Books on Analytical Sciences

AOAC is pleased to announce that the Fourth revision 2011 of the 18th Edition of the Official Methods of Analysis (OMA) is available now. OMA is the most comprehensive and reliable collection of chemical and microbiological methods available.

LC/MS: A Practical User's GuideMarvin McMasterIHardcover184 pages

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.

Chapter 1. Introduction to LC/MS.

Chapter 2. The HPLC System.

Chapter 3. The HPLC Column and Separation Modes.

Chapter 4. HPLC and Column Maintenance.

Chapter 5. Sample Preparation and Separations Development.

Chapter 6. LC/MS Interfaces.

Chapter 7. LC/MS Overview.

Chapter 8. The Mass Analyzers.

Chapter 9. Mass Spectrometer Maintence.

Chapter 10. Application Areas for LC/MS.

Chapter 11. Trace Analysis and LC/MS/MS.

Chapter 12. Drug Discovery and Benchtop LC/MS.

Chapter 13. Proteomics: LC/MALDI/TOF and MS/MS Libraries.

Chapter 14. The Future of LC/MS.

Appendix A: LC/MS Frequently Asked Questions.

Appendix B: Solvents and Volatile Buffers for LC/MS.

Appendix C: A Guide to Structure Interpretation.

Appendix D: A Glossary of LC/MS Terms.

Appendix E: LC/MS Selective Reading List.

Practical HPLC Method Development, 2nd EditionLloyd R. Snyder, Joseph J. Kirkland, Joseph L. GlajchHardcover800 pages

This revision brings the reader completely up to date on the evolving methods associated with increasingly more complex sample types analyzed using high-performance liquid chromatography, or HPLC. The book also incorporates updated discussions of many of the fundamental components of HPLC systems and practical issues associated with the use of this analytical method. This edition includes new or expanded treatments of sample preparation, computer assisted method development, as well as biochemical samples, and chiral separations.


Getting Started.

Basics of Separation.

Detection Sensitivity and Selectivity.

Sample Preparation.

The Column.

Non-Ionic Samples: Reversed- and Normal-Phase HPLC.

Ionic Samples: Reversed-Phase, Ion-Pair, and Ion-Exchange HPLC.

Gradient Elution.

Systematic Approach to the Reversed-Phase Separation of Regular Samples.

Computer-Assisted Method Development.

Biochemical Samples: Proteins, Nucleic Acids, Carbohydrates, and Related Compounds.

Chiral Separations.

Preparative HPLC Separation.

Quantitation (Including Trace Analysis).

Completing the Method: Validation and Transfer.

Appendices.

Index.

Edited By
Satinder Ahuja, Ahuja Consulting, Calabash, NC, USA
Stephen Scypinski, R.W. Johnson Pharmaceutical Research Institute, Raritan, New Jersey, U.S.A.

Hardbound, 598 pages
Published: SEP-2010


Handbook of Modern Pharmaceutical Analysis, Second Edition, synthesizes the complex research and recent changes in the field, while covering the techniques and technology required for today's laboratories. The work integrates strategy, case studies, methodologies, and implications of new regulatory structures, providing complete coverage of quality assurance from the point of discovery to the point of use.

Audience:
Method development chemists, analytical chemists, organic chemists, pharmaceutical chemists, biochemists, medicinal chemists and licensing authorities.

TABLE OF CONTENTS :

Overview (Satinder Ahuja);

High Throughput Screening in Drug Discovery and Development (Ken Apple);

Solid-State Analysis (Harry Brittain);

Degradation Studies of Drug Candidates (Karen Alsante);

Analytical Considerations for Genotoxic and Other Impurities (Scott Miller);

Quality by Design (James Drennen);

Preformulation Studies (tba);

Process Analytical Technology (Christine Richardson);

Solid Dosage-Form Analysis (Joe Etse);

Parenteral Dosage Form Analysis (Greg Birrer);

Analysis of Alternate Drug Delivery systems (Ron Smith);

Method Development for Chiral Compounds (S. Ahuja);

Method Development for Early Phase Drug Development (Kevin Bynum);

Method Development for Late Phase Drug Development (Ilias Jimidar);

Analysis of Biomolecules (Ilias Jimidar);

Setting Up Specifications (Doug Raynie);

Validation of Test Methods (Jonathan Crowther);

Stability Evaluations (Jessica Cha);

Transferring Analytical Methods (Stephen Scypinski);

Pharmaceutical Analysis Documentation (H. Chokshi);

Emerging Analytical Methodologies (Jim Lander)

by
B.W. Wenclawiak et al

Quality Assurance in Analytical Chemistry contains a compilation from different areas which deal with QA. Topics covered in this book include:

• Accreditation - ISO 17025
• Certification - ISO 9000
• Proficiency Testing
• Basic Statistics
• Measurement Uncertainty
• Glossary / Institutions
• Fit for the purpose (Philosophy)
• Quality Manual
• Validation of Methods
• Accreditation vs. Certification
• GLP
• Calibration - Detection Limit
• Reference Materials
• Control Charts
• Metrology/Traceability
• TQM and Cost of Quality

Standards such as ISO 17025, accreditation, measurement uncertainty amongst many others are topics which are often not covered. This reference provides basic information in all fields that are of interest for quality assurance in chemical measurement regarding management requirements as well as technical requirements. It is also very valuable for all those leaving the university, before they seek their first employment and to get ready for the job interview.

