Books
Laboratory Lore from Some Eminent Chromatographers Glass Capillary Chromatography in Clinical Medicine and Pharmacology. Halvor Jaeger, Ed. xi + 640 pp. Marcel Dekker, 270 Madison Ave., New York, N.Y. 10016. 1985. $99.75 Reviewed by Brian Middleditch, Department of Biochemistry and Biophysical Sciences, University of Houston, Houston, Tex. 77004 The blurb on the back cover of this book promises "chapters that detail the latest developments in capillary gas chromatography for clinical applications and drug analyses, [discussing] such topics as the influence of fused silica... high reproducibility of oncolumn injection . . . washability of bonded-phase columns . . . and much more." The introduction of the bonded-phase fused-silica capillary column has indeed revolutionized the art and science of gas chromatography, yet this invaluable tool is mentioned in only three of the 30 chapters. Why? A quick glance at the bibliographies indicates that most of the chapters were written three to five years ago. Indeed, only 24 of the 1615 articles cited by the various authors were published after 1981, and one third of the chapters contain no citations from the 1980s. The editor claims in his introduction that "efforts have been made to update this material throughout the editorial and publication process so as to provide the reader with the latest possible developments," but there is scant evidence that this has been done. Are we left with a book that is obsolete? Not entirely. The better chapters contain a wealth of useful information and provide detailed accounts of the developments that led to the adoption of the procedures they espouse. They are not merely annotated bibliographies. The most outstanding chapter is Cedric Shackleton's encyclopedic discussion of steroid analysis. He takes the reader into his laboratory and provides step-by-step instructions on how to select, install, and test columns; extract steroids from body fluids and convert them to suitable derivatives;
and choose the most appropriate method of sample introduction. Much practical advice is given concerning the design of procedures for quantitative analysis, but qualitative analysis by combined gas chromatographymass spectrometry receives only a brief mention. Detailed accounts are given of illustrative analyses of endogenous steroids from urine, serum and tissues, bile acids, vitamin D metabolites, and steroid drugs. The development of methods for the analysis of intact conjugates is (correctly) forecasted. Other chapters providing a similar degree of detail are devoted to the analysis of amino acids (Frank and
The most outstanding chapter is Cedric Shackleton's encyclopedic discussion of steroid analysis.
Jaeger), carbohydrates (Pfaffenberger), thyroid hormones (Corkill et al.), fatty acids (Jaeger et al.), phospholipids (Gaskell), bile acids (Jaeger et al.), nucleosides (Gelikjens et al.), and peptide antibiotics (Koenig). Walter Jennings contributed three introductory chapters. His discussion of the state of the art is, of course, quite dated, although his accounts of gas chromatographic theory and quantitative analysis are timeless and highly recommended. Essays of a more general nature are devoted to profiling of metabolic disorders (Liebich), metabolism of drugs and environmental chemicals (Horning et al.), pharmacokinetics and drug metabolism (de Boer et al.), and internal standards (VandenHeuvel et al.). Topics that receive a more cursory treatment and are largely of historical value relate to microliter-scale techniques of sample preparation
1414 A · ANALYTICAL CHEMISTRY, VOL. 57, NO. 13, NOVEMBER 1985
(Diinges); analysis of lower fatty acids, phenols, and indoles (Hoshika); quantitation of serotonin and its metabolites (Sunol and Gelpi); and determination of the absolute configuration of chiral hydroxy acids (Kamerling and Vliegenthart). Also included are seven chapters, coauthored by the editor, on the quantitative analysis of specific drugs. Three of these (on isosorbide dinitrate, bencyclane, and diphenhydramine and orphenadrine) are reprints of journal articles. Others describe the assay of bromhexine, hydrochlorothiazide, clofibrate, and codeine. The two remaining chapters are devoted to the derivatization of barbiturates and diphenylhydantoin (Diinges) and the analysis of cannabis (McCallum). The latter cites no articles published later than 1979. It is a great pity that the long gestation time of this book precluded discussion of the multitude of exciting developments that have evolved in the 1980s. Many of the chromatograms in the book obtained using WCOT and SCOT glass and metal capillaries have rising baselines attributable to increased column bleed at higher temperatures. This problem is avoided entirely with bonded-phase fused-silica capillary columns. There is no mention of wide-bore capillary columns, bonded-phase glass capillary columns, or the newer methods of multidimensional chromatography and sample introduction (with sample volumes measured in milliliters rather than microliters). More information could have been provided on GC/MS, particularly with regard to the need for high scan rates, data manipulation, and the newer ionization methods. Applications that might have been included are the investigation of catecholamine metabolism, analysis of exhaled air, microbial taxonomy, identification of drugs of abuse, and forensic analysis. There are some errors that might have caught the eye of a more critical editor. Identical glossaries of abbreviations relating to gas chromatography are appended to two of Jennings's
Books
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chapters (pp. 30-31 and 50-51); the structure of asparagine is missing from the table of protein amino acids on page 74; the structural formula for Chirasil-Val on page 99 is inverted; there is some text missing from the second paragraph of page 158; the two figures on page 226 are reversed; and there are numerous instances of incor rect reference numbers, mismatched cross-references, and incomplete lit erature citations. Other typographical errors tend to be more amusing than misleading (perhaps the electron cap ture detector with a volume of 300 μΙΡ [p. 257] is used in some new type of mind-boggling multidimensional chro matography). The subject index (only 317 entries) is merely an alphabetical listing of subheadings from the various chap ters, and there is no author index. Jaeger has done an admirable job of persuading an imposing roster of eminently qualified chromatographers to divulge laboratory lore beyond that normally included in journal articles. Although the state of the art is not well represented, most of the material is far from obsolete, and I expect to consult my review copy frequently. I have recommended that the book be purchased by our library.
Books Received Chromatography—The State of the Art. Vols. I and II. Proceedings of the Budapest Chromatography Conference, June 1-3, 1983. H. Kalasz, L. S. Ettre, Eds. 903 pp. Akademiai Kiado Buda pest, P.O. Box 24, H-1363 Budapest, Hungary. 1985. $75 Structure Determination by X-ray Crystallography. 2nd ed. M.F.C. Ladd, R. A. Palmer, xxli + 502 pp. Plenum Press, 233 Spring St., New York, N.Y. 10013. 1985. $39.50 Spectral Atlas of Polycyclic Aromatic Compounds. W. Karcher et al. vi + 818 pp. Kluwer Academic Publishers, 190 Old Derby St., Hingham, Mass. 02043. 1985. $94 Oils, Lubricants, and Petroleum Prod ucts: Characterization by Infrared Spectra. John Coates, Lynn Setti. xxvi + 297 pp. Marcel Dekker, 270 Madison Ave., New York, N.Y. 1985. $145
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Trace Residue Analysis: Chemometric Estimations of Sampling, Amount, and Error. David Kurtz, Ed. χ + 286 pp. American Chemical Society, 1155 16th St., N.W., Washington, D.C. 20036. 1985. $71.95
1416 A · ANALYTICAL CHEMISTRY, VOL. 57, NO. 13, NOVEMBER 1985
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