Principles and Practice of Bioanalysis, Second Edition PDF
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PRINCIPLES AND PRACTICE OF BIOANALYSIS Second Edition 3857.indb 1 1/11/08 12:14:47 PM 3857.indb 2 1/11/08 12:14:47 PM PRINCIPLES AND PRACTICE OF BIOANALYSIS Second Edition Richard F. Venn Boca Raton London New York CRC Press is an imprint of the Taylor & Francis Group, an informa business 3857.indb 3 1/11/08 12:14:47 PM CRC Press Taylor & Francis Group 6000 Broken Sound Parkway NW, Suite 300 Boca Raton, FL 33487-2742 © 2008 by Taylor & Francis Group, LLC CRC Press is an imprint of Taylor & Francis Group, an Informa business No claim to original U.S. Government works Version Date: 20110715 International Standard Book Number-13: 978-1-4200-0560-8 (eBook - PDF) This book contains information obtained from authentic and highly regarded sources. Reasonable efforts have been made to publish reliable data and information, but the author and publisher cannot assume responsibility for the validity of all materials or the consequences of their use. 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Visit the Taylor & Francis Web site at http://www.taylorandfrancis.com and the CRC Press Web site at http://www.crcpress.com Contents Preface to the Second Edition ..........................................................................................................vii Preface to the First Edition ...............................................................................................................ix About the Editor ................................................................................................................................xi Contributors ...................................................................................................................................xiii Chapter 1 Physicochemical Properties of Drugs and Metabolites and Their Impact on Bioanalysis ...................................................................................................................1 Hugh Wiltshire and Angus Nedderman Chapter 2 Sample Preparation ....................................................................................................19 Christopher A. James Chapter 3 Basic HPLC Theory and Practice ..............................................................................41 Andy Gray and Peter Lawrence Chapter 4 HPLC Optimisation ...................................................................................................69 David Bakes Chapter 5 HPLC Detectors .........................................................................................................99 Kenneth C. Saunders and Richard F. Venn Chapter 6 Gas Chromatography: What It Is and How We Use It .............................................123 Peter Andrew and Mira V. Doig Chapter 7 Thin-Layer Chromatography ...................................................................................141 Hugh Wiltshire and Angus Nedderman Chapter 8 Immunoassay Techniques ........................................................................................151 Richard F. Venn Chapter 9 Automation of Sample Preparation ..........................................................................177 Kenneth C. Saunders and Christopher A. James Chapter 10 Fundamental Aspects of Mass Spectrometry ..........................................................193 Mira V. Doig and David M. Higton v 3857.indb 5 1/11/08 12:14:48 PM vi Principles and Practice of Bioanalysis, Second Edition Chapter 11 Quantitative LC–MS ................................................................................................223 David M. Higton and Mira V. Doig Chapter 12 Mass Spectrometric Identification of Metabolites ...................................................237 Gordon Dear Chapter 13 Nuclear Magnetic Resonance in Drug Metabolism .................................................261 Phil Gilbert Chapter 14 Metabolite Isolation ..................................................................................................285 Gordon Dear, Angus Nedderman, and Hugh Wiltshire Chapter 15 Strategy for the Development of Quantitative Bioanalytical Procedures ................303 David Bakes Index ..............................................................................................................................................317 3857.indb 6 1/11/08 12:14:48 PM Preface to the Second Edition Over the 7 years since the first edition of Principles and Practice of Bioanalysis was published, bioanalytical methodologies have remained largely the same. Liquid chromatography is still pre- eminent as a means of separating out the analytes of interest, and this is still usually preceded by an extraction step. What has changed dramatically is the endpoint: the detector. Today, almost every small-molecule analytical method in the pharmaceutical industry relies on triple-quadrupole mass- spectrometry for selective detection of the analyte. Advances in quadrupole design, coupled with advances in ionisation techniques, have allowed huge leaps in sensitivity as well as permitting higher flow rates into the analyser; combined, these bring unprecedented sensitivity and selectivity to mass spectrometry. The corollary is that sample cleanup is less important, in turn allowing fast, online sample workup. Very few methods now rely on UV, fluorescence, or other detection methods. The drivers for all these innovations have been largely twofold: the desire for greater sensitiv- ity—to allow smaller