Analyst, September 1996, Vol. 121 129N Book and Video Reviews Principal Components Video Course: A, Principal Com- ponents as Display Method; B, Display Variables and Relationships Between Variables and Objects; C, Sin- gular Value Decomposition, Eigenvalues, Evolving Fac- tor Analysis, Software and Exercises; D, The Display of Latent Variables in Tabulated Data (Complete Set VHS PAL). By D. L. Massart and P. J. Lewi. Elsevier. 1994. Total running time 233 min. Price Dfl1750.00; US$lOOO.OO. ISBN 0-444-81622-4. This course comes in the form of four videos, each approxi- mately one hour in length, a manual to accompany the videos and software, a tutorial version of the package Spectramap and a Matlab program for principal-components analysis (PCA). The-videos consist primarily of a series of slides (presumably developed over the years for use in a number of lecture courses), together with a slide by slide commentary by the two authors and a third narrator.Occasional soft music is played in the background, and there are some very short clips of the two authors in a library making comments at the beginning, and occasionally in the middle, of each video. The manual is primarily a list of slides, with selected diagrams from the slides and selected text from the commentary. The appendix to the manual describes some Spectramap examples and the Matlab PCA program. Video A begins with a descriptive introduction to PCA. An uninitiated user may gain some misapprehensions from this part, especially the implication that the number of variables is less than the number of objects, matrices being long thin matrices; in many areas of chemometrics, quite the reverse situation is encountered.The second part of this video is a list of examples where PCA has been applied. Although many of them are interesting, they are presented in a very descriptive manner, with little extra insight. Several of the original references are to journals that are not easily accessible; although this is perfectly acceptable in research, for tutorial material, the source refer- ences of the case studies should be very easy to find. Part B concentrates primarily on loading plots. Some dangerous oversimplifications are presented. For example, the statement that PC 1 is an indicator of size and PC2 of contrast only applies to a very specific type of problem.Assumptions that column centring is routine may mislead the listener. Some statisticians invent names such as SMA (spectral map analysis) and CFA (correspondence factor analysis) for PCA on preprocessed data, whereas others simply use the generic term PCA and report the method of preprocessing (this is very common in the chemical literature when uncentred PCA is used; this approach really looks for very different patterns in data from column centred PCA but has not been given a special name). The idea of a vector is introduced about a third of the way through this tape, perhaps rather late in the series. According to the introduction, tape C is primarily about mixture analysis. Many analytical chemists will be disappointed by the scope which is restricted to one variant of EFA (evolving factor analysis) and the two component problem of detection of a small impurity.Some rather unusual assumptions, that data is normally centred down the columns, the number of columns is larger than the number of rows, eigenvalues measure variance (only true if the columns are not centred), that the number of significant PCs in EFA should equal the number of significant compounds in a mixture (not true if there are stereoisomers with identical spectra) and that the scores should be computed in the direction of elution time (this can result in serious problems if data are centred) are introduced. Although this is supposed to be a tutorial and not a research video, very detailed, and excellent, discussion of the influence of data scaling and preprocessing is introduced in other contexts, so it is a pity that this important aspect is not also described in the tape on EFA.This section concludes with some useful mathematical descriptions, but one overall difficulty is a difference in notation in different parts of the videocourse, leading to ambiguities, such as the use of h for wavelength and eigenvalue, and different notations for load- ings. This aspect could easily have been edited out. The final tape is a very detailed analysis of a clinical case study. A weakness of the video is that the two very eminent chemometricians are primarily interested in pharmaceutical chemistry and perhaps assume that the audience will have an equally detailed interest; perhaps if a non-pharmacist had joined the team a better perspective may have been gained.Hence, for the general user of the course, the lengthy pharmaceutical discussion at the beginning may lose attention. Most of this tape consists of a detailed interpretation of various graphs obtained from a number of clinical and pharmacological tests on a series of drugs. There is a strong emphasis on biplots. At the end, partial least squares (PLS) is introduced. The emphasis is on PLS2. Although extremely interesting to the researcher (this case study must be one of the very best in existence), the novice will emerge with the impression that PLS is primarily a method for graphical comparison of two sets of data. There is no discussion of quantitative aspects of PLS, of errors of prediction and of comparison with univariate calibration. I think that this part of the video is far too brief and perhaps should have been omitted.The overall emphasis on the qualitative and graphically descriptive uses of PCA-based methods virtually ignores the importance of quantitation and measurement common in analytical chemistry. In my opinion, the presentation is not very high in quality for such a highly priced video. For example, several of the red slides have a dirty background; in the library, figures