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Meeting Information

WCDG hosts monthly public meetings from September to May on the 3rd Wednesday of the month.  A light dinner and social hour begin at 6:00 pm, followed by a speaker at 7:00 pm.


Future Meetings

        
  • September 20, 2017 - Annual Poster Session & Open House
  • October 18, 2017 - John Hanover (NIH-NIDDK) at ACS Headquarters
  •  November 15, 2017 - TBD
  • December 6, 2017 - Joseph Zaia (Boston University) at USP


Past Meetings

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May Meeting
Wednesday, May 17, 2017
6:00 pm - 8:00 pm at US Pharmacopeia (Directions)

Speaker: Christian Wolf, Dept. of Chemistry, Georgetown University, Washington, DC
Title: Chromatographic and Spectroscopic Analysis of Chiral Compounds

Abstract: The ever-increasing demand for biologically active chiral compounds, in particular pharmaceuticals and agrochemicals, continues to nurture tremendous interest in asymmetric synthesis. At the same time, the development of time-efficient methods for the analysis of chiral compounds is vigorously pursued at numerous academic and industrial research laboratories. In recent years, the practicality of combinatorial and parallel synthesis has been matched with significant advances in enantioselective analytical techniques. The usefulness of enantioselective chromatography and optical chemosensing for the determination of enantiomeric composition of chiral compounds in complex mixtures and for the determination of racemization kinetics will be discussed with several case studies.

Bio: Dr. Christian Wolf earned his doctorate from the University of Hamburg, Germany in 1995 in the lab of Wilfried Konig. He was awarded a Alexander von Humboldt Feodor Lynen Postdoctoral Fellowship under William Pirkle at the University of Illinois at Urbana-Champaign, IL. In 1997, he became a senior scientist at SmithKline Beecham Pharmaceuticals in King of Prussia, PA. Dr. Wolf joined the Department of Chemistry at Georgetown University in 2000 and was promoted to full professor in 2011. His research interests include synthetic methodology, chiral recognition and chemosensing, dynamic stereochemistry of chiral compounds, transition metal catalysis, and medicinal chemistry. Dr. Wolf had been awarded the Distinguished Georgetown University Investigator, the President's Award for Distinguished Scholars-Teachers, the Georgetown University Patent Award, the NSF CAREER Award, and the Gold Impact Award from SmithKline Beecham.
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April Meeting
Wednesday, April 19, 2017
6:00 pm - 8:00 pm at US Pharmacopeia (Directions)

Student Speaker: Rosemary Onjiko & Erika Portero, 2016 Student Poster Honorable Mentions

Featured Speaker: Walter B Wilson, Research Chemist, NIST, Gaithersburg, MD
Title: Liquid and gas chromatographic retention behavior of polycyclic aromatic compounds on stationary phases of different selectivities

Abstract: One of the most widely studied groups of environmental contaminants today is polycyclic aromatic compounds (PACs), which are comprised of a complex class of condensed multi-ring benzoid compounds. The majority of the research with PACs has focused on polycyclic aromatic hydrocarbons (PAHs). Along with PAHs, heterocyclic compounds containing at least one heteroatom such as polycyclic aromatic sulfur heterocycles (PASHs) are largely present in the same environmental samples. The total number of possible isomeric structures for PASH is greatly increased compared with the corresponding PAH because both ring arrangement and position of the sulfur atom substitution within the rings give rise to unique isomers. In the current study, the retention behavior for many key isomeric groups of PACs and their alkyl-substituted derivatives were evaluated by gas chromatography (GC) and reverse-phase liquid chromatography (RPLC). In the GC studies, three stationary phases of different selectivities were studied: a ~50% (mole fraction) phenyl-substituted methylpolysiloxane phase, smectic liquid crystalline phase, and an ionic liquid phase. In the RPLC studies, multiple LC columns consisting of C18, C30, phenyl-hexyl, and penta-fluoro-phenyl stationary phases are evaluated.

Bio: Dr. Wilson completed his PhD in chemistry in 2014 from the University of Central Florida under the mentorship of Prof. Andres Campiglia. During his time in Campiglia’s lab, his work focused on the development of new analytical extraction methods for PACs in conjunction with liquid chromatography, gas chromatography, and low temperature fluorescence spectroscopy techniques. Dr. Wilson was awarded a two-year appointment as a National Research Council post-doctoral research associate at the National Institute of Standards and Technology (NIST) under advisement of Dr. Stephen Wise and Dr. Lane Sander, where he specialized in the development of new liquid and gas chromatographic separation techniques for PACs in complex sample matrices. Currently Dr. Wilson is a research chemist at NIST, where he focuses on the development of new dietary supplements and environmental reference materials.
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March Meeting
Monday, March 27, 2017 Joint meeting with WBMSDG
6:15 pm - 8:00 pm at Shimadzu Training Center, Columbia, MD (Directions)

Speaker: Robert N. Cole, Assistant Professor Dept. Biological Chemistry, Johns Hopkins School of Medicine
Title: Adventures of Capillary Electrophoresis in Proteomics from Top-down to Bottom-up

Abstract: Capillary zone electrophoresis (CE)-MS has become more accessible with robust electrospray interfaces, presenting a potential alternative to LC-MS. CE achieves rapid and high resolution analyte separation based on net charge and hydrodynamic volume. CE is orthogonal to reversed phase LC with additional benefits of low carryover, low (nanogram) sample injection, and rapid sample loading. CE-MS analysis of complex peptide mixtures is challenging due to the seconds-wide elution peaks produced during the rapid separations. However, increases in MS data acquisition speeds warrant re-examination of the role of CE in proteomics. We are evaluating a microfluidic chip-based CE interface (ZipChip, 908 Devices Inc) for top-down analysis of intact proteins, analysis of high charge/high pI peptides, and bottom-up quantification of proteins. Even with major challenges of sample concentration, protein complexity and automation, CEMS has a bright future in protein analysis.

Bio: Dr. Robert Cole is an assistant professor of biological chemistry at the Johns Hopkins School of Medicine. His research focuses on mass spectrometry strategies to characterize proteins and their modifications in malnutrition, neurological diseases and cancer. Dr. Cole serves as the director of the Mass Spectrometry and Proteomics Facility for the Johns Hopkins University School of Medicine and director of the Mass Spectrometry Core for the Johns Hopkins Kimmel Cancer Center. Dr. Cole received his undergraduate degree in zoology/physiology from the University of Massachusetts, Amherst. He earned his M.S. in biology/physiological ecology from the University of South Carolina and his Ph.D. in physiology/neuroscience from Michigan State University. He completed postdoctoral training in glycobiology/neuroscience at the University of Alabama at Birmingham and the Johns Hopkins School of Medicine. He joined the Johns Hopkins faculty in 1998. He is a member of the American Society for Mass Spectrometry, and his work has been recognized with a National Research Service Award from the National Institutes of Health.
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February Meeting
Wednesday, February 15, 2017
6:00 pm - 8:00 pm at US Pharmacopeia (Directions)

Student Speaker: Sam Choi, 2016 Georges Guiochon Poster & Travel Award recepient

Featured Speaker: Peter Nemes, Assistant Professor, Dept. of Chemistry, George Washington University
Title: Capillary Electrophoresis Mass Spectrometry for Understanding Early Vertebrate Embryonic Development One Cell at a Time

Abstract: A critical step during normal embryonic development is differentiation of pluripotent stem cells into all the different types of tissues of the vertebrate body. By unbiased and label-free detection, high-resolution mass spectrometry (HRMS) provides a direct window to follow molecular changes during cell differentiation, especially at the level of the metabolome that responds dynamically to intrinsic/extrinsic events. To enhance detection sensitivity, traditional HRMS pools large cell populations, albeit at the expense of potentially averaging out cell-characteristic processes such as a cell’s commitment to a specific tissue fate. In this presentation, we will discuss the development and utilization of single-cell capillary electrophoresis electrospray ionization HRMS platforms and protocols that we have developed and validated to enable the ultrasensitive detection of metabolites and proteins in single embryonic cells. Last, we will demonstrate how discovery metabolomics and proteomics data by single-cell MS opens new investigative potentials in basic cell and developmental biology, including the discovery of small molecules with previously unknown impact on cell fate specification in the vertebrate embryo of the South African clawed frog (Xenopus laevis), a powerful model of embryonic development and health studies.