Quality Assurance in Analytical Chemistry includes a CD-ROM which accompanies the book. Material provided thereon can be used as memory card or as ready to use transparencies for teaching purposes in educational institutions and for in-house training of the laboratory staff. Specialists from different fields have contributed to this book sharing their expertise with the reader to get started in QA.

Contents

1. Glossary of Analytical Chemistry Terms
2. Fit for Purpose—A Customers View
3. Accreditation—ISO/IEC 17025
4. ISO 9000:2000 Quality Management System
5. Accreditation or Certification for Laboratories?
6. Good Laboratory Practice
7. Total Quality Management and Cost of Quality
8. Quality Manual
9. Basic Statistics
10. Calibration and Detection Limits
11. Metrology in Chemistry and Traceability of Analytical Measurement Results
12. Validation of Analytical Methods
13. Measurement Uncertainty
14. Control Charts
15. (Certified) Reference Materials
16. Interlaboratory Tests

Index

 

Harold M. McNair (Virginia Polytechnic Institute and State Univ.),

James M. Miller (Drew Univ.) Hardcover256 pagesJuly 2009, ©2009

The New Edition of the Well-Regarded Handbook on Gas Chromatography

Since the publication of the highly successful first edition of Basic Gas Chromatography, the practice of chromatography has undergone several notable developments. Basic Gas Chromatography, Second Edition covers the latest in the field, giving readers the most up-to-date guide available, while maintaining the first edition's practical, applied approach to the subject and its accessibility to a wide range of readers.

The text provides comprehensive coverage of basic topics in the field, such as stationary phases, packed columns and inlets, capillary columns and inlets, detectors, and qualitative and quantitative analysis. At the same time, the coverage also features key additions and updated topics including:

• Gas chromatography-mass spectrometry (GC-MS)
• Sampling methods
• Multidimensional gas chromatography
• Fast gas chromatography
• Gas chromatography analysis of nonvolatile compounds
• Inverse gas chromatography and pyrolysis gas chromatography

Along with these new and updated topics, the references, resources, and Web sites in Basic Gas Chromatography have been revised to reflect the state of the field. Concise and fundamental in its coverage, Basic Gas Chromatography, Second Edition remains the standard handbook for everyone from undergraduates studying analytical chemistry to working industrial chemists.

PREFACE TO THE SECOND EDITION.

PREFACE.

ACKNOWLEDGMENTS.

1 INTRODUCTION.

A Brief History.

Definitions.

Overview: Advantages and Disadvantages.

Instrumentation.

References.

2 INSTRUMENT OVERVIEW.

Carrier Gas.

Flow Control and Measurement.

Sample Inlets and Sampling Devices.

Columns.

Temperature Zones.

Detectors.

Data Systems.

References.

3 BASIC CONCEPTS AND TERMS.

Definitions, Terms, and Symbols.

The Rate Theory.

A Redefinition of H.

The Achievement of Separation.

References.

4 STATIONARY PHASES.

5 PACKED COLUMNS AND INLETS.

6 CAPILLARY COLUMNS AND INLETS.

7 DETECTORS.

8 QUALITATIVE AND QUANTITATIVE ANALYSIS.

 

9 PROGRAMMED TEMPERATURE.

10 GAS CHROMATOGRAPHY–MASS SPECTROMETRY (GC–MS).

11 MULTIDIMENSIONAL GAS CHROMATOGRAPHY.

12 SAMPLING METHODS.

Overview.

Liquid–Liquid Extraction (LLE).

Solid–Liquid Extraction: Soxhlet Extraction and Accelerated Solvent Extraction (ASE).

Liquid–Solid Extraction: Solid-Phase Extraction (SPE).

Liquid- or Solid-Vapor Extraction: Headspace Extraction.

Solid-Phase Micro-extraction (SPME).

Additional Techniques and Summary.

References.

13 SPECIAL TOPICS.

Fast GC.

Chiral Analysis by GC.

GC Analysis of Nonvolatile Compounds.

References.

14 TROUBLESHOOTING GC SYSTEMS.

APPENDIX I SYMBOLS AND ACRONYMS.

APPENDIX II GUIDELINES FOR SELECTING CAPILLARY COLUMNS.

APPENDIX III GC: HOW TO AVOID PROBLEMS.

