Energize Your Laboratory at the 2012 Eastern Analytical Symposium

October 1, 2012

The 2012 EAS program chair presents highlights of the invited symposia in spectroscopy and related fields, from the perspective of what the chairs of the invited sessions had in mind when developing the sessions and what you can expect to learn.

From November 12 to 15, 2012, as in the preceding 50 years, the Eastern Analytical Symposium will bring a rich assortment of potential solutions and collaborations to its

attendees and contributors.

Summer is long gone now and as our minds focus on the luscious fall foliage and long, cold winter months ahead, we should also turn to the positive feelings that come from having new problems to solve and the ability to productively contribute to their solutions. This year's Eastern Analytical Symposium (EAS), being held November 12–15 in Somerset, New Jersey, will offer those positive feelings and a wealth of knowledge to help you find the solutions you need. To highlight the invited symposia in spectroscopy and related fields we have asked some of the chairs of the invited sessions to briefly describe their intentions as they pulled together well-known and well-respected speakers for their chosen topics. My hope, as the 2012 EAS program chair, is that this synopsis will encourage you to come, see, hear, and enjoy the directions that spectroscopy has taken over the past year. This is with the goal that once you return from EAS in November, you can use your new-found knowledge to energize your own laboratory and solve problems.

Mass Spectrometry

This year, Fred McLafferty, of Cornell University, is being recognized for his many transformative innovations over the last half century with the Award for Outstanding Achievements in Mass Spectrometry, to be given at a symposium in his honor. From developing electron-capture dissociation to offering fundamental understanding of gas-phase-rearrangement phenomena, McLafferty has been a towering figure in the field. Beyond his more than 500 publications on all aspects of the technique, the hundreds of colleagues McLafferty has trained over seven decades, many of whom have themselves made major contributions in mass spectrometry (MS), make his impact on the field almost unparalleled. Several former students will present in this symposium, including Neil Kelleher of Northwestern University, Gary Valaskovic of New Objective, Inc., and Edward Chair of Life Sciences Consulting, Inc. Among the topics to be discussed are the latest technologies for electrospray MS of whole proteins in the gas phase (the so-called "top down proteomics"), and recent advances in application of this technology to the area of expression genomics.

A two-session mini symposium titled "Mass Spectrometry of Large and Biomolecules" will feature leaders and emerging scientists from academia, industry, and instrument manufacturing. A wide array of recent developments that overcome challenges faced when using MS for the study of large and biomolecules will be discussed, including method development and applications for proteomics and metabolomics, as well as the analysis of oligonucleotides, polymers, and supramacromolecules. For example, Martin Gilar of Waters Corporation will discuss liquid chromatography (LC) separations for complex mixtures of oligonucleotides, peptides, and glycopeptides. Kimberly Ralston-Hooper of Duke University will present proteomic applications in environmental toxicology. Jiong Yang of Merck will speak on modified oligonucleotide sequencing for identity confirmation of phosphorothioate-containing siRNAs. Chrys Wesdemiotis of the University of Akron will discuss method development for MS analysis of synthetic polymers and supramacromolecules. The effect of peptide structure on matrix-assisted laser desorption–ionization time-of-flight mass spectrometry (MALDI TOF-MS) signal intensity will be presented by Kevin Owens of Drexel University. Sarah Trimpin of Wayne State University will put forth new ionization approaches, Gary Kruppa of Bruker Daltonics, Inc., will touch on applications using MALDI-TOF for biopharmaceutical quality control, and Mark Cancilla of Merck will acquaint the audience with MS-based assays for the characterization of oligonucleotides.

NMR

Jeffrey A. Reimer of the University of California at Berkeley is the 2012 recipient of the EAS Award for Achievements in Magnetic Resonance. This award recognizes his contributions to solid-state nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI), in catalysis, electrochemistry, polymer science, and semiconductor physics. Joining Reimer are three distinguished colleagues who will reflect on the connection between basic knowledge and applications of magnetic resonance. Anant K. Paravastu of Florida State University will speak on multidimensional NMR and 13 C-13 C nuclear dipolar couplings for the structural characterization of designer self-assembling proteins that form biomedically important nanofiber matrices. Alexej Jerschow of New York University will discuss newly discovered long-lived magnetic resonance signals in solids, which may enable new approaches for the analysis and imaging of hard tissues (such as bone) as well as battery materials. Cecil Dybowski of the University of Delaware will report on NMR of heavy metals with enormous chemical shift ranges, and how measurements can be applied to problems such as elucidating the properties of formulations of artists' paints or the nature of semiconducting materials.

Advances in NMR hardware and techniques are allowing increasingly rapid identification of metabolites. Two areas are key: first, the development of hyphenated techniques such as LC–MS–NMR, and second, the introduction of cryogenic probes. Dr. Steve Cheatham of DuPont Crop Protection has assembled a session entitled "NMR Techniques for Metabolite ID." The session focus is on applications of these tools toward metabolite identification. The first two talks in the session will focus on the use of hyphenated techniques, as representatives from both Bruker and Agilent provide perspective and results of the latest technology in the field.

