QC - Analytical Chemistry

May 30, 2012 - Sensors, MS, Proteins, Forensics, and QA/QC. Anal. Chem. , 1991, 63 (14), pp 734A–737A. DOI: 10.1021/ac00014a724. Publication Date: J...
1 downloads 0 Views 2MB Size
BOOKS

Sensors, MS, Proteins, Forensics, and QA/QC Sensors in Bioprocess Control. John V. Twork and Alexander M. Yacynych, Eds. 326 pp. Marcel Dekker, 270 Madison Ave., New York, NY 10016. 1990. $115 Reviewed by K. S. Fletcher, Corporate Research, The Foxboro Company, 600 North Bedford St., East Bridgewater, MA 02333 The explosion of research in sensor technology is clearly matched by that in biotechnology and bioprocessing. This book attempts to bring these technologies together and provide a framework to improve bioprocess control through the use of a large and increasing portfolio of new analytical techniques. This multiauthored, 330page, 12-chapter book is a generally useful overview of this subject, but it is also an uneven collection of reviews; some are strong on teaching, some emphasize new research, and some emphasize commercial equipment. Some redundancy also occurs; for example, nearly every chapter describes the i m p o r t a n c e of sample handling, even though one chapter is devoted exclusively to this important topic. The chapters on fiber-optic sensors, thermistor probes, and electrochemical biosensors r e p r e s e n t t h e newest research related to sensors. They are well-written, well-referenced reviews of applications in bioprocess measurement, and they provide excellent discussions of operation principles. A common theme bonds these chapters: the use of biochemical processes coupled to the sensor, which allows light, heat, or the generation of electrochemically observable species to be used for detection. The difficulty of these applications and their potential for solving measurement selectivity of complex biomolecules are perhaps understated. However, the bioprocess engineer, who already has an understanding of the biochemical processes t h a t these sensors seek to exploit, will find these chapters of significant interest. The c h a p t e r on electrochemical sensors invests considerably more

space in the operational aspects of electrochemical devices t h a n in their application; it contains little new material. The chapter on NADH- dependent fluorescence sensors is a wellbalanced b u t cursory overview of techniques for measurement of viable biomass using light launched directly into the medium as well as through fiber optics with immobilized NAD(P)H precursors. Two chapters on HPLC provide a comprehensive overview of chromatography—its history, operation, system architecture, availability, and

. . . well-written reviews of applications in bioprocess measurement... power to solve complex analytical problems—but only one application of bioprocessing is discussed, and brief reference is made to a few others. Solving a biochemical analysis/ control problem by using the material in t h i s c h a p t e r would pose a significant challenge for the biotechnologist. The chapters on chemometrics and flow-injection analysis should also be of high value to the biotechnologist— the former from the point of view of adding selectivity to otherwise less t h a n ideal sensors and the latter from the perspective of both accomplishing sampling and using known chemistry to effect automated analyses. The space allotted to chemometrics is insufficient for teaching purp o s e s ; one m u s t be e i t h e r a mathematician working with matrix techniques or a chemometrician to glean much useful information from this chapter. The chapter "Sensors in Bioprocess

734 A · ANALYTICAL CHEMISTRY, VOL. 63, NO. 14, JULY 15, 1991

Control" provides an excellent overview of process control from the basics to implementation with modern control systems and strategies. The thrust of this chapter is not sensors. However, several examples provide valuable insight into the methodology available for automation and control of bioprocesses. Sampling, sensors, automated instrumentation and control—all focused on bioprocessing—are found under one cover in this book, and it is highly recommended both for the biotechnologist interested in learning about new sensor technology and the analytical chemist seeking insight into the measurement needs of the biochemistry community.