APPENDIX IV CALCULATION OF SPLIT RATIO FOR SPLIT INJECTION ON OT COLUMNS.

APPENDIX V OPERATING CONDITIONS FOR CAPILLARY COLUMNS.

APPENDIX VI OV LIQUID PHASES PHYSICAL PROPERTY DATA.

APPENDIX VII SOME COMPRESSIBILITY CORRECTION FACTORS (J).

APPENDIX VIII SOME INTERNET WEBSITES FOR GAS CHROMATOGRAPHERS.

APPENDIX IX OTHER BOOKS ON GAS CHROMATOGRAPHY.

INDEX OF APPLICATIONS.

INDEX.

Organic Structures from Spectra, Fourth Edition consists of a carefully selected set of over 300 structural problems involving the use of all the major spectroscopic techniques. The problems are graded to develop and consolidate the student’s understanding of Organic Spectroscopy, with the accompanying text outlining the basic theoretical aspects of  major spectroscopic techniques at a level sufficient to tackle the problems.

Specific changes for the new edition will include

• A significantly expanded section on 2D NMR spectroscopy focusing on COSY, NOESY and CH-Correlation
• Incorporating new material into some tables to provide extra characteristic data for various classes of compounds
• Additional basic information on how to solve spectroscopic problems
• Providing new problems within the area of 10 2D NMR spectroscopy
• More problems at the ‘simpler’ end of the range

As with previous editions, this book combines basic theory, practical advice and sensible approaches to solving spectra problems. It will therefore continue to prove invaluable to students studying organic spectroscopy across a range of disciplines.

PREFACE.

LIST OF TABLES.

LIST OF FIGURES.

1 INTRODUCTION.

1.1 GENERAL PRINCIPLES OF ABSORPTION SPECTROSCOPY.

1.2 CHROMOPHORES.

1.3 DEGREE OF UNSATURATION.

1.4 CONNECTIVITY.

1.5 SENSITIVITY.

1.6 PRACTICAL CONSIDERATIONS.

2 ULTRAVIOLET (UV) SPECTROSCOPY.

2.1 BASIC INSTRUMENTATION.

2.2 THE NATURE OF ULTRAVIOLET SPECTROSCOPY.

2.3 QUANTITATIVE ASPECTS OF ULTRAVIOLET SPECTROSCOPY.

2.4 CLASSIFICATION OF UV ABSORPTION BANDS.

2.5 SPECIAL TERMS IN ULTRAVIOLET SPECTROSCOPY.

2.6 IMPORTANT UV CHROMOPHORES.

2.7 THE EFFECT OF SOLVENTS.

3 INFRARED (IR) SPECTROSCOPY.

3.1 ABSORPTION RANGE AND THE NATURE OF IR ABSORPTION.

3.2 EXPERIMENTAL ASPECTS OF INFRARED SPECTROSCOPY.

3.3 GENERAL FEATURES OF INFRARED SPECTRA.

3.4 IMPORTANT IR CHROMOPHORES.

4 MASS SPECTROMETRY.

4.1 IONIZATION PROCESSES.

4.2 INSTRUMENTATION.

4.3 MASS SPECTRAL DATA.

4.4 REPRESENTATION OF FRAGMENTATION PROCESSES.

4.5 FACTORS GOVERNING FRAGMENTATION PROCESSES.

4.6 EXAMPLES OF COMMON TYPES OF FRAGMENTATION.

5 NUCLEAR MAGNETIC RESONANCE (NMR) SPECTROSCOPY.

5.1 THE PHYSICS OF NUCLEAR SPINS AND NMR INSTRUMENTS.

5.2 CONTINUOUS WAVE (CW) NMR SPECTROSCOPY.

5.3 FOURIER-TRANSFORM (FT) NMR SPECTROSCOPY.

5.4 CHEMICAL SHIFT IN 1H NMR SPECTROSCOPY.

5.5 SPIN-SPIN COUPLING IN 1H NMR SPECTROSCOPY.

5.6 ANALYSIS OF 1H NMR SPECTRA.

5.7 RULES FOR SPECTRAL ANALYSIS.

6 13C NMR SPECTROSCOPY.

6.1 COUPLING AND DECOUPLING IN 13C NMR SPECTRA.

6.2 DETERMINING 13C SIGNAL MULTIPLICITY USING DEPT.

6.3 SHIELDING AND CHARACTERISTIC CHEMICAL SHIFTS IN 13C NMR SPECTRA.

7 MISCELLANEOUS TOPICS.

7.1 DYNAMIC PROCESSES IN NMR - THE NMR TIME-SCALE.

7.2 THE EFFECT OF CHIRALITY.

7.3 THE NUCLEAR OVERHAUSER EFFECT (NOE).

7.4 TWO DIMENSIONAL NMR.

7.5 THE NMR SPECTRA OF "OTHER NUCLEI".

7.6 SOLVENT - INDUCED SHIFTS.

8 DETERMINING THE STRUCTURE OF ORGANIC MOLECULES FROM SPECTRA.

9 PROBLEMS.

9.1 ORGANIC STRUCTURES FROM SPECTRA.

9.2 THE ANALYSIS OF MIXTURES.

9.3 PROBLEMS IN 2-DIMENSIONAL NMR.

9.4 NMR SPECTRAL ANALYSIS.

APPENDIX.