Bio: Peter Nemes is an Assistant Professor of Chemistry (2013–present) at the George Washington University (GWU), whence he obtained a PhD in chemistry in 2009 (advisor: Prof. Akos Vertes). He completed postdoctoral training in analytical neuroscience at the University of Illinois—Urbana-Champaign (mentor: Prof. Jonathan V. Sweedler). After serving as a Laboratory Leader and Staff Fellow at the US Food and Drug Administration between 2011–2013, Dr. Nemes joined the faculty of the GWU Department of Chemistry. Research in the Nemes Laboratory develops ultrasensitive and microanalytical platforms for high-resolution mass spectrometry to study how metabolic and proteomic processes orchestrate normal cell heterogeneity during early development of the vertebrate embryo and the central nervous system. Prof. Nemes has authored 34 peer-reviewed publications, 6 book chapters, and 100+ presentations. He is co-inventor of the patented and licensed LAESI mass spectrometry technology. In 2015, Prof. Nemes was named a Beckman Young Investigator by the Arnold and Mabel Beckman Foundation and received the Arthur F. Findeis Award for Achievements by a Young Analytical Chemist by the Division of Analytical Chemistry of the American Chemical Society. In 2016, Prof. Nemes received the DuPont Young Professor Award and the US-HUPO Robert J. Cotter New Investigator Award.
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January Meeting
Wednesday, January 18, 2017
6:00 pm - 8:00 pm at US Pharmacopeia (Directions)

Speaker: Abigail Turner, National Institute of Standards and Technology
Title: The NISTmAb: Capillary Electrophoresis-based Characterization and Life Cycle Management

Abstract: The National Institute of Standards and Technology (NIST) has recently developed the NISTmAb Reference Material (RM 8671), an IgG1κ class-representative monoclonal antibody. The NISTmAb is intended to serve as a platform for harmonization and open innovation in the biopharmaceutical analysis community.  It is a widely and longitudinally available test material that will support novel technology and method development, serve as an external system suitability control, and provide a medium for open access information sharing.  Here, we describe NIST’s approach to characterization and lifecycle management of the reference material.  We discuss, by way of example, the role of capillary electrophoresis-based assays in NISTmAb quality assurance, including CE-SDS, cIEF, CZE, and CE-ESI-MS/MS.

Bio: Dr. Turner completed her doctoral degree in Chemistry in 2015 at the University of North Carolina at Chapel Hill under the mentorship of Prof. Nancy Allbritton.  In the Allbritton lab, Dr. Turner developed capillary electrophoresis-based measurement tools for quantifying enzyme activity in single human cells.  Dr. Turner is currently a National Research Council post-doctoral research associate at the National Institute of Standards and Technology and the Institute for Bioscience and Biotechnology Research, where she specializes in leveraging capillary electrophoresis and mass spectrometry for detailed structural characterization of proteins including the NISTmAb RM 8671.
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November Meeting
Thursday, November 17, 2016
ACS Headquarters, 1155 16th St NW, Washington, DC
Joint meeting with Chemical Society of Washington (CSW)
6:00PM social hour, 6:30PM dinner, 7:15PM presentation
Free event. RSVP by November 14 to csw@acs.org

Speaker: Mark L. Miller, FBI Counterterrorism and Forensic Science Research Unit, Quantico, VA
Title: Challenges in Forensic Separations

Abstract: The popularity of forensic science on TV shows and movies has glamorized forensic scientists and their work for the last couple of decades. But can you really inject a DNA sample in your GC and instantly obtain the name and address for the criminal? Can your arsenal of instruments perform an analysis and find a chemical database for every reference material related to the evidence? While practicing chemists recognize that this is not the case in real life, we can be thankful that these TV shows inspire many young people to seek careers in science. Research in forensics manifests many challenges as new and unusual samples present themselves in casework. One of the first tasks of a researcher is to determine what is the relevant target molecule(s) and what is the matrix one must analyze? Often in casework these are common matrices such as biological material (e.g. blood, urine, etc.) or an environmental sample (e.g. soil, water, etc.).  But many times there is a twist to the complexities of getting the right results. For example, who could have foreseen that one day we would need to or be able to detect drugs in bugs or hair? Forensic chemistry research deals with these challenges by developing new methods that require both a separation of a complex mixture and a detection technique. The evolving threats mean that both small and large, organic and inorganic chemicals must be separated and analyzed for evidence examinations. GC and LC are the most useful tools for the separation of complex mixtures for everything from hydrogen peroxide to ricin. One of the tricks to effective use of chromatography is to have adequate retention of your analyte on the separation column, which from review of the literature is not always present in forensic practice. This talk will provide real examples of improved and new methods developed for different types of evidence for application in toxicology and explosives casework.

Bio: Mark L. Miller is a Research Chemist at the FBI Laboratory's Counterterrorism and Forensic Science Research Unit in Quantico, Virginia. He has been working on various chromatographic and mass spectrometric applications in forensic science since joining the FBI in 1992. His research interests include trace analysis in toxicology, drugs, explosives, chemicals and materials. Prior to working at the FBI, he was a Senior Research Chemist for Monsanto Chemical Company in the R&D group. Dr. Miller received a Ph.D. in Analytical Chemistry from the University of North Carolina in Chapel Hill where he was under the direction of Professors Richard Linton and James Jorgenson. He has a B.S. in Chemistry from Indiana University in Bloomington and did research in Professor Milos Novotny's lab. He is an avid Tarheel fan and from a family of UNC graduates or impending graduates.

Parking: Parking is available in nearby commercial parking garages. Please be aware that garage closing times vary. Parking is also available on the street after 6:30 pm, but be aware that most parking meters are in effect until 10:00 pm and may be limited to 2 hours. You should check the individual meters for details and payment methods as some are no longer coin-operated.

Metro: Blue/Orange/Silver Line: McPherson Square or Farragut West; Red Line: Farragut North.
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October Meeting
Wednesday, October 19, 2016
6:00 pm - 8:00 pm at US Pharmacopeia (Directions)

Speaker: Trina Formolo, National Institute of Standards and Technology
Title: Considerations for Optimization of Multi-Attribute Peptide Mapping Protocols

Abstract: Peptide mapping is a widely used methodological platform in the biopharmaceutical industry.  This analytical tool uses the chromatographic profile of enzymatically generated peptides to establish protein identity, evaluate stability and monitor new drug lots for variation.  The use of peptide mapping for multi-attribute method (MAM) applications is becoming more widespread in the industry.  These platforms have been developed to streamline the quality control process by replacing multiple analytical methods with one comprehensive peptide mapping analysis. While a powerful, streamlined data analysis workflow is important in building a successful multi-attribute method (MAM) platform, the platform must also incorporate optimized sample preparation and analysis protocols.  The generation of reliable, meaningful results from any MAM platform begins with quality sample preparation and analysis.  This includes developing robust, reproducible tryptic digestion protocols and optimizing chromatographic separation methods to facilitate the detection and quantitation of critical quality attributes (CQA).

Bio: Dr. Formolo received her BS in biology from the University of Dallas and her PhD in molecular medicine from the Institute for Biomedical Sciences at The George Washington University.   As a research chemist in the Biomolecular Measurement Division within the Material Measurement Laboratory of the National Institute for Standards and Technology (NIST) she focuses on the development of reference materials, methods and data relevant to the biopharmaceutical industry.  Her interests include the mass spectrometry characterization of biotherapeutic proteins.  She recently completed the LC-UV-MS/MS peptide mapping characterization of a recombinant IgG1κ monoclonal antibody (NISTmAb RM 8671) which was recently released as a Reference Material.
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Open House & Poster Session
Wednesday,September 21, 2016
6:00 pm - 8:00 pm at North Bethesda Marriott Hotel and Conference Center

Congratulations to Sam Choi, our 2016 winner of the Georges Guiochon travel award for best student poster at the WCDG Open House & Poster Session on September 21!
Sam Choi from George Washington University won the award for his outstanding poster on "CE-nanoESI-MS for Untargeted Proteomic Characterization of Single Embryonic Cells and Small Neuron Populations". He will receive complementary travel to a separations-related conference of his choice. Congratulations, Sam!.

 We also want to acknowledge our Honorable Mentions, Erika Portero and Rosemary Onjiko from George Washington University, and thank all of our poster presenters, vendors, and attendees for making this year's event a success! Download 2016 Program
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May Meeting
Wednesday, May 18, 2016
6:00 pm - 8:00 pm at US Pharmacopeia (Directions)

Speaker: Milton L. Lee, Professor Dept. Chemistry and Biochemistry, Brigham Young University, UT
Title: Compact Capillary LC Separations

Abstract: Compact, easy-to-use capillary LC systems are desirable for applications that require (or at least would benefit from) instrument mobility, such as for analyses on location (e.g., first responder applications). Furthermore, coupling to mass spectrometry would benefit from mobile instrumentation because the LC system could be located close to the ion source for improved performance, and easily removed when not in use. Portable LC systems are not common due to difficulties encountered in engineering LC pumping and detection systems that provide acceptable weight, robustness, power usage, and mobile phase consumption. We have developed a gradient nano-flow LC system with stop-flow injector that can be easily coupled to miniaturized light-emitting diode (LED) UV-absorption detection or mass spectrometry. The pumping system is comprised of two approximately 30-uL volume syringe pumps that deliver accurate nL flow rates under gradient conditions. The extra-column dead volume of the system is much lower than commercial capillary LC systems. Detection limits have been considerably improved by paying specific attention to improved light focusing, low stray light, low noise, and novel signal averaging routines. Signals down to the ppb level are easily detected. While the system can accommodate small particle packed columns (>15,000 psi), monolithic capillary columns can be used to minimize the pressure drop needed for rapid LC analysis. Fabricated polymeric monolithic columns produce efficiencies approaching 200,000 plates/m (non-retained uracil).