uncon- nected with the video sometimes move past in the background; the DOS based Spectramap is rather limited in capacity; slides are numbered in tapes A to C but not in tape D; voices are very flat and expressionless. ‘a valuable teaching aid which could use- fully be distributed more widely’ However, the authors are certainly extremely well known in the field, and the slides are a valuable teaching aid which could usefully be distributed more widely; there is a major shortage of public domain tutorial material in chemometrics.The price of the video will reduce rather than increase the audience for this work, and a more modern solution might be to make the slides, together optionally with audio commentary, available on the Internet. Alternatively, a cheaper solution for a publisher would be to produce all the slides in manual format together with simple audio cassettes. Richard G. Brereton 5190090E University of Bristol High Performance Liquid Chromatography. Fundamental Principles and Practice Edited by W. J. Lough and I.W. Wainer. Pp. xii + 276. Blackie. 1955. Price f22.50. ISBN 0-7514-0076-9. This text is edited by John Lough and Irving Wainer with contributions from nine other authors. These two editors are well known in chromatography circles and the contributing130N Analyst, September 1996, Vol. 121 authors have wide experience in HPLC. The major target audience for this book is those undergraduates undertaking courses in analytical chemistry although the editors have indicated other students who might benefit from the material. The early chapters, concerned with definitions, modes of chromatography, solvents, stationary phases and instrumenta- tion, seek to detail the essentials required for a basic understanding of HPLC. I was impressed with these sections, particularly the chapter on support materials and solvents.The details concerned with the preparation of silica and the production of chemically-bonded stationary phases were lu- cidly presented and, in my opinion, emphasize several of the most important aspects of stationary phase development and usage to those new to HPLC. Following the introductory material, there are two chapters concerned with sample preparation and method development, the latter containing a useful introduction to validation methods. The final chapters are concerned with applications of HPLC and should prove earemely valuable to the intended audience. The first two chapters in this part of the book (polymer analysis and biomedical and forensic analysis) introduce the important concept of defining the analytical problem before embarking on the development of an assay.Each of the chapters concerned with applications provide useful examples of the differing problems to be overcome in the utilisation of HPLC in the various areas. The wide variety of applications presented should enable undergraduate students to obtain a thorough grounding in HPLC techniques and the related methodologies. This book is a useful introduction to HPLC and as such fulfils the objectives laid down in the introduction. The text has a sensible balance between the theoretical basis, equipment design and practical applications of this important analytical technique. I found few typographical errors in the book, the majority of chapters were easy to read and a useful index is included.My only (minor) criticism is concerned with the bibliographies. Some chapters have no bibliography at all and in others the majority of references are pre 1990 (admittedly, given the objectives of this book, it is easy to appreciate the reasons for including many of the ‘classic’ early references). I believe this text to be a valuable addition to the range of books available to undergraduate students studying this analytical technique. .I. S . Millership 61900096 Queen’s University of Belfast Dietary Fibre Analysis By D. A. T. Southgate. RSC Food Analysis Monographs. Series editor P. S. Belton. Pp. ix + 174. Royal Society of Chemistry. 1995. Price f37.50. ISBN 0-85404-556-2. A very readable book which has clearly been written by not just an expert in the topic, but an enthusiast as well.The name of David Southgate has been associated with studies on the role and analysis of dietary carbohydrates, including dietary fibre for the past 25 years at least. Indeed it was he who devised a comprehensive scheme for the characterization of food carbo- hydrates, and the Southgate method is still the basis of one of the dietary fibre values quoted in the 1992 version of McCance and Widdowson’s ‘The Composition of Foods’. He is thus well qualified to review and assess the current options for the analysis of dietary fibre and this he does with commendable clarity and objectivity. In the preface he outlines the aims, which are to debate a strategy for analysis, discuss the principles of the method options, and thereby to allow the analyst to make sound decisions on choice of method.The first couple of chapters provide the background to the Dietary Fibre Hypothesis and to the chemistry of dietary fibre, which he describes as ‘. . . not a single analyte, but a complex mixture of variable composition’. There then follows a chapter describing and debating the various definitions and attendant methods, tracing and explain- ing their evolution to the two main ‘families’ of methods, AOAC based or Englyst based, that we have today. Next, and demonstrating the real analyst in him, he pays great attention to sampling, sample handling, and sample pretreat- ment, for without the proper start, as he quotes, ‘the most elegant and accurate methods will not provide reliable values’. To further ensure reliability he then goes on to describing the quality procedures that need to be in place.The chapters following then get down to exploring, dissecting and catalogu- ing in some detail each of the methods and their variants in turn, providing with