2.3.3 Ion Suppression;76 8.2.3.4;2.3.4 Unknown Mass Signals in the Mass Spectrum;77 8.2.3.5;2.3.5 Instrumental Reasons for the Misinterpretation of Mass Spectra;83 8.2.4;2.4 Conclusion;86 8.2.5;2.5 Abbreviations;87 8.2.6;References;87 8.3;3 Aspects of the Development of Methods in LC/MS Coupling;91 8.3.1;3.1 Introduction;91 8.3.2;3.2 From Target to Screening Analysis;92 8.3.2.1;3.2.1 Target Analysis;92 8.3.2.2;3.2.2 Suspected-Target Screening;92 8.3.2.3;3.2.3 Non-target Screening;92 8.3.2.4;3.2.4 Comparable Overview of the Different Acquisition Modes;93 8.3.3;3.3 The Optimization of Parameters in Chromatography and Mass Spectrometry;93 8.3.3.1;3.3.1 Requirements and Recommendations for HPLC/MS Analysis Taking DIN 38407-47 as an Example;93 8.3.3.2;3.3.2 The Definition of Critical Peak Pairs in the Context of HPLC/MS Coupling;95 8.3.3.3;3.3.3 The Separation of Polar Components from the Column Void Time;97 8.3.3.4;3.3.4 Determining the HPLC Method Parameters Using the Example of the Separation of Selected Pharmaceuticals;98 8.3.3.5;3.3.5 Carrying out Screening Experiments;102 8.3.3.6;3.3.6 Evaluation of the Data and Discussion of the Influencing Parameters;104 8.3.3.7;3.3.7 Using Simulation Software for Fine Optimization;116 8.3.3.8;3.3.8 Choosing the Stationary Phase Support;117 8.3.3.9;3.3.9 The Influence of the Inner Column Diameter and the Mobile Phase Flow Rate;121 8.3.3.10;3.3.10 The Influence of the Injection Volume;122 8.3.3.11;3.3.11 Establishing the Mass Spectrometric Parameters;133 8.3.3.12;3.3.12 Optimization of the Mass Spectrometric Parameters;135 8.3.3.13;3.3.13 Quantification Using LC/MS;140 8.3.3.14;3.3.14 Screening Using LC/MS;146 8.3.3.15;3.3.15 Miniaturization160`-8211`- LC/MS Quo Vadis?;150 8.3.4;References;152 9;Part II Tips, Examples, Trends;157 9.1;4 LC/MS for Everybody/for Everything? - LC/MS Tips;159 9.1.1;4.1 Introduction;159 9.1.2;4.2 Tip Number 1;160 9.1.2.1;4.2.1 Choosing the Right LC/MS Interface;160 9.1.3;4.3 Tip Number 2;166 9.1.3.1;4.3.1 Which Mobile Phases Are Compatible with LC/MS?;166 9.1.4;4.4 Tip Number 3;167 9.1.4.1;4.4.1 Phosphate Buffer - The Exception;167 9.1.5;4.5 Tip Number 4;168 9.1.5.1;4.5.1 Paired Ions;168 9.1.5.2;4.5.2 Which "Antidote" Is Available?;169 9.1.5.3;4.5.3 Summary;170 9.1.6;4.6 Tip Number 5;1