Bio: Milton Lee is Professor of Chemistry in the Department of Chemistry and Biochemistry at Brigham Young University. He received his Ph.D. in Analytical Chemistry from Indiana University in 1975. Dr. Lee’s area of specialization is in microseparation techniques and instrumentation for capillary separation and mass spectrometry. Dr. Lee was involved in the commercialization of the capillary supercritical fluid chromatograph, the atmospheric pressure ionization TOF mass spectrometer, and the hand-portable gas chromatograph toroidal ion trap mass spectrometer. He has over 570 publications, 20 patents, and has mentored 63 doctoral students. He is the recipient of the 2016 LCGC North America Lifetime Achievement Award and the 2012 ACS Award in Separations Science and Technology, among many others. Dr. Lee has also been named on the Analytical Scientist Power List in 2013 and 2015.
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April Meeting
Joint with Washington Baltimore Mass Spectrometry Discussion Group
Monday, April 11, 2016
6:15 PM - 8:00 PM at Shimadzu Training Center, 7100 Riverwood Drive, Columbia, MD 21046

Speaker: Stephen E. Stein, NIST Fellow, Director of NIST Mass Spectrometry Data Center in Biomolecular Measurement Division, Gaithersburg, MD
Title: Mass Spectral Libraries of Everything

Abstract: Libraries of mass spectra of known compounds have long been used for identifying compounds in GC/MS experiments and are finding increased use in tandem LC/MS experiments, especially in metabolomics and proteomics studies. Even given the substantial coverage of current libraries, a large fraction of the spectra remain unidentified. In some areas only a small fraction of components can be identified and even for well-developed areas (GC/MS of urine, for example), the origin of many spectra is unknown and likely to remain so for some time. To characterize these unknowns, we have been involved in building annotated libraries of good quality, but unidentified spectra in GC/MS and LC/MS experiments. Progress in three areas will be discussed: 1) GC/MS – multiple occurrences of spectra at fixed retention indices have been collected, clustered and annotated for a range of materials including urine, essential oils and various NIST reference materials; 2) LC/MS proteomics - we have constructed extensive libraries of unidentified peptide from proteomics analysis and developed special methods for their annotation and identification; 3) LC/MS metabolomics - we have built an collection of unidentified spectra from NIST urine reference materials and developed tools for organizing and identifying them. Illustration of the use of these libraries alongside more conventional libraries of reference spectra of identified compounds will be presented.

Bio: Dr. Stein is a NIST Fellow, Group Leader and Director of the NIST Mass Spectrometry Data Center in the Biomolecular Measurement Division, Material Measurement Laboratory, National Institute of Standards and Technology. He conceives, plans, directs and personally conducts advanced research and development in the area of chemical data analysis, with emphasis on mass spectral data and search algorithms, deconvolution algorithms, quality measurement and new approaches for chemical identification in proteomics and metabolomics, methods for automated chemical data analysis, algorithms for spectra and property prediction from chemical structural data. He received his undergraduate degree in Chemistry at the University of Rochester and did his graduate work at the University of Washington as a NSF pre-doctoral trainee. He then did his post-doctoral training at SRI International in Menlo Park, CA. Over the years his research has culminated in over 120 peer-reviewed publications and numerous awards including the Gold Medal from the Department of Commerce (2015), the Mike Lynch Award from the Chemical Structure Association (2014), and the Presidential Rank Award (2011).
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March Meeting
Wednesday, March 16, 2016
6:00 pm - 8:00 pm at US Pharmacopeia

Speaker: Nicholas H. Snow, Department of Chemistry and Biochemistry, Center for Academic Industry Partnership, Seton Hall University, South Orange, NJ
Title: Six Dimensions of Separations: Are we holding ourselves back with packed column thinking?

Abstract: The advent of readily available high-resolution and sensitivity multidimensional separation and detection techniques such as GCxGC-ToFMS and GC-MS-MS has provided chromatographers with unprecedented separation and detection capability. When combined with on-line sample preparation techniques such as SPME and static headspace extraction, there are now numerous avenues for chromatographers to improve separation selectivity and ultimately resolution. These additional dimensions also provide opportunities to compromise selectivity, especially when combined with historical lessons originally applied to packed columns. Considered holistically, an SPME-GCxGC-ToFMS method actually has up to six dimensions of separation: sampling, extraction, injection, two dimensions of GC and MS detection. Each can generate both desired and undesired selectivity that impacts the ultimate resolution and sensitivity generated by the full method. Using examples from forensic, pharmaceutical and organic contaminant analysis, each of the multiple dimensions of analyses involving SPME, GCxGC-MS and GC-MS-MS will be examined in terms of selectivity (both desired and undesired) selectivity generation and whether they still suffer from packed column thinking. For example, in environmental analysis, it will be shown that, if desired selectivity is maximized and undesired selectivity minimized, the sensitivity of SPME-GC-MS-MS is easily competitive with LC-MS-MS for the analysis of emerging contaminants in water. In pharmaceutical analysis, the six “non-volatile” compounds not included in the standard USP and ICH headspace methods can, in fact, be determined by headspace extraction.  To maximize the potential of GC, all of the six dimensions must be understood and optimized.

Speaker Bio: Nicholas H. Snow is Professor of Chemistry and Biochemistry and Director of the Center for Academic Industry Partnership at Seton Hall University. He is currently teaching advanced undergraduate and graduate courses in analytical chemistry and separation science. He has been recognized twice by the Seton Hall University Board of Regents for outstanding teaching and service to students. He maintains an active research group with projects involving rapid separations of complex mixtures, multidimensional separations, sampling techniques for chromatography, gas chromatography and gas chromatography/mass spectrometry. He is especially interested in working with industrial and private partners in solving difficult analytical problems. He earned his PhD in 1992 from Virginia Tech.
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February Meeting
Wednesday, February 17, 2016
6:00 pm - 8:00 pm at US Pharmacopeia

Speaker: Robert diTargiani, U.S. Army Medical Research Institute of Chemical Defense, Aberdeen Proving Ground, MD
Title: Analytical Methods for the Verification of Human Exposure to the Chemical Warfare Agents

Abstract: While chemical warfare agents (CWAs) have generally been regarded as a threat to the military, events in Japan and more recently Syria have demonstrated that the civilian population is also at risk.  The two main CWA threats are organophosphorus nerve agents and sulfur mustard and unfortunately humans have been exposed to both.  It is important to have analytic methods available to identify those that have been exposed to CWAs and to verify the CWA used. Verification of exposure to CWAs typically involves determinations of urinary metabolites or adducted proteins in blood. While the intact CWA might last for just a few minutes, a biomarker can last for weeks or months (We have detected a CWA up to 42 days after exposure). Methods have been developed at USAMRICD to detect CWAs and its metabolites in blood or urine samples using both LC-MS and GC-MS.

Speaker Bio: Dr. Robert diTargiani received his PhD in chemistry from the Johns Hopkins University in 2004. He currently works at US Army Medical Research Institute of Chemical Defense (USAMRICD) as a research chemist. He is a member of the Medical Diagnostics team and ADME core at the institute. Recently, he has developed a proteomic method to verify exposure of chemical warfare agents and agent fate with high-resolution mass spectrometers. He has also collaborated with other government agencies to adopt liquid chromatography electrospray ionization tandem mass spectrometry (LC-MS/MS) techniques for analysis of organophosphate nerve agent urinary hydrolysis products and assay of protein adducts of butyrylcholinesterase and human serum albumin.
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January Meeting

 

 

Wednesday, January 20, 2016
6:00 pm - 8:00 pm at US Pharmacopeia

Speaker: Steve J. Lehotay, USDA-ARS Eastern Regional Research Center (ERRC), Wyndmoor, PA
Title: Improving the quality of chromatographic peak integration and analytical results without human review in multi-analyte high-throughput methods

Abstract: Are you tired of spending all your time in front of a computer staring at screen-after-screen of hundreds of chromatographic peaks?  Don’t you get frustrated at peak integration software costing thousands of dollars that can’t consistently integrate your chromatograms any better than a teenager?  As a quality control officer, aren’t you sick of all the mistakes you find in the results?  Rather than pulling your hair out over subjective close calls in analyte identifications, wouldn’t you like a simple mathematical method to give yes/no answers with minimal false positives and negatives?  As a manager, do you want higher lab efficiency to analyze more samples and make more money?  If you said yes to any of these questions, then consider good old fashioned summation integration, including noise, at the consistent analyte retention times in your MS(/MS) chromatograms followed by postrun data processing that reliably identifies and determines analyte concentrations with no (or very little) human review.  Comparisons of this approach vs. conventional integrations in both GC- and LC- MS/MS of many real-world chemical residue analyses in foods show that it provides better results overall.