each, data from the various collaborative studies made to test performance. As one who shares the same enthusiasm for analysis as David, I was enthralled with the insight, the understanding and the attention to detail provided. ’well presented and expertly discussed and assessed’ The concluding chapter reviews the various debates that prevail (and bedevil) the topic of dietary fibre. The continuing discord on the definition, the question of purpose for which the analysis is made, the inclusion or not of ‘resistant starch’, the collaborative comparative studies on performance, all are presented and rationally discussed. Furnished with this wealth of information, well presented and expertly discussed and assessed, the ultimate decision on choice of method is left to the analyst themself.Derek Favell 51901 0 I D Unilever Research Colworth Laboratory Bedford Mass Spectrometry in the Biological Sciences Edited by A. L. Burlingame and Steven A. Carr. Pp. xii + 570. Humana Press. 1995. Price $145.00. ISBN 0-89603-340-6. This book contains the text of twenty six papers presented at the 3rd International Symposium on Mass Spectrometry in the Health and Life Sciences held in San Francisco on 13-18th September 1994. Mass spectrometry is becoming an increasingly important technique in the biological sciences following the recent introduction of the ionisation techniques, electrospray and matrix-assisted laser desorption which have enabled mass measurements to be made on proteins, large carbohydrates and other important bipolymers.Coupling of electrospray with liquid chromatography has further added to the armoury of recent techniques for biomolecule characterization. These advances are adequately reflected in this book with most chapters describing applications of at least one of these methods. Much of this work has been in the area of peptide and protein research and such applications comprise a major section of this book. One of the most active research areas is the identification of proteins, separated on 2-dimensional electrophoretic gels, by matching the masses of parent or fragment ions from enzyme- derived peptide fragments with those obtained from published protein sequence data bases.Such methods are discussed in detail. The use of deuterium exchange reactions to probe protein structure represents another recent development that is also discussed at length. Post-translational modifications of proteins, particularly by glycosylation, is another topic that is being extensively studied by mass spectrometry and several authorsAnalyst, September 1996, Vol. 121 131N describe fragmentation and derivatization studies for obtaining detailed structural information on these complex molecules. This theme continues with studies of glycolipids including such molecules as lipid-A which have provcd to be particularly difficult to ionize by mass spectrometry, and investigations of nucleic acid structure.With much recent work being devoted to the study of biopolymers, one tends to forget that mass spectrometry, particularly when coupled with either gas or liquid chromato- graphy, is still a major tool for the analysis of small molecules. Although such work is reflected by investigations of drug metabolism, eicosanoids and the use of stable isotopes in toxicology, a more blanced view of the uses of mass spectrometry in biological sciences could have been achieved by incorporation of more papers on small molecules. Three chapters describe instrumentation and methods for improving sensitivity and include developments in time-of- flight (TOF) and ion cyclotron resonance (ICR) spectrometer design.Delayed extraction is revolutionising the use of TOF instruments by greatly improving resolution and allowing fragment ions produced in the ion source to be observed. Work with ICR instruments emphasises their potential to provide extremely high resolution and the ability to perform effective collisionally activated dissociation. ‘a valuable addition to the library of anyone working in the area of biomolecule charac- terization by mass spectrometry’ This book is very well produced and should provide a valuable addition to the library of anyone working in the area of biomolecule characterization by mass spectrometry. Many of the chapters contain useful review material, as well as recent applications of the techniques, and most record the question- and-answer sessions following presentation of the papers at the Symposium, The book concludes with author and subject indices and eleven useful appendices listing data such as atomic masses, amino acid residue masses, carbohydrate structures and fragmentation nomenclature relevant to mass spectrometry.David J . Harvey 6l90002.1 University of Oxjord Lipid Analysis By F. W. Hemming and J. N. Hawthorne. lntroduction to Biotechniques. Series editors: J. M. Graham and D. Billington. Pp. xii + 176. Bios Scientific Publishers. 1996. Price f 17.95. ISBN 1-872748-98-8. The book covers a very practical approach to lipid analysis. However, the reader should be advised that the methods are related to biochemical applications and it is not aimed at the lipid chemist.For example, sections are included that relate to the extraction of lipids from tissue, and to immunochemical methods. However, one of the strengths is that no single text has been available for those wanting to become involved in this area. The approach taken is to cover the principles of separation and chromatographic analysis in a basic chapter which extends to almost half of the text. The techniques covered include partition, adsorption ion-exchange and complexing chromato- graphy including PC, TLC, HPLC and other column methods. The approach is qualitative. The chapter includes very valuable sections on radioisotope methods and a very useful range of immunochemical technique<, including ELISA, immunostain- ing and immunoradiometric assays. These are