Treatise on Analytical Chemistry, Vol. 11: Theory and Practice. I. M. Kolthoff, James D. Winefordner, and Maurice Bursey. 311 pp. John Wiley & Sons, 605 Third Ave., New York, NY 10158. 1989. $80 Reviewed by Jeanette Adams, Department of Chemistry, Emory University, Atlanta, G A 30322 This treatise is dedicated to different aspects of gas-phase ion chemistry. The five chapters cover very different topics that range from basic MS to plasma chromatography (PC). The quality of each chapter is as varied as the topics themselves. Chapter 1, "Mass Spectrometry of Organic and Biological Compounds," is an overview of basic MS t h a t includes detailed discussions of classic inlet systems, ion sources, mass analyzers, and detectors. Some theory and applications also are addressed. Although C h a p t e r 1 covers t h e classic techniques in detail, many techniques t h a t were developed in the 1980s and that had appeared by 1987 or 1988—especially regarding MS of biological compounds—are not discussed. Hyphenated techniques of continuous-flow fast atom bombardm e n t MS, supercritical fluid MS, capillary zone electrophoresis/MS, electrospray MS, and matrix-assist-

ed laser desorption MS are not covered. Some basics of quadrupole, sector, and time-of-flight machines are described, but ion trap mass spectrometers are not. Classic detectors are detailed, but the advent of array detectors t h a t significantly reduce detection limits, especially for biomolecules, is not discussed. Metastable ions and collision-induced dissociations (CIDs) are briefly covered, and the Rice-Ramsperger-Kassel (RRK) theory (not the R i c e - R a m sperger-Kassel-Marcus/quasi equilibrium theory, or RRKM/QET) is used to explain unimolecular reactions. Half of the applications described in Chapter 1 involve interpretation of EI m a s s spectra; the rest include quantitation of environmental poll u t a n t s , MS of some biomolecules, and mixture analysis by MS/MS. The discussion of MS/MS focuses on triple q u a d r u p o l e s a s well a s r e v e r s e geometry and three-sector machines. One application of a four-sector mass spectrometer is discussed, although peptide sequencing is not. There are inaccuracies in the basic MS equations and elsewhere t h a t would be misleading to a nonpractitioner. Chapter 2 covers in depth some specific and exciting a r e a s of r e search in Fourier transform ion cyclotron resonance (FT-ICR) MS and includes many references from 1988. It is written for the graduate student or expert, and a B. S. chemist might need to consult an introductory review to fully understand the technique. A brief description of basic fundamentals is followed by some of the innovative changes in instrumentation and their underlying principles. These include detailed descript i o n s of t w o - s e c t i o n ICR c e l l s , external ion sources, and new ion excitation and ejection techniques. One problem of ICR, 2-axis excitation, is discussed in detail in Chapter 2. Applications include recent studies of metal ions and metal ion clusters, carbon clusters, and ion-molecule reactions of metal ions and neutrals; CID of organometallics and studies of ion structure and thermochemistry; and photodissociation of peptide ions, determination of dissociation thresholds, and studies of other physical processes. Chapter 3 describes the use of rf spark source MS for determining elements at ultratrace levels. Anyone unfamiliar with the technique can gain an understanding and appreciation of both the power and limitations of the methodology. Instrumentation and methods for qualitative

and quantitative analysis, including sample p r e p a r a t i o n and handling, are discussed. Other topics include analyses of metals; thin films and surfaces; and biological, geological, environmental, and forensic samples. Chapter 4 is a short description of PC, also known as ion mobility spectrometry. The discussion covers the literature through 1976, except for a brief mention of two references published in 1985 (a book and a review of t h a t book). There is no historical background regarding the purpose for the original development of PC, and its impact and use in analytical chemistry are not clearly defined. Thus there is no indication of why one would choose PC over other analytical techniques. The applications section lists compounds t h a t have been studied by PC and respective literature references; one would have to read the previous literature to understand the role of PC in analytical chemistry. Chapter 5, a thorough description of the fundamentals, methodology, and uses of ion scattering for elemental analysis of surfaces, covers the literature through 1986. This chapter would be useful for any chemist. The m a t h e m a t i c s and fundamentals of the technique, which include theories of binary elastic collisions and scattering cross sections, are clearly explained. Effects of a t o m - a t o m shadowing, atom m o t i o n , a n d ion n e u t r a l i z a t i o n on signal intensity and peak shape are discussed in detail along with experimental apparatus and techniques used in qualitative and q u a n t i t a t i v e analyses. Applications include determination of in-depth concentration profiles as well as metals on surfaces of conductors, insulators, and catalysts.