sample volumes to be analysed or to enable smaller doses of experimental medicines to be administered—and the need for greater throughput and faster analysis. We have omitted one chapter entirely from this second edition—that on capillary electro- phoresis (CE). This is now entirely a niche technique and is barely used for quantitative bioanalysis. The chapter on CE in the first edition may be referred to if necessary. At one time it appeared that immunoassay might also become an obsolete method, but until greater advances are made in mass spectrometers and their associated data systems, the technique remains indispensable for a number of biomarkers and, of course, for the high molecular-weight biological analytes such as proteins and, in particular, therapeutic antibodies. All the chapters in this edition have been overhauled or rewrit- ten to reflect modern practice by authors who are expert practitioners in their field. Thus this second edition reflects modern practice in bioanalysis, largely in the pharmaceutical industry, and mainly in drug metabolism and pharmacokinetics laboratories. The course that the book originally derived from (see the preface to the first edition) is still running on a biennial basis, rooting the authors in modern practice. We hope that this second edition is as well-received as the first and will provide a useful intro- duction, starting point, and reference for both students and bioanalysts beginning their careers in a crucial field. Richard F. Venn vii 3857.indb 7 1/11/08 12:14:48 PM 3857.indb 8 1/11/08 12:14:48 PM Preface to the First Edition We hope you enjoy this book and find it helpful and informative. Analysis—and in particular, bioanalysis—is a vital part of life today. It is fundamental to our increasing understanding of the complexities we meet in our universe (from microscopic to cosmic). It is also fundamental to our daily lives as members of a regulated society. Almost every industry or activity is subject to regulation: analysis of compounds (pollutants, toxins, endogenous substances, drugs (medicinal or recreational), growth agents, herbicides, pesticides…the list is endless) in the relevant matrix (soil, plasma, tissues, cerebrospinal fluid, urine, meat, cereal, water, etc.) is an essen- tial part of complying with these regulations. While the examples used in the book are drawn from the pharmaceutical world, the analytes and matrices discussed will not be very different form those being studied elsewhere. The book may be used as a reference to specific techniques, as a guide to assist the analyst in achieving the desired end result (a sufficiently sensitive and selective analytical method suited to the analyte and matrix under investigation) or as a textbook for the student of bioanalysis or metabolism. As such it will be of much wider use than merely for those involved in the pharmaceutical industry. Almost every chemistry and biochemistry student (undergraduate and postgraduate) will need to use the techniques described in this book at some time in their student life; some will use them throughout their careers. Thus we hope that this book will fill a gap and provide some basic instruction in what is a central part of our world today. The genesis of this book lies in the history of the Drug Metabolism Discussion Group (DMDG), an umbrella organisation set up by those involved in drug metabolism within the British pharma- ceutical industry. Major aims of the DMDG are to encourage co-operation and training in drug metabolism within the industry. One incentive for this is that there is no university course in drug metabolism; graduates (and, to a lesser extent, postgraduates) coming into drug metabolism depart- ments require specialist training. Out of this grew the DMDG and a number of courses, for example the basic training course, the clinical and pre-clinical pharmacokinetics courses, the immunoassay course and the methods for bioanalysis and metabolism course. This latter course was first run in 1992 and has run every other year since then, proving popu- lar and successful. The aims of the course are to provide attendees with sufficient basic knowl- edge and background of bioanalysis to enable them to tackle the difficult analytical problems they face in a drug metabolism department such as pharmacokinetic determinations and metabolite identification. Individual lecturers and tutors on the course are drawn from drug metabolism departments throughout the pharmaceutical industry and are usually specialists in their fields. Each lecture and tutorial was devised in consultation with all the other lecturers and the course is regularly updated as a result of the feedback obtained from delegates at each course. In this way we have tried to keep the course fresh, stimulating and up to date; we hope that the book reflects this, being, in essence, the course manual of the methods for bioanalysis and metabolism course. The notes from each lecture have been overhauled and edited to make a coherent whole and the order of the chapters is very similar to the order in which the lectures and tutorials on the course are given. We start with an explanation of the importance of the physicochemical properties of various analytes. This is then related to extraction and analysis. From there the principles of the major analytical technique of liquid chromatography are dealt with, focusing on optimisation and detection methods. Richard F. Venn ix 3857.indb 9 1/11/08 12:14:48 PM
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