THE OILY PRESS

Edited by Richard O. Adlof, USDA-ARS-NCAUR, Peoria, Illinois, USA.

On this page you can read the Author's Preface, and any reviews of this book written in the scientific literature which have been sent to us. For more details of the chapters and to buy the book, please see the main Advances in Lipid Methodology web page.

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Preface | Reviews

Welcome to Advances in Lipid Methodology. This is the fifth volume in the Advances series, with a new editor (replacing the irreplaceable William Christie) and a new publisher (PJ Barnes & Associates, Bridgwater, Somerset, UK), but the objectives of this series have not changed. As noted in the prefaces of previous volumes, the goal of the Advances series is "to provide readable, up-to-date reviews of rapidly expanding areas of lipid analysis and practical examples which should be of immediate use to lipid analysts". These have been, are and will continue to be the goals of the authors and Editors of this series.

As in previous volumes of Advances, the Editor has attempted to choose leading international experts to author individual chapters. Volume 5 contains four chapters of specific methodologies of lipid analysis. Professor Yakoob D. Che Man (Faculty of Food Science & Biotechnology, Universiti Putra, Serdang, Selangor, Malaysia) describes the application of differential scanning calorimetry to study the physical properties of individual fats and oils and fats and oil blends, to relating fatty acid unsaturation and chain length to an oil's physical properties, to the detection of adulteration, to monitoring the oxidative stability of an oil and characterization of antioxidant effects in heated oils. The analysis of lipids by silver ion chromatography, a topic originally reviewed by Dr Boryana Nikolova-Damvanova (Institute of Organic Chemistry, Bulgarian Academy of Sciences, Sofia, Bulgaria) in Advances 1 (1992), has been expanded and updated by the author in Advances 5. Recent developments relating changes in sample retention patterns/resolution(s) with silver ion/solvent (Ag ion-related vs. normal phase effects)/solute form (fatty acids, fatty acid esters, TAG, etc.)/substrate interactions and the mechanisms of silver ion bonding have been applied to thin layer (TLC; one- and two-dimensional), high performance (Ag-HPLC), reversed phase (RP-HPLC), and supercritical fluid (SFC) chromatography. Specific examples of separation are included, as are such topics as TLC plate preparation/impregnation and methods of sample visualization.

The historical development of atmospheric pressure chemical ionization-mass spectrometry (APCI-MS), its utilization with HPLC as a "hyphenated technique", and its application to the characterization of complex mixtures of lipids are reviewed in depth by Dr Craig Byrdwell, Florida State University, Boca Raton, FL, USA. Areas of APCI-MS discussion include instrument configuration, theory and applications, the latter including both the qualitative and quantitative analysis of complex TAG configurational isomer mixtures, oxidized TAG, fatty acids, phospholipids and other lipid classes such as carotenoids, vitamins, and cholesterols. Concepts such as dual parallel APCI and APCI plus electrospray (ESI) MS, multiple ion probe MS, and atmospheric pressure photoionization (APPI) MS are discussed.

Another methodology discussed in Advances 1, supercritical fluid chromatography (SFC), has been updated and expanded by Dr Jerry King, Los Alamos National Laboratory, Los Alamos, New Mexico, USA. The advantages of SFC relative to GC or HPLC and its use in sample preparation and as a coupled technique are discussed, as are recent advances in analytical (both capillary and packed column), preparative and plant scale SFC. Specific applications include the characterization of TAG formulations, the isolation of lipid classes, the profiling of marine-derived oils, the detection and/or selective removal/isolation of minor seed oil components (such as estolides, cholesterols, phospholipids, free fatty acids, fat soluble vitamins), as well as their oxidation/degradation products (polymers, peroxides) and for detection of miscellaneous contaminants including herbicides, organochlorine pesticides, and antibiotics. The utilization of analytical SFC with a variety of detectors (ELSD, UV) and the inter-relationship of sorbent type with supercritical CO2 pressure and flow rates is discussed. The chapter also includes an extensive listing of SFC-related books and internet sites.