The second two speakers in this session are representatives of the pharmaceutical industry and will provide insight into the practical aspects of metabolite identification using NMR techniques. While focusing on metabolite identification, the structure elucidation techniques to be discussed in the session should prove relevant to a variety of areas including natural product chemistry, food chemistry, and mixture analysis.

Surface Science

Dan Strongin of Temple University has organized a session titled "Environmental Surface Chemistry" that will highlight recent research on redox transformations in the environment. Redox chemistry that occurs between mineral surfaces and aqueous organic and inorganic species contributes to geochemical cycling of metals, to remediation of toxic aqueous environmental pollutants, and to processes such as the sequestration of CO2. One talk will focus on the reactivity of ferrous iron with aluminum oxide and montmorillonite clay and the reactivity of these systems toward redox-active species such as hexavalent Cr and U. Another will concentrate on the redox chemistry of Cr(VI) as it applies to the photochemistry of the mineral phases of the small-band-gap semiconductor FeOOH. A further talk will spotlight how mixtures of binary metal oxides drive redox chemistry relevant to the removal of pollutants from wastewaters. Research on potential redox chemistry involving mineral phases will highlight the potential of metal carbonation that is relevant to CO2 sequestration.

"Surface Spectroscopy," organized by Lars Gundlach of the University of Delaware, will turn attention to the interaction of molecular adsorbates and solid surfaces. Piotr Piotrowiak of Rutgers University will show the sensitivity of spectroscopy of a titanate cluster to every atom, although other properties like the density of states show bulk-like characteristics. Graphene, a hybrid between a molecular and a solid state material (being atomically thin in one dimension), is the focus of X-ray photoelectron spectroscopy (XPS) and reflected electron energy loss spectroscopy (REELS) investigations by Brian Strohmeier of Thermo Fisher Scientific. With these techniques, he addresses chemical surface modification, surface impurities, and substrate interaction. Hsuan Kung of the University of Delaware will report on a novel, highly controlled route for depositing metal nanoparticles on zinc oxide particles that allows precise control of the surface morphology. Eric Borguet of Temple University will present time-resolved infrared measurements on the water–silica interface to allow for the study of these important materials. Laurel Kegel of the University of Delaware, in discussing studies of plasmonic nanostructures, will emphasize the importance of penetration depth and resonance wavelength for the sensitivity of surface plasmon resonance sensors.

Vibrational Spectroscopy

As a workhorse analytical technique in so many industries for such a long time, vibrational spectroscopy might possibly be in danger of being taken for granted. In the session "Bringing Home the Bacon — Vibrational Spectroscopy Gets the Job Done," organized by Linda Kidder of Malvern Instruments, presentations about out-of-the-box applications of mid-infrared, near-infrared, and Raman spectroscopy will show that there are many new ways to analyze materials with vibrational spectroscopy. Nancy Jestel of Sabic Innovative Plastics will provide an industrial perspective for using vibrational spectroscopy's unique capabilities to solve critical analytical problems. The proliferation of multivariate algorithms and their increasingly "routine" application to spectroscopic data has been critical in enabling development of vibrational spectroscopy. Katherine Bakeev of Camo Software will explore data visualization and analysis. Cutting-edge vibrational spectroscopic tools and their applications to chiral drugs and biotherapeutics will be the topic of a presentation by Rina Dukor of BioTools. As Raman spectroscopy has become more "mobile," it has assumed a new dimension, as will be seen in the presentation focusing on Raman five-component identification from Edita Botonjic-Sehic of Morpho Detection.

A Coblentz Society–sponsored session entitled "Spectroscopy in the Palm of your Hand," organized by Heinz Siesler of the University of Duisburg-Essen (Germany), will provide a new perspective on spectroscopic control of drug-product production and analysis. For example, Benoit Igne of Duquesne University will present a case study in which specific algorithms and analyses of on-line blend data were evaluated to determine their ability to provide quality control of tablets. Douglas Both of Bristol-Myers Squibb (BMS) will describe an approach to designing real-time-release (RTR) testing–based control strategies for commercial manufacturing and how it relates to and evolves from the quality-by-design (QbD) work performed during development, where the fundamental understanding of the product's critical quality attributes were established. Like BMS, Pfizer has also received regulatory approval for RTR-based control strategies, and Steve Hammond will demonstrate why it is beneficial to measure one's process in real-time. Martin Warman of Vertex will describe a systematic approach to defining the critical steps in making an acceptable product, defining the process space within which we should operate to ensuring the process stays within that defined space. His talk will provide a wide range of examples in which spectroscopic techniques have supported QbD and RTR.

Conclusion

Spectroscopy is a vast field with diverse uses and results — both fundamental and applied. EAS 2012 offers a full range of spectroscopy sessions, both theoretical and applied. A trip to EAS 2012 will be rewarded with ideas, understanding, and learning, but more importantly with the atmosphere to make connections to others who work at the cutting edge of these spectroscopic technologies. The EAS 2012 full technical program, list of short courses, and registration is available at the following website: www.eas.org

Mary Ellen McNally is the Program Chair of EAS 2012 and a Technical Fellow at Dupont Crop Protection in Newark, Delaware. Please direct correspondence to: Mary-Ellen.McNally@USA.dupont.com.