Speaker Bio: Steve Lehotay has worked with USDA-ARS since 1992, starting soon after completing his Ph.D. in Chemistry at the University of Florida, where he also received his B.S. in 1987.  He worked as a Research Chemist at the Beltsville Agricultural Research Center in Maryland until 1999, when he relocated to the ERRC.  Steve’s research involves the development of new methods to efficiently monitor many types of chemical contaminants in food.  He investigates all aspects of the analytical process in his research using diverse techniques in novel and useful ways.  To date, he has authored/co-authored 136 scientific papers and >200 presentation abstracts.  He is a Thomson Reuters Highly Cited Researcher and recipient of a NACRW Excellence Award (2015), ACS-AGRO Innovation in Chemistry of Agriculture Award (2012), and several awards from AOAC Int., including the Wiley Award (2011), and within the USDA, including a Secretary’s Honor Award (2014).
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December Meeting

 

Wednesday, December 16, 2015
6:00 pm - 8:00 pm at US Pharmacopeia

Speaker: Ronald E. Majors, LCGC North America, West Chester, PA
Title: Top Ten HPLC/UPLC Column Myths

Abstract: In any field there are often "misconceptions" or "myths" that are perpetuated and passed on to the next generation. These myths are often driven by a lack of understanding by practitioners of the real issues. And these myths can change as time moves on. Since HPLC is approaching its 50th year, many column myths have already been passed down to 2 generations of liquid chromatographers. Recently, ultrahigh pressure liquid chromatography (UHPLC) has come into its own and a new set of myths are arising. The purpose of this tutorial is to try to dispel some of these myths before they get further perpetuated. Some of the myths to be discussed are: “all C18 columns are the same”; “it takes a minimum of 10 column volumes to re-equilibrate an LC column”; “you can’t reverse an HPLC column to flush out particulates”; “UHPLC packed columns plug easier than conventional HPLC packed columns” and the list goes on. With help of a team of myth-busters, notables in the chromatography field, I will provide proof statements and literature references that showed that these myths are unjustified. There are many myths that are still around but didn’t make the top ten. However, most likely old myths will continue, some will fade away, and new myths will arise as more practitioners enter the chromatography community. Those new arrivals to this community may have to discover these myths on their own (since they don’t necessarily listen to the old timers anyway). Perhaps new myth-busters will take on the next generation of myths.

Speaker Bio: In November, 2013, Ron Majors retired from Hewlett-Packard/Agilent Technologies after 45 years of working in the area of sample preparation and chromatography column and instrumentation technology. He currently serves as a consultant. Ron received his B.S. in chemistry at California State University, Fresno, in 1963 and his Analytical Chemistry Ph.D. degree in 1968 from Purdue University under the direction of L.B. Rogers. His Ph.D. thesis was in the area of molecular-imprinted phases for chromatography and sample preparation. He is the author of over 150 publications in HPLC, GC, sample preparation and surface chemistry. Among his current activities, he has been editor for the monthly feature, "Column Watch" in LC/GC Magazine (33 years) for which he is also serves on the Editorial Board. Dr. Majors has served as Chairman of HPLC '86 and Anabiotec '90 and as a member of the Instrumentation Advisory Board of Analytical Chemistry.  His current interests include sample preparation especially solid-phase extraction and automation, and HPLC and GC column technology. Ron is a lifetime member of The Chromatography Forum of Delaware Valley, a member of the American Chemical Society, and The Chromatography and Separations Chemistry Sub-division of the Analytical Division of the ACS where he had served as Chairman and Secretary. He has also been a member of the Chromatographic Society (U.K.) and Board of Directors for the California Separations Society (CaSSS).  Ron has been an invited lecturer, session organizer, and session chairman at many national and international symposia. Dr. Majors has received many awards from chromatography societies, the most recent being the Chromatographic Society’s 2007 Martin Gold Medal from the United Kingdom, named for the Nobel Prize winner, A.J.P. Martin. Ron and his wife Carol are avid birdwatchers and travel all over the world in search of these feathered creatures.
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November Meeting 

 

Wednesday, November 18, 2015
6:00 pm - 8:00 pm at US Pharmacopeia

Speaker: Claude R Mallet, Waters Corporation, Workflow Integration, Milford, MA
Title: Optimized Workflow for Metabolite Identification using 3D LC/MS/MS

Abstract: The ‘holy grail’ for a biotransformation group is the irrefutable isolation and identification of a putative metabolite.  When achieved, it requires several hours of patient incubation or in vivo sample collection to generate the raw starting material.  This is followed by multiple chromatographic steps, manual fraction collection with concomitant lengthy evaporative steps and compromised losses in yield for gains in purity.  Even with meticulous planning and sample handling, the definitive NMR spectrum is elusive.  It is not uncommon for a purification to absorb 3-6 weeks of dedicated instrument and analyst time with the futile result of a complicated, un-interpretable NMR spectrum.  A reasonable compromise of this fit-for-purpose process would be to automate the isolation and purification steps.As new technology emerges, new options become available thus bringing effective performance for difficult applications.  The concept of hyphenated systems or multi-dimension chromatography was designed for solving complex analyses. The peak capacity or separation power can be increased by combining several separation dimensions (most instances utilize two) each using optimized conditions for maximum resolution.  The main challenge is the transfer of closely resolved analytes from the primary resolving dimension (PRD) to the secondary resolving dimension (SRD).  The concept of multi-dimensional-chromatography is a well established technique for the analysis of complex mixtures.  However, since its beginning, the technique is also perceived as highly complex in term of hardware and also difficult to gain in depth insight for practical usage. In recent years, advances in software control and automation, are enabling hyphenated instrumentation platforms to offer enhance performances. The use of multi-fluidic circuits can decrease sample handing in term of time, resources and consumable.  In this application, an intermediate API entity from a reputable pharmaceutical will be use to demonstrate the 3D LC/MS/MS workflow process.

Speaker Bio: Dr. Mallet received his Ph.D. in analytical chemistry from the University of Montreal, Montreal, Canada (1997).  His thesis was entitled “Time-Coupled-timed-Resolved Chromatography or TCRC”.  This new hyphenated system was based on an experimental GC/GC/MS/MS orthogonal chromatograph using a mobile heated pulse.  In 1997, Dr. Mallet was hired as a senior application chemist in several biotech, contract research organization (CRO’s) and life-science firms, before accepting a senior scientist’s position at Waters Corporation in 2000. From his doctoral work with Time Decoupled Chromatography concept, the technique was extended to Waters Liquid Chromatography portfolio.  Since 2013,  Dr. Mallet is currently a senior scientist with the Separation Technology Division and pursuing research interest in automated 2D & 3D LC/MS/MS technologies.

2015 George Guiochon Student Poster Award recipient, Jason Reck from University of Virginia, will present his work 6:45 pm - 7:00 pm.
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October Meeting
Wednesday, October 21, 2015
6:00 pm - 8:00 pm at US Pharmacopeia

Speaker:  Irving W. Wainer, PhD, DHC,  Chief Scientific Officer, Mitchell Woods Pharmaceuticals
Title: The adventures of a bioanalytical chemist in the never-never land of antidepressants: Finding a way out of the “ketamine paradigm”

Abstract: (R,S)-Ketamine is a chiral phencyclidine derivative that produces rapid and short-lived anesthesia via inhibition of the N-methyl-D-aspartate (NMDA) receptor. The anesthetic activity of this drug has been associated with the parent compound and to a lesser degree with the N-demethylated metabolite (R,S)-norketamine, while other (R,S)-ketamine metabolites were designated as “inactive”, the “Ketamine Paradigm”. Recent studies demonstrated that a single sub-anesthetic dose of (R,S)-ketamine produces rapid and profound antidepressant response.  As part of our studies of this effect in patients with treatment-resistant and bipolar depression, we developed a stereoselective  lc/ms/ms assay capable of quantifying all of the major (R,S)-ketamine metabolites. The analysis of plasma samples demonstrated that (R,S)-ketamine was rapidly transformed in to multiple metabolites including (R,S)-dehydronorketamine and (2S,6S;2R,6R)-hydroxynorketamine and that these metabolites were associated with clinical response. The dehydro and hydroxy metabolites of (R,S)-ketamine are weak NMDA inhibitors, raising the question of the viability of the “Ketamine Paradigm” as an explanation (R,S)-ketamine’s antidepressant effects.  In addition, pharmacometabolomics analysis identified a positive relationship between reduced D-serine plasma levels and response and a second study demonstrated that basal D-serine plasma levels predict antidepressant response.  This talk will address how our ability to accurately measure chemical and biological changes led us to a new “Ketamine Paradigm” and new antidepressant drugs.