INDEX.

By Lloyd R. Snyder (Technicon Instruments Corp.), Joseph J. Kirkland (E. I. du Pont de Nemours & Co.), John W. Dolan (LC Resources) Hardcover912 pagesDecember 2009, ©2010


The latest edition of the authoritative reference to HPLC

High-performance liquid chromatography (HPLC) is today the leading technique for chemical analysis and related applications, with an ability to separate, analyze, and/or purify virtually any sample. Snyder and Kirkland's Introduction to Modern Liquid Chromatography has long represented the premier reference to HPLC. This Third Edition, with John Dolan as added coauthor, addresses important improvements in columns and equipment, as well as major advances in our understanding of HPLC separation, our ability to solve problems that were troublesome in the past, and the application of HPLC for new kinds of samples.

This carefully considered Third Edition maintains the strengths of the previous edition while significantly modifying its organization in light of recent research and experience. The text begins by introducing the reader to HPLC, its use in relation to other modern separation techniques, and its history, then leads into such specific topics as:

• The basis of HPLC separation and the general effects of different experimental conditions
• Equipment and detection
• The column—the "heart" of the HPLC system
• Reversed-phase separation, normal-phase chromatography, gradient elution, two-dimensional separation, and other techniques
• Computer simulation, qualitative and quantitative analysis, and method validation and quality control
• The separation of large molecules, including both biological and synthetic polymers
• Chiral separations, preparative separations, and sample preparation
• Systematic development of HPLC separations—new to this edition
• Troubleshooting tricks, techniques, and case studies for both equipment and chromatograms

Designed to fulfill the needs of the full range of HPLC users, from novices to experts, Introduction to Modern Liquid Chromatography, Third Edition offers the most up-to-date, comprehensive, and accessible survey of HPLC methods and applications available.

PREFACE.

GLOSSARY OF SYMBOLS AND ABBREVIATIONS.

1 INTRODUCTION.

1.1 Background Information.

1.2 A Short History of HPLC.

1.3 Some Alternatives to HPLC.

1.4 Other Sources of HPLC Information.

References.

2 BASIC CONCEPTS AND THE CONTROL OF SEPARATION.

2.1 Introduction.

2.2 The Chromatographic Process.

2.3 Retention.

2.4 Peak Width and the Column Plate Number N.

2.5 Resolution and Method Development.

2.6 Sample Size Effects.

2.7 RELATED TOPICS.

References.

3 EQUIPMENT.

4 DETECTION.

5 THE COLUMN.

6 REVERSED-PHASE CHROMATOGRAPHY FOR NEUTRAL SAMPLES.

7 IONIC SAMPLES: REVERSED-PHASE, ION-PAIR, AND IONEXCHANGE CHROMATOGRAPHY.

8 NORMAL-PHASE CHROMATOGRAPHY.

9 GRADIENT ELUTION.

10 COMPUTER-ASSISTED METHOD DEVELOPMENT.

11 QUALITATIVE AND QUANTITATIVE ANALYSIS.

12 METHOD VALIDATION.

13 BIOCHEMICAL AND SYNTHETIC POLYMER SEPARATIONS.

14 ENANTIOMER SEPARATIONS.

15 PREPARATIVE SEPARATIONS.

16 SAMPLE PREPARATION.

17 TROUBLESHOOTING.

APPENDIX I. PROPERTIES OF HPLC SOLVENTS.

I.1 Solvent-Detector Compatibility.

I.1.1 UV Detection.

I.1.2 RI Detection.

I.1.3 MS Detection.

I.2 Solvent Polarity and Selectivity.

I.3 Solvent Safety.

References.

APPENDIX II. PREPARING BUFFERED MOBILE PHASES.

II.1 Sequence of Operations.

II.2 Recipes for Some Commonly Used Buffers.

Reference.

Index.

By Stephen Richards, John HollertonHardcover228 pagesFebruary 2011

This book describes the use of NMR spectroscopy for dealing with problems of small organic molecule structural elucidation. It features a significant amount of vital chemical shift and coupling information but more importantly, it presents sound principles for the selection of the techniques relevant to the solving of particular types of problem, whilst stressing the importance of extracting the maximum available information from the simple 1-D proton experiment and of using this to plan subsequent experiments. Proton NMR is covered in detail, with a description of the fundamentals of the technique, the instrumentation and the data that it provides before going on to discuss optimal solvent selection and sample preparation. This is followed by a detailed study of each of the important classes of protons, breaking the spectrum up into regions (exchangeables, aromatics, heterocyclics, alkenes etc.). This is followed by consideration of the phenomena that we know can leave chemists struggling; chiral centres, restricted rotation, anisotropy, accidental equivalence, non-first-order spectra etc.  Having explained the potential pitfalls that await the unwary, the book then goes on to devote chapters to the chemical techniques and the most useful instrumental ones that can be employed to combat them.