Protein Purification: From Molecular Mechanisms to Large-Scale Proc e s s e s . Michael R. Ladisch, Richard C. Wilson, Chih-duen C. Painton, and Stuart E. Builder, Eds. 280 pp. American Chemical Society, 1155 16th St., N.W., W a s h i n g t o n , DC 20036. 1990. $65 Reviewed by Yuan C. Lee, Department of Biology, The Johns Hopkins University, Baltimore, MD 21218 This book is the outcome of a 1988 ACS symposium, "Design of Biochemical Technology." The development of biotechnology based on mol e c u l a r b i o l o g y c a l l s for n e w approaches to the age-old problem of protein purification. This book pro-

vides a platform by which to examine some new potentialities. The range of topics is selective and not expansive. The first three chapters, which address general problems associated with large-scale preparation of proteins, are perhaps the best in the book. Topics include the following: aqueous two-phase systems, hydrophobic interaction chromatogr a p h y (HIC), r a d i a l flow affinity chromatography, metal affinityrecycle extraction, and immunoaffinity chromatography. Some chapters, such as "Site-Specific Proteolysis of Fusion Proteins" and "Chelating Peptide-Immobilized Metal-Ion Affinity Chromatography," apparently are linked to the molecular biology of this problem. The overall focus of the book, however, is more on chemical engineering. Obviously, large-scale preparation of proteins from a production medium is different from, for example, analysis of minute quantities of enzymes from urine. In the latter case, purity may be attained even at a considerable cost, whereas in the former, economy is t h e d o m i n a n t factor. Therefore high-resolution chromatographic methods as commonly practiced in research laboratories may not be suitable for mass production of proteins. Although many of the contributors recommend nonchromatographic methods, they do not advocate abandoning high resolution. Instead, high resolution is being attempted in different forms, sometimes based on different principles. Although some advice—such as reducing the working volume early in the process—is common wisdom, each case presents different problems and challenges because of the diverse nature of the proteins being mass produced. What is a large scale for one protein may be only a microscale for another. For some proteins, HIC may be very effective, but for others it is of limited value. Because no universal singlestep purification is available, making accessible a larger number of different tools would offer greater possibilities for different problems. It is interesting that although the title professes to deal with "largescale processes," capillary zone electrophoresis (CZE) is discussed more t h a n once (in conjunction with other e l e c t r o p h o r e t i c forms). However, CZE is inferior even for microscale preparative operations. Despite its newness, inclusion of this topic here is rather questionable. The book is cleanly produced, although the type size could be larger

ANALYTICAL CHEMISTRY, VOL. 63, NO. 14, JULY 15, 1991 · 735 A

BOOKS for easier reading. The index should have included abbreviations such as HIC and CZE, which are used profusely throughout the text. As an alternative, a unified list of abbreviations would have helped r e a d e r s . Nonetheless, this is a timely and welcome volume in t h e emerging field of biotechnology.