Speaker Bio: Professor Irving W Wainer is Chief Scientific Office for Mitchell Woods Pharmaceuticals. He received his PhD degree in chemistry from Cornell University and did postdoctoral doctoral studies in molecular biology (University of Oregon) and clinical pharmacology (Thomas Jefferson Medical School).  He worked for the FDA as a Research Chemist, at St. Jude’s Children's Research Hospital (Associate Member), McGill University (Professor, Department of Oncology), Georgetown University (Professor, Department of Pharmacology) and until March 31, 2014 as Senior Investigator, National Institute on Aging/NIH.  Professor Wainer has published 375 scientific papers, 10 books, holds 11 patents, and was founding editor of the journal Chirality and Senior Editor of the Journal of Chromatography B. His awards include: the "A.J.P. Martin Medal" presented by The Chromatographic Society; Elected Fellow of the American Academy of Pharmaceutical Sciences; Doctor Honoris Causa degrees awarded by the Medical University of Gdansk and University of Liege, the 2013 Dal Nogare Award and the 2013 Eastern Analytical Symposium Award for Outstanding Contributions to the Fields of Analytical Chemistry. Professor Wainer’s research in chromatographic science is centered on the development of new chromatographic methods for the online study of ligand-receptor interaction and drug screening.  Professor Wainer’s laboratory is also engaged in the development of new therapeutic agents for the treatment of oncologic and CNS diseases.
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September Poster Session
Thursday, September 17, 2015
6:00 pm - 8:00 pm
Bethesda North Marriott Hotel
5701 Marinelli Road, North Bethesda, MD 20852

If you have presented a separations related poster at a scientific meeting recently, submit your abstract and present the poster at our event.  There is no cost to attend, and there will be plenty of oppSave & Closeortunities to network with other local scientists and begin or strengthen collaboration in our area.

This will be the inaugural year for the Georges Guiochon Student Travel Award, which will provide for travel expenses and registration to HPLC 2016 in San Francisco, CA, as well as the opportunity to present the winning student's work at an upcoming WCDG meeting. Student posters (undergraduate & graduate students) will be judged at the poster session, and we encourage our members (and their students) to submit poster titles and abstracts as soon as possible. Posters which have been recently presented at other meetings are both allowed and encouraged.
Jason Reck (University of Virginia) is the recipient of the Georges Guiochon Student Travel Award to attend 2016 HPLC Conference in San Francisco.
Camille Lombard-Banek (George Washington Univeristy) received Honorable Mention and a $500 award for travel. Contact: clombard@gwu.edu

This year we are also offering the opportunity to self-identify as "seeking opportunities" or "offering opportunities" for the purposes of job hunting, and we will mark your badge accordingly. If you are looking for new opportunities, please bring your resume and/or business cards. If you represent a company that is seeking new talent, please identify one person that would like to discuss the opportunities your company can offer to potential new employees.

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May Meeting
Wednesday, May 20, 2015
6:00 pm - 8:00 pm at US Pharmacopeia

Speaker:  Dr. Jianghao Sun, Research Associate, Food Composition and Method Development Lab Beltsville Human Nutrition Center, USDA-ARS
Title:  Fingerprinting and Metabolomics for Botanical Authentication and Identification of Dietary Biomarkers

Abstract:  Metabolomics is a rapidly developing area which aims to profile small-molecules to support research on complex biological systems. The strategy used in metabolomics has shown great potential for food and nutrition sciences. In this presentation, the qualitative evaluation of botanical and related dietary supplements, identification of dietary biomarkers under different dietary patterns, and chemical changes during food storage/processing will be discussed using HPLC/UHPLC-MS fingerprinting and metabolomic approaches based on the work in this lab.

Speaker Bio:  Dr. Jianghao Sun obtained his Ph.D from the Peking University (Top 1 in China) in 2007 majoring in Phamacognosy. He moved to the U.S. in the late 2009 and joined Food Composition and Method Development Lab (FCMDL) at Beltsville Human Nutrition Center (BHNRC) of USDA-ARS as a post-doctoral fellow under cooperative agreements with Johns Hopkins University and University of Maryland. Then he was promoted as a research associate of FCMDL in 2014. Dr. Sun has 8 years of research and working experience primarily as a mass spectrometrist and food chemist. The training and work experience at FCMDL made him an expert of food constituents analysis, food composition and nutritional research. He had been worked on developing the liquid chromatography tandem mass spectrometry based fingerprinting and metabolomics approaches for food/botanical authentication, food component and dietary biomarker analysis. Dr. Sun has authored and/or co-authored more than 40 peer-reviewed papers. Many of his papers were published in the top peer-reviewed journals such as Journal of Agricultural and Food Chemistry, Food Chemistry, Anal and Biochemical Chromatography and Journal of Chromatography A. Furthermore, he presented his research findings at many professional conferences, and has served as a reviewer for 11 peer-reviewed journals in the area.
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April Meeting
Joint with Washington-Baltimore Mass Spectrometry Discussion Group (MSDG)
Wednesday, April 15, 2015
6:00 pm - 8:00 pm at US Pharmacopeia

Speaker:  Dr. Matthew C. Crowe, The Dow Chemical Company, Philadelphia, PA
Title:  Multidimensional Liquid Separations Coupled to Electrospray Ionization Mass Spectrometry for the Analysis of Complex Polymers
Co-Authors:  Lu Bai, Miroslav Janco

Abstract: In an effort to comprehensively characterize the molecular structure of complex tetrapolymers up to 10,000 u, multidimensional separations coupled to electrospray ionization mass spectrometry (ESI/MS) were developed. Polymers composed of four different monomers were characterized to determine if performance differences could be correlated with differences in molecular structure. The polymers were analyzed with negative polarity ESI/MS, taking advantage of the presence of a permanent negative charge on one of the monomers. Direct infusion ESI/MS experiments did not provide full molecular weight coverage, so ultrahigh performance liquid chromatography (UHPLC) ESI/MS methods were developed which allowed separation of polymer components by molecular structure and the observation of a wider polymer molecular weight range with mass spectrometry. The UHPLC/ESI/MS results were dominated by low molecular weight polymer signals, making sample-to-sample comparisons difficult. To combat this, a size exclusion chromatography (SEC) fractionation technique was developed to separate polymer components by molecular weight prior to UHPLC/ESI/MS analysis. SEC fractionation followed by UHPLC/ELSD and UHPLC/ESI/MS of collected fractions was used to analyze complex tetrapolymers, increasing the mass range observable with ESI/MS over what was seen with direct infusion ESI/MS and UHPLC/ESI/MS. The results of these experiments will be presented, along with what was learned about the strengths and limitations of this analytical approach. Data analysis allowing statistical differentiation of complex polymer samples will also be discussed.

Speaker Bio: Matthew (Matt) C. Crowe received his Ph.D. in Chemistry from the University of Texas at Austin (2005) and a B.S. in Chemistry from the University of North Carolina at Chapel Hill (2000). Following graduate school, Matt served as the director of the mass spectrometry facility in UNC-Chapel Hill’s chemistry department. In 2008, Matt began work as a post-doctoral researcher at the University of Washington in Seattle doing UHV adsorption microcalorimetry. In 2010, Matt left Seattle to begin work as a Senior Analytical Chemist-Mass Spectrometrist at The Dow Chemical Company in 2010. In 2014, Matt was promoted to his current position of Associate Research Scientist at Dow, with technical focus on liquid separations and mass spectrometry. Matt has been a member of several scientific societies over the years, including the American Chemical Society (ACS), the American Society for Mass Spectrometry (ASMS), and the American Vacuum Society (AVS). He has served as a manuscript reviewer for Langmuir (2007), on the ASMS program review committee (2007 & 2008), and as a career panelist for the Center for Enabling New Technologies Through Catalysis (CENTC) (2009-2010). Matt has served on several awards committees and regularly organizes and chairs symposia for the ACS and ASMS. Matt has served as a director (2012-2013), Chair (2014), and is currently Past Chair and Councilor for the Trenton local section of the ACS.
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March Meeting
Chromatography Community Mixer at PittCon
Tuesday, March 10, 2015
5:30 pm - 8:30 pm
Generations Hall, 310 Andrew Higgins Dr.
New Orleans, LA
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February Meeting
Wednesday, Feburary 11, 2015
6:00 pm - 8:00 pm at US Pharmacopeia

Speaker:  Dr. Rabih Jabbour, Edgewood Chemical Biological Center, Edgewood, MD
Title:  Utilization of a Mass Spectrometry Proteomics Method for Detection of Biological Agents and Toxins in Complex Matrices

Abstract: Food safety and bio-surveillance are growing fields of interest to government and private sectors, as a necessary action to protect ourselves from threats disseminated through the food system. Nefarious individuals can and have intentionally contaminated food sources using biological warfare agents and other pathogens. Methods to detect the causative agent can be laborious and often require enrichment of the sample as well as a reasonable assumption of what the pathogen may be. A mass spectrometry based proteomics method (MSPM) has been developed for identification and classification of pathogens including bacteria, viruses, and toxins. The MSPM and does not require prior knowledge of microbes in the sample or an enrichment step. Utilization of MSPM in the detection and identification of food borne toxins is advantageous over genomic based methods because those toxins are proteinaceous substances with no genomic complimentary compounds.