A discussion is then presented on carbon-13 NMR, detailing its pros and cons and showing how it can be used in conjunction with proton NMR via the pivotal 2-D techniques (HSQC and HMBC) to yield vital structural information. Some of the more specialist techniques available are then discussed, i.e. flow NMR, solvent suppression, Magic Angle Spinning, etc. Other important nuclei are then discussed and useful data supplied. This is followed by a discussion of the neglected use of NMR as a tool for quantification and new techniques for this explained. The book then considers the safety aspects of NMR spectroscopy, reviewing NMR software for spectral prediction and data handling and concludes with a set of worked Q&As.

TABLE OF CONTENTS :

Introduction.

1 Getting Started.

The Technique.
Instrumentation.
CW Systems.
FT Systems.
Origin of the Chemical Shift.
Origin of "Splitting".
Integration.

2 Preparing the Sample.

How much sample do I need?
Solvent Selection.
Deutero Chloroform (CDCl3).
Deutero Dimethyl Sulfoxide (DMSO).
Deutero Methanol (CD3OD).
Deutero water (D2O).
Deutero Benzene (C6D6).
Carbon Tetrachloride (CCl4).
Trifluoroacetic acid (CF3COOH).
Using Mixed Solvents.
Spectrum Referencing (Proton NMR).
Sample Preparation.
Filtration.

3 Spectrum Acquisition.

Number of Transients.
Number of Points.
Spectral Width.
Acquisition Time.
Pulse Width.
Relaxation Delay.
Number of Increments.
Shimming.
Tuning and Matching.
Frequency Lock.
Run unlocked.
Internal lock.
External lock.
To Spin or Not to Spin.

4 Processing.

5 Interpreting Your Spectrum.

6 Delving Deeper.

7 Further Elucidation Techniques – Part 1.

8 Further Elucidation Techniques – Part 2.

9 Carbon-13 NMR Spectroscopy.

10 Some of the Other Tools.

HPLC-NMR.

Flow NMR.

Solvent Suppression.

MAS (Magic Angle Spinning) NMR.

Other 2-D Techniques.

INADEQUATE.

J-Resolved.

DOSY.

3-D Techniques.

11 Some of the Other Nuclei.

12 Quantification. 

13 Safety. 

14 Software.

15 Problems.

Hints.

Answers.

Glossary.

Index.

Features

• Describes the techniques and instrumentation of HPLC analysis, such as gradient elution and computer-assisted methods, HPLC/mass spectrometry, HPLC/nuclear magnetic resonance spectrometry, HPLC with photodiode array detection, HPLC chiral analysis, and much more
• Discusses how HPLC is used for analyzing herbal drugs and dietary supplements
• Explores the application of HPLC to primary and secondary plant metabolites, including carbohydrates, lipids, amino acids, peptides, proteins, shikimic acid derivatives, coumarins, flavonoids, lignans, isoprenoids, diterpenes, tripenes, polyterpenes, steroids, iridoids, amino acid derivatives, alkaloids, polyacetylenes, and quinoids
• Draws on the unparalleled expertise of an international team of contributors

 

Summary

The powerful, efficient technique of high performance liquid chromatography (HPLC) is essential to the standardization of plant-based drugs, identification of plant material, and creation of new herbal medicines. Filling the void in this critical area, High Performance Liquid Chromatography in Phytochemical Analysis is the first book to give a complete description of the techniques, materials, and instrumentation of column HPLC and its application to essentially all primary and secondary plant metabolites. Hailing from around the world and with vast expertise in HPLC phytochemical analysis, the contributors present a global, authoritative view of the field.

 

The book looks at the role of HPLC in the analysis of herbal drugs, quality control of plant products in dietary supplements, and chemosystematics. It also covers the phytochemistry, pharmacology, and biological role of plant metabolites as well as various modes and techniques of HPLC analysis. The book then focuses on HPLC separation, identification, and quantification of particular classes of compounds in a variety of sample types, including plants, plant extracts, and plant-derived products.

 

Along with its companion volume Thin Layer Chromatography in Phytochemistry, this comprehensive book presents the most important analytical approaches used in phytochemical analysis. It will help in solving problems connected with practical separations and the analyses of plant extract fractions of active metabolites.