Biological Mass Spectrometry. A. L. Burlingame and J. A. McCloskey, Eds. 700 pp. Elsevier Science Publ i s h e r s , P . O . Box 8 8 2 , M a d i s o n S q u a r e S t a t i o n , N e w York, NY 10159. 1990. $230 Reviewed by Julie A. Leary, Department of Chemistry, University of California, Berkeley, Berkeley, CA 94720 This book is a compendium of manuscripts (36 chapters) t h a t was presented in August 1989 at the Second International Symposium on Mass Spectrometry in the Health and Life Sciences. The researchers comment on a variety of mass spectral techniques for use in the characterization of proteins, glycoconjugates, nucleic acids, and other biopolymers. Ionization methods include plasma desorption, matrix-assisted laser desorption, electrospray, a n d fast atom b o m b a r d m e n t / l i q u i d SIMS. The mass spectrometer designs that incorporate these techniques are triple q u a d r u p o l e s , t a n d e m four-sector, F o u r i e r t r a n s f o r m , a n d time-offlight (TOF) instruments. The book begins with three strong chapters. Sundqvist covers the basic concepts of sputtering large organic molecules in simple but accurate terms and supplements the text with excellent references. Equally impressive are the chapters by Roepstorff and Hillenkamp who, respectively, cover the applications of plasma desorption and laser desorption TOF to large proteins. C h a p t e r s in the middle portion comment on electrospray in combination with a variety of instruments, a r r a y detectors, and strategies for sequencing proteins, glycopeptides, and oligosaccharides, whereas the last few chapters focus on the interaction of MS in the biotechnology and biopharmaceutical arenas. The last chapter, by Cantor, offers an entertaining discourse on the Human Genome Project. The overall strength of this book lies in the experts who report on their specializations within the field of biological MS. It was refreshing to see that a number of chapters were

written by young, bright scientists. However, the overall weakness is that much of the research is now two years old and somewhat outdated. This is unfortunate but can be salvaged by the fact that all of these individuals remain active in their respective a r e a s , a n d a l i t e r a t u r e search on the authors provides the reader with the most c u r r e n t r e search results in the various fields. The book is well organized and easy to read. At the end of each chapter are actual questions and answers that were parleyed during the symposium. I found these particularly useful because often they were directed at specific experimental details or nuances associated with the research that were not discussed in sufficient detail in the text. One major criticism, however, is the lack of experimental detail. If the major emphasis was to provide an overview and/or historical account of the various aspects of MS in the area of structural characterization of biological molecules, then I believe this has been accomplished. If, however, the intent was to provide a graduate student or junior researcher with the tools for duplicating or extending these techniques to his or her own research, then it clearly is lacking. The experimental section in some chapters was very sparse and altogether omitted in others. With the exception of this one item, I found the book interesting and fairly informative.

Analytical Methods in Forensic Chemistry. Mat H. Ho, Ed. 440 pp. Prentice Hall Publications, 66 Wood Lane End, Hemel Hempstead, Hertfordshire, HP2 4RG, U.K. 1990. $90 Reviewed by Thomas A. Brettell, New Jersey State Police, P.O. Box 7068, West Trenton, NJ 08628-0068 This book provides an overview of current analytical techniques and future directions of analytical chemistry in forensic science. Certain chapters deal with well-established methods, b u t most are concerned with analytical methods t h a t have shown substantial progress and that are not found in routine use in the working crime laboratory. The author has focused mostly on modern analytical instrumentation or normal analytical methods concerned with drug or toxicology analysis. Individual chapters vary substantially in format and discussion; some chapters provide reviews of various techniques on a specific application