Speaker Bio: Dr. Jabbour holds a Ph.D. in bioanalytical chemistry with more than 15 years of research experience in academia and industry in the field of chemistry and biology of microorganisms that are of vital interest to the Department of Defense. He is leading the development of the automated sample processing system for extraction and preconcentration of biological biomarkers for the detection and identification biological warfare agents down to strain level using mass spectrometry technology. His instrumentation expertise is in the area of bioseparation techniques, preconcentration of biological biomarkers method and engineering development, optical spectroscopy, chromatography and mass spectrometry. He has contributed to various DOD and DHS projects such as water monitoring and microbial fate using Raman imaging for JSAWM, toxin fate by LC-MS, Biowatch-DHS, and microbial mapping by MALDI-MS for EPA projects. He was awarded the DTRA "Best Basic Research Award" and SAIC as " Excellence in Science Award". He serves as a reviewer of articles with J. Analytical Chemistry in the area of microbial proteomics and genomics; acted as a volunteer for the ASTM committee on Raman Imaging standard operation procedure. He has published over 25 peer-review articles and proceedings in the field of chemistry, biochemistry, spectroscopy, molecular biology, bacteriology, and protein chemistry.
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January Meeting
Wednesday, January 21, 2015
6:00 pm - 8:00 pm
US Pharmacopeia
Speaker:  Dr. Jeffrey W. Hudgens, NIST, Gaithersburg, MD
Title:  Hydrogen-Deuterium Exchange Mass Spectrometry: A Valuable Tool for the Biopharmaceutical Industry

Abstract: In recent years many biopharmaceutical companies have established hydrogen-deuterium exchange mass spectrometry (HDX-MS) laboratories. Such facilities contribute to the research of drug mechanisms, of protein-ligand and protein-protein interactions, and of determinations of protein functional changes induced by environment and post-translational modifications. HDX-MS measurements involve immersion of protein or glycoprotein samples in a D2O solution, rapid protease digestion of the protein to peptides, separation of the peptides on a cold (1 °C) UPLC, and mass measurements by high resolution mass spectrometry. Evaluation of HDX-MS data can determine the hydrogen exchange rates of amide hydrogens along protein chains. These H/D exchange rates are substantially governed by three-dimensional protein structure. HDX-MS quality could be substantially improved if the UPLC can be operated at lower temperature, e.g., 20 °C. To develop a HDX-MS program that is responsive to the needs of the biopharmaceutical industry, our NIST laboratory has conducted research to gain experience with problems similar to those encountered by the biopharmaceutical industry. First, we developed a new mass spectrometry method involving electron transfer dissociation (ETD) that enables determinations of the deuterium uptake by glycans within glycoproteins. The resulting increase in D-uptake measurement accuracy allowed us to demonstrate that changes in the glycan structure within glycoproteins can cause measurable changes in the HDX-MS patterns. This result is important for evaluation of similarity among biosimilars. Secondly, we present a case study where HDX-MS accelerated elucidation of a mechanism by which a small regulating protein induces the unclamping of the homotrimer, proliferating cell nuclear antigen (PCNA), from DNA. The approach is important for epitope characterization.

Speaker Bio: Dr. Jeffrey Hudgens researches methods that enable H/D exchange mass spectrometry (HDX-MS) to measure the similarity among an innovator drug, its subsequent production lots, and its competing biosimilars. His HDX-MS studies also include ligand interactions with proteins and transmembrane proteins. Dr Hudgens received his BS in Chemistry from Miami University (Ohio) and his PhD in Physical Chemistry from the University of Illinois at Urbana. He was awarded a National Research Council Postdoctoral Associateship at the Naval Research Laboratory. He remained at NRL for another seven years as a staff scientist, where he pioneered applications of laser spectroscopy and mass spectrometry. In 1984 he moved to the National Bureau of Standards (now NIST). His 125+ scientific publications and two patents span many disciplines including biochemistry, optical spectroscopy, mass spectrometry, chemical kinetics, thermochemstry, and nanochemistry. His awards for metrology include the Chemical Science Technology Laboratory’s Technical Achievement Award and a Bronze Medal. Dr. Hudgens is a Fellow of the American Physical Society.
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December Meeting
Wednesday, December 17, 2014
6:00 pm - 8:00 pm
US Pharmacopeia
 
Speaker:  Dr. Bill LaCourse, University of Maryland Baltimore County, Baltimore, MD
Title:  Adventures in Analysis:  New Approaches to Old Problems

Abstract:  The University of Maryland, Baltimore County (UMBC) has been at the forefront of new and innovative ways to promote student success. Motivation is a key ingredient of persistence. One approach is to provide opportunities for undergraduate and graduate students to work on real-world problems using high-end analytical instrumentation (e.g., mass spectrometers, NMR, HPLC, GC and spectroscopy). In doing so, students learn to collaborate, critically think, communicate, and learn marketable skills. We are achieving this goal by reinventing the typical “core” facility at a university into an active teaching and learning environment, which is operated by a facility manager under the College of Natural and Mathematical Sciences. This presentation will visit an array of analytical applications being investigated in the Molecular Characterization and Analysis Complex (MCAC), which in itself is a new approach for an old problem. One of the oldest analytical techniques in separation science is thin layer chromatography (TLC). This technique has always suffered from lack of ability to rapidly identify separated compounds.  In the MCAC, we have developed an ambient ionization source for mass spectrometry that functions as a surface analysis reader. In a matter of minutes, it can non-destructively scan an entire TLC plate and get mass spectra of each of the spots. This novel approach solves the age old problem of inconclusive information from TLC analysis. The separation and direct detection of carbohydrates and glycans has been successfully accomplished using high performance anion-exchange chromatography followed by pulsed amperometric detection (HPAEC-PAD). A continuing analytical challenge has been the selective identification of carbohydrates versus other compounds, especially for complex samples. Typically, this problem is overcome by offline clean up and isolation. We have been working on the development of multiplex-pulsed amperometric detection (MPAD), which allows the analyst to confirm the presence of glycans/sugars from peptides and other interferences without the need for offline prep or multiple runs. Another issue that has plagued us all is sensitivity, or how low can one go! Since the human olfactory system can sense off flavor compounds (OFCs), such as geosmin, as low as 10 ppt, it is imperative that analytical methods be able to quantitate below these levels. The MCAC has been working on the development of a method for OFCs using gas chromatography with mass spectrometry. Through the use of an improved chromatographic separation, optimized mass spectroscopy parameters, and a novel online trap and purge for a head space sampler, we have been able to achieve parts per quadrillion limits of quantitation and detection for water samples. In conclusion, the MCAC has developed into an active learning facility, which supports internal and external researchers and scientists, for inspiring students to persist in STEM. This presentation will highlight several of their achievements.

Speaker Bio: William R. LaCourse is the Dean of the College of Natural and Mathematical Sciences and Professor of the Department of Chemistry and Biochemistry at the University of Maryland, Baltimore County (UMBC). He is also a Kauffman Fellow of Entrepreneurship, and past CEO/cofounder of Aurora Analytics, LLC. He received his Ph.D. in Analytical Chemistry from Northeastern University in 1987. After completing a postdoctoral appointment at Ames Laboratory, he held the position of Scientists at Iowa State University/Ames Laboratory until he joined the faculty at UMBC in 1992.  In 2005, he founded UMBC’s Chemistry Discovery Center, which has dramatically improved student performance in introductory chemistry courses and now oversees the College’s Active Science Teaching & Learning Environment (CASTLE), which is designed to study active-learning pedagogies across the STEM disciplines. In addition to his administrative experience at the University level, Dr. LaCourse has five years of industrial experience in the pharmaceutical industry on the development of product assays of both human and veterinarian formulations. His research interests include basic and applied research on hydrodynamic electroanalytical techniques in chromatographic and electrophoretic systems. He has 111 publications, including 20 chapters and a sole-authored book entitled Pulsed Electrochemical Detection in High Performance Liquid Chromatography, and two issued patents. He has made over 250 presentations at national and international meetings.  Dr. LaCourse is the recipient of several chemistry and research awards, an Editorial Advisor for Analytica Chimica Acta, an Associate Director of the California Separation Science Society (CASSS), and an active member of local and national professional societies and groups.
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November Meeting
Wednesday, November 12, 2014
6:00 pm - 8:00 pm
US Pharmacopeia