PART I
Overview of the Field of Column High Performance Liquid Chromatography in Phytochemical Analysis and the Structure of the Book,

Herbal Drugs and the Role of Chromatographic Methods in Their Analysis,

Plant Products in Nutrition and Dietary Supplements: Quality Control,

HPLC in Chemosystematics,

Phytochemistry, Phytopharmacology, and the Biological Role of Plant Metabolites,

Sample Preparation of Plant Material,

Stationary Phases and Columns in Analysis of Primary and Secondary Metabolites,

Separation of Nonionic Analytes: Reversed- and Normal-Phase HPLC,

Separation of Ionic Analytes: Reversed-Phase, Ion-Pair, Ion-Exchange, and Ion-Exclusion HPLC,

Gradient Elution and Computer-Assisted Method Development,

LC-MS as a Method of Identification and Quantification of Plant Metabolites,

LC-NMR and Related Techniques for the Rapid Identification of Plant Metabolites,

Photodiode Array (PDA) and Other Detection Methods in HPLC of Plant Metabolites, Quantitative Analysis—Method Validation—Quality Control,

Confirmation of Chirality of Some Natural Products by the HPLC Method,

PART II
Primary Metabolites

Secondary Metabolites—Shikimic Acid Derivatives

Secondary Metabolites—Isoprenoids

Secondary Metabolites—Amino Acid Derivatives

Secondary Metabolites—Compounds Derived from Acetogenine (Acetylocoenzyme A)

Index

Ganapathy Subramanian (Editor)
Hardcover641 pages

Thoroughly revised, with either entirely new or completely updated contents, this is a practical manual for the small and large-scale preparation of enantiomerically pure products. The result is a vital resource for meeting the highest purity standards in the manufacture of chiral pharmaceuticals, food additives and related compounds. All the approaches covered here are highly relevant to modern manufacturing and quality control schemes in the pharmaceutical and biotech industries, addressing the increasingly important issue of drug safety in view of tougher regulatory standards worldwide.


Preface.

List of Contributors.

1 Method Development and Optimization of Enantioseparations Using Macrocyclic Glycopeptide Chiral Stationary Phases (Thomas E. Beesley and J.T. Lee).

2 Role of Polysaccharides in Chiral Separations by Liquid Chromatography and Capillary Electrophoresis (Imran Ali and Hassan Y. Aboul-Enein).

3 Analytical and Preparative Potential of Immobilized Polysaccharide-derived Chiral Stationary Phases (Tong Zhang and Pilar Franco).

4 Chiral Separations Using Supercritical Fluid Chromatography (Karen W. Phinney and Rodger W. Stringham).

5 Chiral Separation by Ligand Exchange (Gerald Gübitz and Martin G. Schmid).

6 Advances in Simulated Moving Bed Chromatographic Separations (Pedro Sá Gomes, Mirjana Minceva, Luís S. Pais, and Alírio E. Rodrigues).

6.1 Introduction.

6.2 Modeling Strategies.

6.3 Simulation.

6.4 Novel SMB Configurations.

6.5 Improvements in Operation Conditions Evaluation (Separation Volume Method).

6.6 Conclusions.

References.

7 Less Common Applications of Enantioselective HPLC Using the SMB Technology in the Pharmaceutical Industry (Stefanie Abel and Markus Juza).

7.1 Introduction – From an Emerging Technology to a Classical Unit Operation.

7.2 Unbalanced Separations and Multi-component Separations Using SMB.

7.3 Unusual Isotherms and Adsorption Behavior.

7.4 Applications of Various Column Configurations.

7.5 Application of Solvent Gradients.

7.6 Chemistry and Racemization.

7.7 Future Developments.

7.8 Conclusion.

Notation.

Greek Letters.

Subscripts.

Acknowledgments.

References.

8 Enantiomer Separation by Chiral Crown Ether Stationary Phases (Myung Ho Hyun).

9 Enantioselective Separation of Amino Acids and Hydroxy Acids by Ligand Exchange with Copper(II) Complexes in HPLC (Chiral Eluent) and in Fast Sensing Systems (Rosangela Marchelli, Roberto Corradini, Gianni Galaverna, Arnaldo Dossena, Francesco Dallavalle, and Stefano Sforza).

10 Enantiomer Separation by Capillary Electrophoresis (Gerhard K. E. Scriba).

11 Counter-current Chromatography in the Separation of Enantiomers (Eva Pérez and Cristina Minguillón).

12 Separation of Enantiomers Using Molecularly Imprinted Polymers (Börje Sellergren).

13 Enantioselective Biosensors (Raluca-Ioana Stefan-van Staden, Jacobus Frederick van Staden, and Hassan Y. Aboul-Enein).

14 Chiral Analysis in Capillary Electrochromatography (CEC) and CEC Coupled to Mass Spectrometry (Jie Zheng and Shahab A. Shamsi).

15 Chiral Analysis Using Polymeric Surfactants in Micellar Electrokinetic Chromatography (MEKC) and MEKC Coupled to Mass Spectrometry (Syed A. A. Rizvi and Shahab A. Shamsi).

