Enhanced descriptions from Syndetics:

A practical guide to using and maintaining an LC/MS system

The combination of liquid chromatography (LC) and mass spectrometry (MS) has become the laboratory tool of choice for a broad range of industries that require the separation, analysis, and purification of mixtures of organic compounds.

LC/MS: A Practical User's Guide provides LC/MS users with an easy-to-use, hands-on reference that focuses on the practical applications of LC/MS and introduces the equipment and techniques needed to use LC/MS successfully. Following a thorough explanation of the basic components and operation of the LC/MS system, the author presents empirical methods for optimizing the techniques, maintaining the instrumentation, and choosing the appropriate MS or LC/MS analyzer for any given problem.

LC/MS covers everything users need to know about: The latest equipment, including quadrupole, time-of-flight, and ion trap analyzers Cutting-edge processes, such as preparing HPLC mobile phases and samples; handling and maintaining a wide variety of silica, zirconium, and polymeric separation columns; interpreting and quantifying mass spectral data; and using MS interfaces Current and future applications in the pharmaceutical and agrochemical industries, biotechnology, clinical research, environmental studies, and forensics An accompanying PowerPoint® slide-set on CD-ROM provides vital teaching tools for instructors and new equipment operators. Abundantly illustrated and easily accessible, the text is designed to help students and practitioners acquire optimum proficiency in this powerful and rapidly advancing analytical application.

Table of contents provided by Syndetics

• Preface (p. xi)
• 1 Introduction to LC/MS (p. 1)
• 1.1 Why LC/MS? (p. 1)
• 1.2 Molecular Weights and Structure Studies (p. 4)
• 1.3 LC/MS Systems (p. 4)
• 1.4 System Costs (p. 7)
• 1.5 Competitive Systems (p. 7)
• 2 The HPLC System (p. 9)
• 2.1 HPLC System Components (p. 9)
• 2.2 Gradient versus Isocratic Systems (p. 14)
• 2.3 Micro HPLC Systems (p. 16)
• 2.4 HPLC Tubing and Fittings (p. 18)
• 3 The HPLC Column and Separation Modes (p. 21)
• 3.1 Column Construction (p. 21)
• 3.2 Column Packing Materials (p. 23)
• 3.3 Normal-Phase Columns (p. 25)
• 3.4 Other Bonded-Phase Silica Columns (p. 26)
• 3.5 Optimizing Reverse-Phase Column Use (p. 28)
• 3.6 Silica Ion-Exchange Columns (p. 30)
• 3.7 Silica Size-Separation Columns (p. 31)
• 3.8 Zirconium Bonded-Phase Columns (p. 31)
• 3.9 Polymer Reverse-Phase Columns (p. 32)
• 4 HPLC and Column Maintenance (p. 33)
• 4.1 HPLC Maintenance (p. 33)
• 4.2 Column Maintenance (p. 37)
• 5 Sample Preparation and Separations Development (p. 41)
• 5.1 Mobile-Phase Preparation (p. 41)
• 5.2 Mobile-Phase pH Control Using Buffers (p. 42)
• 5.3 Sample Preparation (p. 44)
• 5.4 Cartridge Column Cleanup (p. 44)
• 5.5 On-Column Sample Concentration (p. 45)
• 5.6 Isocratic and Gradient Methods Development (p. 46)
• 5.7 Automated Methods Development (p. 49)
• 6 LC/MS Interfaces (p. 51)
• 6.1 Solvent Removal and Ionization (p. 51)
• 6.2 Atmospheric-Pressure Interfaces (p. 52)
• 6.3 Electrospray Interface (p. 53)
• 6.4 Ion Spray Interface (p. 54)
• 6.5 Secondary Detectors (p. 55)
• 7 LC/MS Overview (p. 59)
• 7.1 HPLC and the Ionization Source (p. 60)
• 7.2 Vacuum Pumps (p. 61)
• 7.3 Analyzer and Ion Detector Designs (p. 61)
• 7.4 Data and Control Systems (p. 66)
• 7.5 Peak Detection, ID, and Quantitation (p. 69)
• 8 Mass Analyzers (p. 71)
• 8.1 Quadrupole Analyzer (p. 71)
• 8.2 Ion Trap Analyzer (p. 74)
• 8.3 Linear Ion Trap Analyzer (p. 78)
• 8.4 Time-of-Flight Analyzer (p. 79)
• 8.5 Fourier Transform Analyzer Design (p. 81)
• 8.6 Magnetic Sector Analyzers (p. 83)
• 9 Mass Spectrometer Maintenance (p. 85)
• 9.1 High-Vacuum Operation (p. 85)
• 9.2 MS Hardware Maintenance (p. 88)
• 9.3 System Electrical Grounding (p. 92)
• 10 Application Areas for LC/MS (p. 95)
• 10.1 Compound Discovery (p. 95)
• 10.2 Identification of Complex Biological Compounds (p. 96)
• 10.3 Analysis of Trace Impurities and Metabolites (p. 97)
• 10.4 Arson Residue Investigation (p. 98)
• 10.5 Industrial Water and Pesticide Analysis (p. 98)
• 10.6 Toxicology and Drugs of Abuse (p. 98)
• 10.7 Clinical Therapeutic Drug Screening (p. 99)
• 10.8 Pesticide Manufacturing (p. 101)
• 11 Trace Analysis and LC/MS/MS (p. 103)
• 11.1 LC/MS/MS Triple-Quadrupole System (p. 103)
• 11.2 MS/MS Operating Modes (p. 104)
• 11.3 Ion Trap MS/MS Operation (p. 106)
• 11.4 Hybrid LC/MS/MS Systems (p. 108)
• 12 Drug Discovery and Benchtop LC/MS (p. 111)
• 12.1 Activity Screening (p. 111)
• 12.2 Standardized LC/MS Screening (p. 113)
• 12.3 Molecular Fragmentation for Structural Determination (p. 115)
• 12.4 Process Monitoring (p. 116)
• 13 Proteomics: LC/MALDI/TOF and MS/MS Libraries (p. 119)
• 13.1 Protein Molecular-Weight Determination by LC/MS (p. 120)
• 13.2 De Novo Protein Purification (p. 121)
• 13.3 Protein Analysis by Two-Dimensional GEP and LC/TOFMS (p. 122)
• 13.4 LC/MS/MS Identification of Peptide Structures (p. 122)
• 13.5 Tracer Labeling for Peptide ID (p. 124)
• 13.6 Posttranslational Modified Protein (p. 124)
• 13.7 Transient Peptides and Accumulation Proteins (p. 124)
• 14 The Future of LC/MS (p. 127)
• 14.1 Instrumentation Improvements (p. 127)
• 14.2 Affordable Benchtop LC/LITMS (p. 129)
• 14.3 User-Customized Data Libraries (p. 129)
• 14.4 Nucleomics and Restriction Fragment Analysis (p. 130)
• Appendix A LC/MS Frequently Asked Questions (p. 131)
• Appendix B Solvents and Volatile Buffers for LC/MS (p. 139)
• Appendix C Guide to Structure Interpretation (p. 143)
• Appendix D Glossary of LC/MS Terms (p. 149)
• Appendix E LC/MS Selective Reading List (p. 155)
• Index (p. 157)

Author notes provided by Syndetics