Speaker:  Dr. Abul Hussam, George Mason University, Fairfax, VA
Title:  Measurement of Noncovalent Association and Partitioning of Volatile Solutes by Equilibrium Headspace Gas Chromatography:  Applications in Solvent Extraction, Surfactants, and Nanoparticles

Abstract:  An equilibrium headspace gas chromatographic technique (eHSGC) was developed to measure noncovalent association and partitioning of n-alkylbenzenes in water with substrates such as immiscible solvents for liquid-liquid extraction (LLE), natural (fulvic and humic acids) and synthetic surfactants, and nanoparticles. A general theory based on two step reactions and the experimental methodology were developed to obtain solute-substrate association constant (K11), critical substrate association concentration (cac), and solute-aggregate association constant (Kn1). These parameters were used to calculate the vapor/liquid partition coefficients, infinite dilution activity coefficients inside the aggregate pseudophase, and transfer free energies of alkyl chain – ΔG◦CH2. These values were obtained without the solute concentration, and without a calibration. The existence of a water rich substrate pseudophase is inferred from ΔG◦CH2 values in various phases.  In water-fulvic acid system the inter-aggregate transfer free energies indicate that the aggregate pseudo-phase is more polarizable benzene-like and less n-alkane aliphatic-like. The problem of defining association and partition constants with nanoparticles is discussed.

Speaker Bio:  Abul Hussam is a Professor of Chemistry and the Director for the Center for Clean Water and Sustainable Technologies (CCWST) in the Department of Chemistry and Biochemistry at George Mason University. Dr. Hussam earned his Ph.D. in Analytical Chemistry from University of Pittsburgh in 1982. His research and teaching areas include analytical chemistry, environmental chemistry, and chemistry in organized media. He has published and presented over 100 scientific papers. Professor Hussam was awarded the 2007 Grainger Challenge Prize for Sustainability from the US National Academy of Engineering (NAE) for the SONO arsenic filter, which is now used by hundreds of thousands of people in the affected areas of Bangladesh, Nepal, India, and Pakistan.
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October Meeting
Wednesday, October 15, 2014
6:00 pm - 8:00 pm
US Pharmacopeia

Speaker:  Dr. Peter Nemes, The George Washington University, Washington, DC
Title:  Metabolic Analysis of Single Cells in Embryos by Mass Spectrometry

Abstract:    Measurement of small-molecule changes during embryo development raises a potential to aid the understanding of basic processes underlying states of health and disease, but this requires specialized analytical tools. Particularly needed are technologies that are able to address diverse types of small molecules with single-cell resolution. Although mass spectrometry is the modern method of choice for the measurement of metabolites, typical workflows in the field combine a large cohort, often millions, of cells to improve detection performance. Because pooling inherently averages out the analytical signal among components of the sample, chemical information specific to each cell is lost in this approach.  It would be transformative for cell and developmental biology to extend mass spectrometry to metabolites in developing embryos, but this depends on the development of high-sensitivity mass spectrometry platforms. In this talk, we will explore a single-cell mass spectrometry technology we have recently developed to decipher the metabolic composition of single cells in early-stage embryos of the South African clawed frog (Xenopus laevis), the favorite model in cell and developmental biology. Our approach relies on dissection of single cells from 2- to 16-cell embryos.  Extracts are measured using a custom-built single-cell capillary electrophoresis electrospray ionization system that is coupled to a commercial time-of-flight mass spectrometer. High-efficiency separation, accurate mass measurements, and tandem mass spectrometry have enabled us to confidently identify an appreciable set of metabolites in the metabolome of embryonic cells. Based on this information, we found that certain cell types exhibit metabolic heterogeneity in 16-cell Xenopus embryos. We anticipate that the adaptation of mass spectrometry to single embryonic cells holds exciting, new opportunities for cell and developmental biology as well as other fields where samples are limited in volume or mass.

Speaker Bio:  Peter Nemes, Ph.D., is an Assistant Professor of Chemistry (2013–Present) at the George Washington University, Washington DC, whence he obtained his Ph.D. in Chemistry in 2009. He completed his postdoctoral research in Bioanalytical Chemistry for Neurobiology at the University of Illinois—Urbana-Champaign, IL.  In 2011, he assumed a Laboratory Leader position with the US Food and Drug Administration (Silver Spring, MD), where he established a mass spectrometry facility and regulatory research program with the US Public Health Emergency Medical Countermeasures Enterprise to develop a scientific framework permitting to combat present and future threats (chemicals and biologics) to the public. Prof. Nemes’ current research at the George Washington University is focused on the development of next-generation mass spectrometry platforms to assess the metabolome and proteome of volume-limited samples including single cells.  Prof. Nemes has authored and co-authored 3 book chapters and 24 peer-reviewed publications, and has presented or co-presented the results at 30+ national or international conferences. He has received the 2008 International Research Fellowship Award by the Dimitris N. Chorafas Foundation (Switzerland), the 2009 The American Institute of Chemists prize in Chemistry by The American Institute of Chemists (Washington, DC), the 2010 Science and Technology Innovation Award by Baxter Healthcare Corporation (Chicago, IL), and the 2011 Special Recognition Award by the US Food and Drug Administration. Prof. Nemes is the co-inventor of laser ablation electrospray ionization (LAESI) mass spectrometry and holds four shared patents for the technology.
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May Meeting
Wednesday, May 21, 2014
6:00 pm - 8:00 pm
US Pharmacopeia

Speaker:  Theodore Juarez, MSPH, Uniformed Services University, Bethesda, MD
Title:  Inter-variability of INFICON HAPSITE ER Instruments (man-portable Gas Chromatograph/Mass Spectrometer) operated with Manufacturer Provided Calibration Curves
 
Objective: Determine if the person-portable gas chromatograph/mass spectrometer (INFICON® HAPSITE ER) has comparable inter-instrument accuracy when using the same manufacturer-provided calibration curves.
Results: HAPSITE sample volumes ranged from 95% - 118% of manufacturer designed flow rate. Concentration accuracy ranged between 44% - 218% average agreement with certified concentrations over 34 TO-15 chemicals.  ANOVA analysis demonstrated the instruments differed in their estimate of concentrations (α = 0.05).
Conclusions: A means of manually adjusting the flow rate would increase the concentration estimate confidence. A single calibration curve used on multiple instruments does not achieve equivalent accuracy.  Additional internal standards could potentially increase confidence and accuracy. At 1 ppm, compared with typical 8-hour time-weighted average occupational exposure limits, there is not a significant uncertainty concern.  However, if the instrument were used to assess ceiling, immediately dangerous to life or health or peak exposure limits, the observed uncertainty is potentially a significant concern for human health risk assessment.
 
Speaker Bio: Theodore Juarez is a Lieutenant Commander and an Industrial Hygienist in the United States Navy. He has a Bachelors of Science degree in Chemistry from California Polytechnic State University, San Luis Obispo where he did research in the synthesis of beta-lactam antibiotics. He has a Masters of Science degree in Public Health with a concentration in Industrial Hygiene from San Diego State University, where he conducted GC/MS analysis of nicotine, cotinine and polycyclic aromatic hydrocarbon content in household dust and analysis of their distribution among smoking, non-smoking households and their relation to traffic exposure. While deployed in support of Operation Iraqi Freedom, he conducted numerous Occupational and Environmental Health Site Assessments using person-portable chemical detection equipment, including GC/MS, and became interested in research involving development and evaluation of novel sampling and analysis methodologies for chemical compounds of military and occupational health relevance. He is currently a PhD candidate at the Uniformed Services University of the Health Sciences. He is a member of the Golden Key International Honors Society, Alpha Chi Sigma Professional in Chemistry Fraternity, past recipient of the American Industrial Hygiene Foundation Scholarship and a student member of the American Industrial Hygiene Association and the American Chemical Society.
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April Meeting
Monday, April 14, 2014
6:15 pm - 8:15 pm
Joint Meeting with Washington-Baltimore Mass Spec Discussion Group
Shimadzu Training Center
Speaker:  Maureen Kane, Ph.D., University of Maryland, School of Pharmacy
Title:  The use of fast HPLC multiplexing MRM3 for retinoic acid quantitation in complex matrices

Abstract: Vitamin A is essential to numerous physiological processes including cell proliferation, differentiation, immune response, development, reproduction, cellular metabolism, and nervous system function. Metabolism activates vitamin A into an active metabolite, retinoic acid (RA), which controls gene transcription through activating nuclear receptors and can also function via non-genomic mechanisms. Because the action of RA is amplified through its signaling mechanisms and represents a key signaling node, the abundance of endogenous RA is strictly controlled. Quantification of endogenous RA is essential to understanding its biological actions and the consequences of disruption to the retinoid pathway. Additionally, there are endogenous RA isomers with distinct biological actions must be resolved to achieve accurate quantification and a full understanding of RA function. Here we describe a Fast HPLC multiplexing MRM3 assay that was developed, characterized, and applied to the detection and quantitation of RA isomers from complex matrices in order to remove interfering signal that is observed with MRM detection during some chromatographic separation systems. The combined integration of Fast HPLC using fused-core particles with an embedded polar group C18 stationary phase, LC multiplexing, and MRM3 detection is a novel combination of analysis methodology which resulted in resolution of endogenous (isobaric) RA isomers, rapid analytical throughput and enhanced specificity without compromising assay sensitivity.