16 Polarimeter Chiral Detectors in Enantioseparations (Gary W. Yanik).

17 Preparative Chiral Chromatography – a Powerful and Efficient Tool in Drug Discovery

This fourth edition of the classic guide for every user of gas chromatographic instrumentation is now updated to include such new topics as fast GC using narrow, short columns, electronic pressure control, and basic aspects of quantitative gas chromatography.

The author shares his many years of experience in technical support for gas chromatography users, addressing the most common problems, questions and misconceptions in capillary gas chromatography. He structures and presents the material in a concise and practical manner, suitable even for the most inexperienced user without any detailed knowledge of chemistry or chromatography.

For lab technicians in chemistry, analytical, food, medicinal and environmental chemists, pharmaceutists.


Table Of Contents :

Preface.

Intentions and Introduction.

1 Introduction to Capillary Gas Chromatography.

1.1 What Is Gas Chromatography?

1.2 What Types of Compounds Are Suitable for GC Analysis?

1.3 The Basic Parts of a Gas Chromatograph.

1.4 The Chromatogram.

1.5 The Mechanism of Compound Separation.

1.6 Factors Affecting Separation.

2 Basic Definitions and Equations.

3 Capillary GC Columns: Tubing.

4 Capillary GC Columns: Stationary Phases.  

5 Capillary GC Columns: Dimensions.

6 Carrier Gas.

7 Injectors.

8 Detectors.

8.1 Introduction.

8.2 Detector Characteristics.

8.3 Flame Ionization Detector (FID).

8.4 Nitrogen-Phosphorus Detector (NPD).

8.5 Electron Capture Detector (ECD).

8.6 Thermal Conductivity Detector (TCD).

8.7 Flame Photometric Detector (FPD).

8.8 Mass Spectrometers (MS).

9 Column Installation.

10 Column Test Mixtures.

11 Causes and Prevention of Column Damage.

11.1 Causes of Column Damage and Performance Degradation.

11.2 Column Breakage.

11.3 Thermal Damage.

11.4 Oxygen Damage.

11.5 Chemical Damage.

11.6 Column Contamination.

11.7 Solvent Rinsing Columns.

11.8 Guard Columns and Retention Gaps.

11.9 Packed Injector Liners.

11.10 Gas Impurity Traps.

11.11 Column Storage.

11.12 Column Repair.

12 Troubleshooting Guidelines, Approaches and Tests.

13 Common Capillary GC Problems and Probable Causes.

13.1 Using This Troubleshooting Guide.

13.2 Troubleshooting Checklist and Pre-Work.

13.3 Baseline Problems.

13.4 Peak Shape Problems.

13.5 Split Peaks.

13.6 Negative Peaks.

13.7 Excessively Broad Solvent Front.

13.8 Loss of Resolution.

13.9 Retention Changes.

13.10 Peak Size Problems.

13.11 Extra or Ghost Peaks (Carryover).

13.12 Rapid Column Deterioration.

13.13 Quantitation Problems.

Appendix A Terms.

Appendix B Equations.

Appendix C Mass, Volume and Length Unit Conversions.

Appendix D Column Bleed Mass Spectra.

Appendix E The Basics of High Speed GC Using Small Diameter Columns.

E.1 Introduction.

E.2 Column Considerations.

E.3 Carrier Gas Considerations.

E.4 Injector Considerations.

E.5 Detector and Data System Considerations.

E.6 GC Oven Considerations.

E.7 Sample Considerations.

E.8 An Example of High Speed GC Using a Small Diameter Column.

E.9 High Speed GC Summary.

Appendix F Basic Quantitative Capillary GC.

F.1 Intentions.

F.2 De. nitions.

F.3 Concentration.

F.4 Density (ρ).

F.5 Calibration for Quantitative Purposes.

F.6 Quantitation Calculations.

F.7 Techniques for Preparation of Analytical Standards for GC.

References.

Subject Index.

Joachim Ermer (Editor), John H. McB. Miller (Editor) Hardcover418 pages

Adopting a practical approach, the authors provide a detailed interpretation of the existing regulations (GMP, ICH), while also discussing the appropriate calculations, parameters and tests. The book thus allows readers to validate the analysis of pharmaceutical compounds while complying with both the regulations as well as the industry demands for robustness and cost effectiveness.

Following an introduction to the basic parameters and tests in pharmaceutical validation, including specificity, linearity, range, precision, accuracy, detection and quantitation limits, the text focuses on a life-cycle approach to validation and the integration of validation into the whole analytical quality assurance system. The whole is rounded off with a look at future trends.

With its first-hand knowledge of the industry as well as regulating bodies, this is an invaluable reference for analytical chemists, the pharmaceutical industry, pharmaceutists, QA officers, and public authorities.

Table of Contents :

Preface.