Genetically modified oils (GMOs), their regulation and perceived health problems, continue to be a "hot topic". Dr Jan Hazebroek (Pioneer Hi-Bred International, Johnston, IA, USA) provides an overview of GMOs, with emphasis on methods of analysis, including recent developments in chromatographic and spectrophotometric/colorimetric methods (GC, TLC, HPLC, MS, NMR, NIR) to characterize GMO fatty acid composition/structure (TAG profiling), as well as phospholipids, tocopherols, tocotrienols and other unexpected fatty acids. Methods of seed sampling/seed oil extraction/ derivatization (including potential sources of error) and utilization of the data to define a GMO's biological variability and potential molecular markers are also discussed.

The use of fatty acid profiling in the characterization of metabolic diseases is detailed by Professor Armand Christophe, University Hospital, Department of Endocrinology, Metabolic Diseases, Ghent, Belgium. Professor Christophe discusses the utilization of human plasma, serum or red blood cell phospholipid fatty acid profiling to diagnose such diseases as fatty acid deficiency, Refsum disease, cystic fibrosis, and extrahepatic biliary atresia. Problems in the extraction, storage and fractionation of blood lipids and lipid classes, in their derivatization and with methods of expressing the analytical results are discussed. Specific examples of fatty acid profiles and the effects of such variables as subject gender, age and season are included.

The potential consolidation of at least some of the many standard methods for analysis of fats and oils is currently an issue under serious discussion in Europe and North America. Dr James K. Daun (Program Manager, Canadian Grain Commission, Grain Research Laboratory, Winnipeg, Canada) and Mr Richard Cantrill (Technical Director, American Oil Chemists' Society, Champaign, IL, USA) present an overview of this topic, examining the purpose and types of standard methods, and their development, including sources of error, cost (instrumentation, time), formulation of standards, and validation. Other issues are discussed, such as sponsorship, formal protocol development (ISO), approval and professional associations and organizations for publication of "Official Methods" (AOAC, AOCS, IUPAC, IOC). Extensive listings of addresses, e-mail contacts (current officers, secretariats, and so on) and websites of standards writing organizations, of reference material sources, participating national standards organizations for analysis of animal and vegetable fats and oils (ISO TC 34/ SC 11) are included, as is an intercomparison of methods table.

As exemplified by the chapter on silver ion chromatography, rapid advances in analytical methodologies have resulted in the re-evaluation of chapters published in previous volumes of Advances, often as recently as 8 to 10 years ago. Future volumes of Advances will strive to update or address such wideranging topics as: the chiral separation of lipids, lipid analysis by 13C and 2H-NMR, the analysis and the characterization of phospholipids, the application of stable isotopes to lipid studies, the characterization/preparation of structured lipids, government regulations and method development for trans fatty acids in foods, characterization of low-trans/low-fat formulations, GMO regulation/worldwide impact, lipids as phytonutrients, data acquisition software in analytical chemistry and Internet resources for the analytical chemist.

We, as authors and Editor, hope we have succeeded in our continuing efforts to "provide compact readable texts on all aspects of lipid chemistry and biochemistry". In this and future volumes, we hope to provide relevant, up-todate and extensively-referenced examples of analytical methodologies and their application to the analysis and characterization of lipids. As envisioned by Bill Christie more than a decade ago, the Advances series will continue to strive to be a combination of "cookbook" and overview of lipid analytical methodologies. As always, your comments and suggestions are both solicited and welcome.

Richard O. Adlof

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Dr Eric Murphy, University of North Dakota, Grand Forks, North Dakota, USA, writing in ISSFAL Newsletter, December 2003, pp.24-25 (the newsletter of the International Society for the Study of Fatty Acids and Lipids).