of particular value to any biochemical analyst wanting to work in the field.This is then followed by chapters on some of the functional groups found in biochemical systems and goes into greater depth concerning the specific methods that may be used. With hydrocarbons, the text covers the full range from the biological significance and structure to quantitation. Surprisingly, from a chemical point of view, the next chapter covers alcohols, phenols, aldehydes, ketones and quinones. The reason for this is that they are often met as mixtures in a biosynthetic context and the methods covered are similar. This chapter is a little disappointing in that it does not give a great deal of practical detail that would enable newcomers to carry out analyses without further literature searches and the references to other sources are limited.The chapter on fatty acids also covers prostaglandins and this is a very useful slant to the book. This biochemical approach is continued in other chapters. For example, esters include the alkylglycerols and the phospho-containing lipids include phos- phoinositols and sphingomyelins as well as the normal compounds such as the lecithins. This is a very useful source and does give more practical details. The final two chapters cover the glycolipids and the lipoproteins of some importance to biochemists working in this area as the accounts are clear and sufficiently detailed to be of use to any analyst working in this field. ‘a useful introduction for someone entering the field and some of the coverage of more biochemical lipids would appeal to the lipid specialist’ The first of the appendices is a glossary of terms.The second shows that the authors are aware of the frustrations of working in this type of area as they have listed some 39 UK equipment suppliers, which is not complete but makes a useful starting point. The further reading list is useful but somewhat limited. The text should make a useful introduction for someone entering the field and some of the coverage of more biochemical lipids would appeal to the lipid specialist wanting further information on this aspect. C. G. Beddows 619002 7E Leeds Metropolitan University Spectroscopy with Polarized Light. Solute Alignment by Photoselection in Liquid Crystals, Polymers and Mem- branes By Josef Michl and Erik W. Thulstrup.Pp. xvi + 574. VCH. 1995. Price ca. DM98.00 (Soft cover). ISBN 1-56081-910-3 (Soft cover). ~ ___._____ ~~ ~ _ _ ~ - At a casual glance this appears to be a dauntingly theoretical book with an extremely high density of equations devoted, as the sub-title suggests, to the narrow field of polarisation spectroscopy of partially aligned molecules in matrices. On close reading this proves to be a very unfair description. It is a thorough-going account at a research level, but it is extremely well written and much more readable than expected. There is a good balance of theoretical and practical aspects. One chapter is devoted to experimental techniques of alignment and measure- ment and in fact almost half the book is devoted to applications, with a detailed and very useful worked example on pyrene.The authors cover the whole of the optical spectrum accessible to samples in matrices from the ultraviolet to the infrared and include absorption spectroscopy, fluorescence, Raman, linear and circular dichroism, magnetic circular dichroism and multiphoton processes. The fundamentals of optical spectroscopy and of polarised light are discussed in the132N Analyst, September 1996, Vol. 121 same careful way as the research frontiers. The whole approach is centred around the understanding of transition moments, and the need for correct assignment of transitions is stressed. ‘The authors clearly know their material first-hand.’ The authors clearly know their material first-hand. Both the theoretical and practical aspects are discussed critically.This critical aspect is perhaps the most lasting impression of the book: one feels comfortable with the authors’ judgement of the issues. For other than the section dealing with applications, the references are presented as a substantial and informative discussion of the relevant literature at the end of each chapter. Although the authors appear faintly defensive about this in the preface, it in fact proves to be an admirable system which avoids distractions in the text and is recommended to authors of other instructional texts. Although the content is of course different, in many ways this text is reminiscent of Herzberg’s books on spectroscopy. It is therefore not inappropriate that this ten-year-old book should have been reprinted virtually unchanged-the only new mate- rial is a handful of 1986-1988 references presumably culled from the 1989 beginners’ version of the text. The only hesitation I have in recommending it unreservedly to post-graduates and researchers in the field and to libraries, is that neither the authors nor the publishers have signalled their future intentions. Is there to be a post-1986 supplement or is there a danger of a new updated edition soon making the present one redundant? T. Threlfall 6/90019D University of York NOMINATIONS FOR THE 1997 BENEDETTI-PICHLER AWARD The American Microchemical Society is soliciting nominations for the prestigious 1 997 Benedetti-Pichler Award. The award, established in 1966, is given annually to recognise outstanding achievements in microanalytical chemistry. The award consists of a plaque and Expenses to attend the Eastern Analytical Symposium in Somerset, New Jersey, in November 1997 to receive the award at a session to honour the awardee. Nominations or further information, including at least two supporting letters should be sent no later than October 30, 1996 to: Dr Robert G. Michel Department of Chemistry University of Connecticut Storrs, CT 06269 USA Tel : +1 203 486 3143; Fax : +1 203 486 2981; E-mail : MICHEL@UCONNVM.UCONN.EDU