736 A · ANALYTICAL CHEMISTRY, VOL. 63, NO. 14, JULY 15, 1991

whereas others discuss a specific technique with wide applications. Most are essentially reprints of research papers that have appeared, and some chapters lack up-to-date references of particular applications. The first six chapters cover differing aspects of MS such as MS/MS, GC/MS, stable isotope ratio MS, fast atom bombardment MS, and chemical ionization MS, as well as their applications to forensic science. The next four chapters are devoted to the applications of several spectroscopic methods to the solution of specific forensic problems. Chapter 7 is a compilation of the author's previously published articles on the applications of chiral optical spectroscopy to the detection and quantification of drugs of abuse. It describes in relatively simple terms the concepts of polarimetry, optical rotatory dispersion, and circular dichroism. Chapter 8 focuses on the potential application of three-dimensional fluorescence in forensic analysis of pet r o l e u m - b a s e d products, which shows promise for real casework samples. Chapter 9 discusses the theoretical basis of the radiative energy attention technique and its application to the determination of ethanol in biological fluids. Chapter 10 describes the specimen preparation and analysis for trace metals by flame and flameless atomic absorption spectrophotometry. The next 14 chapters deal with chromatographic methods and their applications to various forensic problems, most of which concern t h e analysis of drugs of abuse and the comparative analysis and profiling of specific types of drugs. Capillary GC and HPLC methods are extensively discussed, and all of Chapter 19 is devoted to the application of gel permeation chromatography as well as the radioimmunological screening, identification, and determination of barbiturates in postmortem blood. The last five chapters deal with various topics of forensic science such as the latex particle agglutination technique in the i m m u n o a s s a y of therapeutic drugs (Chapter 25), a semiautomated extraction and spotting system for the analysis of drugs in physiological fluids (Chapter 26), the detection of firearm residues by several analytical methods (Chapter 27), a systematic approach to toxicology analysis (Chapter 28), and the potential for and limitations of chemical analysis of physiological evidence (Chapter 29). In the last few chapters the author

h a s tried to comprehensively cover most of the analytical techniques a p plicable to the forensic science laboratory. In this attempt he h a s omitted several important areas such as pyrolysis GC, microspectrophotometry, FT-IR, the analysis of dyes from fibers, dynamic headspace techniques in the detection of accelerants, and DNA technology. Despite these omissions, the author has provided an excellent text of current analytical methodology with pertinent applications to forensic science. The practicing forensic scientist cannot help but learn new techniques and information to apply to casework samples. Likewise, few analytical chemists would find it difficult not to learn new techniques to apply to forensic science. This book should be on the shelf of every forensic scientist's library.

Handbook of Quality Assurance for the Analytical Chemistry Laboratory. James P. Dux. 203 pp. Van Nostrand Reinhold, 115 Fifth Ave., New York, NY 10003. 1991. $40 Reviewed by Donald F. Gurka, U.S. Environmental Protection Agency, Environmental Systems Laboratory, Quality Assurance Division, 944 East Harmon Ave., Las Vegas, NV 89159 This is a concise beginner's book t h a t covers the basics of establishing, operating, optimizing, and documenting a quality assurance/quality control (QA/QC) program. Topics include definitions, basic statistics and statistical applications, sampling, analytical methods and materials, documentation and organization, setting up and auditing t h e QA program, and strategies for obtaining laboratory accreditation. Updates to the first edition address computers and laboratory information systems (LIMS). The style is qualitative; few figures and solved problems appear. But this style is appropriate for a startup laboratory and is directed at managerial p e r s o n n e l concerned w i t h QA/QC oversight roles. The rationale for this is accurately stated as "while the cost of a quality assurance program is often easy to establish with routine accounting and labor allocation proced u r e s , m a n y of t h e b e n e f i t s a r e i n t a n g i b l e . " Clearly, m a n a g e m e n t must establish QA/QC cost-benefit philosophy, and this book could provide a cornerstone for such thinking. The strength of the book lies in a detailed exposition of how to establish a n d monitor t h e QA/QC pro-

gram. Example forms and checklists provide a n i n i t i a t i o n point from which the laboratory can evolve to its own goals. The author's computer mentality is ambivalent, at best; contradictory statements are interspersed throughout the book. For example, on page 12, he states t h a t "computers will eliminate calculation errors, but cannot eliminate errors due to incorrect data input." On page 169, however, he says, "We must always be aware of the problem of det e r i o r a t i o n of software q u a l i t y . " Widespread use of optical scanners should enhance t h e possibility of data transcription errors (i.e., input data are correct but misread). Another glaring error is the statement on page 55 t h a t the chain of custody should start after the sample is received. This is too late to guarantee data defensibility. These problems do not m a r the fact t h a t the book has a very pragmatic approach to daily QA/QC activities. However, it does not provide (as claimed on the jacket) the latest a p proach to QA/QC systems. Of 17 references for 13 c h a p t e r s , only two were published after the first edition. A reading list is added at the end to correct this problem, but one-third of these references were previously cited a n d only t h e computer-related references can be considered current. This book is almost perfect for the novice learning about QA/QC. If one already owns the first edition, however, I doubt that it is necessary to purchase the second version.