This book is the fifth in the series by the Oily Press focused on methodologies used in lipid analysis. This series was started some years ago by W.W. Christie and continues today under the editorship of R.O. Adlof. The book doe Ls a good job of providing in-depth chapters covering what the editor considered as rapidly expanding areas of lipid methodologies. Of course I am not so sure that anything is rapidly expanding in the area of lipid methodologies, but then again I am a traditionalist.

Several topics are revisited from the first edition, As in the first edition, these are well covered and very readable chapters. For instance, the chapter two is on silver ion chromatography. Similar to the first edition, this chapter is very well written and put together quite as well as it was in the first edition. More importantly, this chapter adds additional information regarding the use of HPLC argentation chromatography and expands on topics found in the first edition. One disappointment with this chapter is the quality of the chromatograms in the book relative to the first edition, making them more difficult to read.

Chapter four is on APCI-mass spectrometry and is very well written. This chapter introduces the concept of MS to the non-MS person, including very detailed diagrams of the ionization process and of the instruments themselves. Analysis of triglycerides and phospholipids is covered. The authors do not cover fatty acid analysis, but rather focus on analysis of higher order lipids that require additional separation by HPLC prior to mass spectral analysis. Overall, a very good chapter with very readable figures.

There are three chapters related to industrial oils. In the first chapter, the use of differential scanning calorimetry to analyze edible oils is discussed in detail. The chapter is focused on raw material analysis and product analysis from a quality control viewpoint. Hence, for more biologically oriented lipid chemists this chapter will not be of major importance. However, for colleagues interested in oil analysis, the chapter will have some usefulness. Unlike the APCI-MS chapter, this chapter did not provide a solid review of the instrument and the underlying details regarding the processes by which measurements are made. In chapter three, the analysis of genetically modified oils is presented. This chapter is very well written, with a solid introduction, an overview of ''modified fatty acids'', and a section on non-chromatographic methods for oil ana1ysis. Additionally, this chapter covers other non-triglyceride components of plants oils, including phospholipids, carotenoids, and tocopherols. A very well written chapter. In chapter six, methods for the analysis of oils are presented with a general theme centered on standardization. Types of standard methods are covered, with solid discussions regarding accuracy and cost as important factors. A tremendous amount of effort was put into the section discussing the organizations sponsoring method development.

While chapter five is short, it is well put together. This chapter deals with fatty acid profiling of metabolic disorders and contains numerous helpful hints for better analysis. The one drawback is that the figures are difficult to read and the fonts are different between figures. This distracts the reader while trying to read and interpret the information contained in the figures. This chapter did not address measures of fatty acids in adrenoleukodystrophy, which of course has elevated long chain saturated fatty acids. This omission would have added to an already good chapter, but in all fairness the authors were more focused on methods rather than individual diseases.

The final chapter of the book focuses on supercritical fluid chromatography, building on a topic introduced in the first edition. Similar to the APCI-MS chapter, diagrams of the instruments aids the reader in understanding how the procedure works. This chapter contains a good introduction with an additional focus on utility of the method. There is a great deal of effort in describing the application of SFC in analysis of lipids, including details regarding actual methods involved. A very well done chapter.

In summary, this book has chapters devoted to the edible oil field (Chapters 1, 3, and 6) and chapters more relevant to the lipid biochemist (Chapters 2,4 and 5). The chapter on SFC is applicable to both camps, but certainly not a method used by any of the lipid biochemists that I know. However, this does not take away from a well written chapter that needed updating since the first edition came out over 12 years ago. As in the first edition, the argentation chromatography chapter was my personal favorite, although the APCI-MS chapter was a very close second. The one drawback is the mixing of areas, that is the edible oil field (lipid chemistry) and life sciences oriented lipid biochemistry. Putting all of one area in separate books and adding additional relevant chapters would have been ideal.

Overall, this book is recommended for the serious lipid biochemist who desires an update on topics of interest to them.

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