List of Contributors.

Part I: Fundamentals of Validation in Pharmaceutical Analysis.

1 Analytical Validation within the Pharmaceutical Environment (Joachim Ermer).

2 Performance Parameters, Calculations and Tests.

3 Case Study: Validation of an HPLC-Method for Identity, Assay, and Related Impurities (Gerd Kleinschmidt).

Part II: Life-cycle Approach to Analytical Validation.

4 Qualification of Analytical Equipment (David Rudd).

5 Validation During Drug Product Development – Considerations as a Function of the Stage of Drug Development (Martin Bloch).

6 Acceptance Criteria and Analytical Variability (Hermann Watzig).

7 Transfer of Analytical Procedures (Mark Broughton and Joachim Ermer (Section 7.3)).

8 Validation of Pharmacopoeial Methods (John H. McB. Miller).

9 Analytical Procedures in a Quality Control Environment (Raymond A. Cox).

10 Aberrant or Atypical Results (Christopher Burgess).

11 Future Trends in Analytical Method Validation (David Rudd).

Index.

Hans-Joachim HübschmannHardcover736 pages

"The most important advantage [of this text] is that it has not only been written for the practitioner, but also the analyst who wishes to familiarize himself with any or all the aspects of GC/MS."
—AFS - Advances In Food Sciences

An updated edition of its bestselling predecessor, Handbook of GC/MS: Fundamentals and Applications offers broad coverage of the subject, from sample preparation to the evaluation of MS-Data. This edition boasts several new chapters, including Automated Solvent Extraction (ASE), Hyphenation with Isotope Ratio MS, and the TOF-technique.

1. Introduction.

2. Fundamentals.

2.1. Sample Preparation.

2.2. Gas Chromatography.

2.3. Mass Spectrometry.

2.4. Special Aspects of GC/MS Coupling.

3. Evaluation of GC/MS Analyses.

3.1. Display of Chromatograms.

3.2. Substance Identification.

3.3. Quantitation.

3.4. Frequently Occurring Impurities.

4. Applications.

4.1. Air Analysis According to EPA Method TO-14.

4.2. BTEX Using Headspace GC/MS.

4.3. Simultaneous Determination of Volatile Halogenated Hydrocarbons and BTEX.

4.4. Static Headspace Analysis of Volatile Priority Pollutants.

4.5. MAGIC 60 - Analysis of Volatile Organic Compounds

4.6. irm-GC/MS of Volatile Organic Compounds Using Purge and Trap Extraction.

4.7. Vinyl Chloride in Drinking Water.

4.8. Chloral Hydrate in Surface Water.

4.9. Field Analysis of Soil Air.

4.10. Residual Monomers and Polymerisation Additives.

4.11. Geosmin and Methylisoborneol in Drinking Water.

4.12. Substituted Phenols in Drinking Water.

4.13. GC/MS/MS Target Compound Analysis of Pesticide residues in Difficult Matrices.

4.14. Multi-component Pesticide Analysis by MS/MS.

4.15. Multi-method for the Determination of 239 Pesticides.

4.16. Nitrophenol Herbicides in Water.

4.17. Dinitrophenol Herbicides in Water.

4.18. Hydroxybenzonitrile Herbicides in Drinking Water.

4.19. Routine Analysis of 24 PAHs in Water and Soil.

4.20. Fast GC Quantification of 16 EC Priority PAH Components.

4.21. Analysis of Water Contaminants by On-line SPE-GC/MS.

4.22. Determination of Polar Aromatic Amines by SPME.

4.23. Congener Specific Isotope Analysis of Technical PCB Mixtures.

4.24. Polychlorinated Biphenyls in Indoor Air.

4.25. Confirmation Analysis of Dioxins and Dioxin-like PCBs.

4.26. Fast GC Analysis for PCBs.

4.27. Analysis of Brominated Flame Retardants PBDE.

4.28. Trace Analysis of BFRs in Waste Water Using SPME-GC/MS/MS.

4.29. Analysis of Military Waste.

4.30. Detection of Drugs in Hair.

4.31. Detection of Morphine Derivatives.

4.32. Detection of Cannabis Consumption.

4.33. Analysis of Steroid Hormones Using MS/MS.

4.34. Determination of Prostaglandins Using MS/MS.

4.35. Detection of Clenbuterol by CI.

4.36. General Unknown Toxicological-chemical Analysis.

4.37. Clofibric Acid Aquatic Systems.

4.38. Polycyclic Musks in Waste Water.

4.39. Identification and Quantification of Trichothecene Mycotoxins.

4.40. Highly Sensitive Screening and Quantification of environmental Components Using Chemical Ionisation with Water.

4.41. Characterization of Natural Waxes by Pyrolysis-GC/MS.

4.42. Quantitative Determination of Acrylate Copolymer Layers.

5. Glossary.

Subject Index.