Books Received Spectroscopic Properties of Inorganic and Organometallic Compounds, Vol. 23. G. Davidson and E.A.V. Ebsworth, senior reporters, xiv + 495 pp. Royal Society of Chemistry, Distribution Centre, Blackhorse Rd., H e r t s SG6 1HN, U.K. 1990. $143 This book, a review of the recent literature published up to late 1989, contains more t h a n 5700 references. The eight chapters are " Nuclear Magnetic Resonance Spectroscopy," "Nuclear Quadrupole Resonance Spectroscopy," "Rotational Spectroscopy," "Characteristic Vibrations of C o m p o u n d s of M a i n G r o u p E l e m e n t s , " " V i b r a t i o n a l S p e c t r a of Transition-Element Compounds," "Vibrational Spectra of Some Coordinated Ligands," "Môssbauer Spectroscopy," and "Gas-Phase Molecular S t r u c t u r e Determined by Electron Diffraction."

Photon Migration in Tissues. Britton Chance, Ed. χ + 195 pp. P l e n u m Press, 233 Spring St., New York, NY 10013. 1989. $63 This book is the result of a work­ shop held in April 1988 in Philadel­ phia. The presentations include opti­ cal properties of t i s s u e , a d a p t i n g fluorescence instrumentation, in vivo near-IR spectroscopy, ultrashort la­ ser pulse tomography, a n d t i m e resolved methods. The book contains more than 200 references, with a p ­ proximately half since 1985. Author and subject indexes are included. Analytical Chemistry of Silicones. A. Lee Smith, Ed. xxii + 550 pp. John Wiley and Sons, 605 Third Ave., New York, NY 10158. 1991. $125 This is Volume 112 in the series C h e m i c a l A n a l y s i s : A S e r i e s of Monographs on Analytical Chemis­ try and Its Applications. Topics in­ clude trace analysis, surfaces, per­ sonal care applications, microscopical characterization, chromatography, NMR, and MS. Approximately half of the 1100 references span the 1980s, with a few as late as 1989. A subject index and an appendix listing physi­ cal properties of organosilicon com­ pounds are included. Introduction to Laboratory Automa­ tion. Victor Cerdâ and Guillermon Ramis. xiv + 321 pp. John Wiley & Sons, 605 Third Ave., New York, NY 10158. 1990. $70 This is Volume 110 in the series C h e m i c a l A n a l y s i s : A S e r i e s of Monographs on Analytical Chemistry and Its Applications. The nine chapters are "Automation and Chemistry," "Basic Concepts and Elements of Analog Electronics," "Digital Electronics," "Microprocessors," "Transduction, Signal Conditioning, Data Acquisition, and Control," "Communications," "Instruments and Appar a t u s for Laboratory Automation," "Automation of Analytical Methods," and "Laboratory Robotics." A bibliography and an index are included. Chromatographic Analysis of Alkaloids. Milan Popl, J a n Fàhnrich, and Vlastimil Tatar, viii + 667 pp. Marcel D e k k e r , 270 M a d i s o n Ave., N e w York, NY 10016. 1990. $150 The seven chapters are "Classification of Alkaloids," "Properties of Alkaloids Relevant to Chromatography," "Chromatography," "Gas Chromatography," "Liquid Chromatography," "Thin-Layer Chromatography," and "Applications." Of the 1300 references, about half span the 1980s, through 1988. An index is included.

ANALYTICAL CHEMISTRY, VOL. 63, NO. 14, JULY 15, 1991 · 737 A