Speaker Bio: Maureen A. Kane, Ph.D., is an Assistant Professor in the Department of Pharmaceutical Sciences at the University of Maryland, School of Pharmacy and Co-Director of the University of Maryland, School of Pharmacy Mass Spectrometry Center. She received a B.S. in Chemistry from Canisius College (Buffalo, NY) and a Ph.D. in Analytical Chemistry from the University at Buffalo, State University of New York. She completed postdoctoral training at the University of California, Berkeley. She has published 43 papers in peer-reviewed journals and two book chapters. The Kane Lab uses mass spectrometry to answer biological questions in a quantitative manner. Dr. Kane specializes in retinoid metabolism and quantitative analysis of active metabolites via mass spectrometry.  Retinoids (compounds that exhibit vitamin A activity) regulate cell proliferation, differentiation, apoptosis, development, nervous system function, reproduction, and the immune response. Her tandem mass spectrometric methods for retinoic acid detection have been used to establish functional links between retinoid metabolism and normal physiological function, development, and various disease states. In addition to retinoid metabolism, the Kane Lab has a number of other foci including mass spectrometry imaging, biomarker discovery and validation, targeted and untargeted metabolomics/lipidomics, assay development, and PK/PD profiling.
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Pittcon Mixer
Tuesday, March 4, 2014
5:30 - 8:30 PM
Buddy Guy's Legends, 700 S Wabash Ave, Chicago, IL
Pictures
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March Meeting
Wednesday, March 19, 2014
6:00 pm - 8:00 pm
US Pharmacopeia

Speaker:  Trina Formolo, Ph.D., NIST, Gaithersburg, MD
Title: Resolution of Sialylated Glycopeptides Using a Pentafluorophenylpropyl (PFP) Stationary Phase

Abstract: Protein-based therapeutics comprise a fast-growing class of pharmaceuticals.  However, the inherent variability of these biologics poses a challenge to the industry.  Protein drugs with the same primary structure can vary greatly in their glycosylation patterns, which in turn can affect many properties of the drug, including safety, efficacy and stability.  Characterizing these glycan structures is therefore an essential step in the evaluation of protein biologics. For proteins that carry multiple glycosylation sites it is often necessary to not only identify each glycan structure present, but also map each structure to the individual occupied sites.  This can be performed via enzymatic digestion of the protein followed by glycopeptide enrichment and LC-MS/MS analysis.  This presentation will discuss the use of a pentafluorophenylpropyl (PFP) stationary phase to resolve enriched sialylated glycopeptides and compare its chromatographic properties with the commonly used C18 and bridged ethyl hybrid (BEH) phases.
Speaker Bio:  Dr. Trina Formolo holds a post-doctoral position at the National Institute of Standards and Technology (NIST) and has been working with her mentor Dr. Karen Phinney in the Biomolecular Measurement Division since May 2012.  Trina received her B.S. in Biology from the University of Dallas in Irving, Texas, and her Ph.D. in Molecular Medicine from The George Washington University Institute for Biomedical Sciences under the mentorship of Dr. Yetrib Hathout in the Center for Genetic Medicine Research at Children’s National Medical Center in Washington, DC.  There she performed proteomic analyses of the glioblastoma secretome to elucidate the mechanisms of tumor cell aggressiveness as well as characterization of the glycoprotein chitinase-3-like protein 1 and its role in this process.  Trina’s work at NIST is focused on the development of standard reference materials for the biopharmaceutical industry as well as the development of methods for glycoprotein quantitation.
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February Meeting
Wednesday, February 12, 2014
6:00 pm - 8:00 pm
US Pharmacopeia

Speaker:  Fabrice Gritti, Ph.D., University of Tennessee, Knoxville, TN
Title: Importance and constraints of the recent progress made in column and instrument technologies for accurate sample quantification by HPLC

Abstract:   The quantitative analysis of real mixtures by high performance liquid chromatography (HPLC) requires the complete separation of the target compounds from the other sample components. Then, their accurate and precise quantification may be obtained by using highly controlled protocols if standard solutions of these target compounds are available. Excellent repeatability of the injection device, the column flow rate, the system temperature, the response of the detector, and other column and system performance are to perform reliable quantitative analysis. The increasing complexity of the samples provided by the new requirements brought by genomics, proteomics, or food analyses is constantly demanding advanced performance from the LC column and the instrumentation. High peak resolution is required for accurate quantification. As a result of recent progress, the column volume, the size of the particles with which they are packed, and the analysis times have decreased. The reproducibility of instruments improved. Yet, columns must be operated under pressures as high as 1300 bar and can no longer be run under isothermal conditions. Often, the instrument contribution to band broadening limits the column performance because instrument technology has progressed more slowly than column performance. This makes difficult the transfer of classical slow HPLC methods to advanced UPLC methods. This presentation will discuss the evolution of the performance and robustness of HPLC systems from the 1990s to today (e.g., from the 1090 HP to the 1290 Agilent) and the modern requirements of reliable sample quantifications. Then, we report on column-to-column repeatability (retention, retention, and efficiency), on the evolution of column resolution power and on our expectations for further improvements of column technology. Finally, the possible negative impacts of modern instruments on the resolution provided by highly efficient columns and of the use of very high pressures in fast gradient analyses on data reproducibility will be illustrated.

Speaker Bio:  Fabrice G. Gritti received a B.S. degree in Chemistry and Physics from the University Joseph Fourier of Grenoble (France) in 1995, a graduate Engineering school degree in Chemistry and Physics from the University of Bordeaux I (France) in 1997, and a Ph.D. in Chemistry and Physics from the University of Bordeaux I (France) in 2001.  He came in the U.S. in 2002 for a post-doctoral study at the University of Tennessee with Prof. Georges Guiochon. He is now a Research Scientist in the Department of Chemistry at the same university. Fabrice’s research interests involve liquid/solid adsorption thermodynamics and mass transfer in heterogeneous media for characterization and design of new HPLC column technology.  He developed experimental protocols that helped refine (1) the models of adsorption isotherms used in preparative chromatography for the prediction of the band profiles of neutral and ionizable compounds and (2) the theory of band broadening along analytical columns in linear chromatography.  He has published over 190 papers.
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December Meeting
Joint Meeting with the Chemical Society of Washington
Wednesday, December 11, 2013
6:00 pm - 8:00 pm
ACS Headquarters, 1155 16th St NW, Washington, DC

Speaker:  Isiah Warner, Ph.D., Louisiana State University, Baton Rouge, LA
Title: GUMBOS: Tunable Materials for Biomedical Applications

Abstract:   Modern analytical methods continue to improve the ability of analysts to sensitively identify and quantify the structure and composition of complex drugs. The increased information content these technologies provide increases the level of assurance of these products' quality. For this reason, the FDA has investigated the use of information rich analytical techniques to assess the quality of complex drug products including therapeutic proteins, monoclonal antibodies, and naturally derived small molecules. I will present examples of these techniques applied to currently marketed products.

Speaker Bio:  Professor Warner is an analytical chemist with more than 300 refereed publications in a variety of journals relevant to his general area of research.  He has particular expertise in the area of fluorescence spectroscopy, where his research has focused for more than 35 years. He is considered one of the world’s experts in this analytical spectroscopy. For example, he is the corresponding author in the highly cited biannual reviews on “Molecular Fluorescence, Phosphorescence, and Chemiluminescence Spectrometry“, for the journal, Analytical Chemistry.  Over the past 20 years, he has also maintained a strong research effort in the areas of organized media and separation science. Professor Warner has been performing research in the more specific area of analytical measurements using ionic liquids (ILs) for several years. It is this research on ionic liquids which has lead to the recent conceptualization and implementation of a group of uniform materials based on organic salts (GUMBOS) as novel materials which can be exploited for a variety of applications. Novel nanoparticles (nanoGUMBOS) have been derived from these materials which can primarily be classified as frozen ILs.  However, some GUMBOS are not ionic liquids since they do not fit the traditional definition of ILs. The utility of these materials is that they provide solid phase materials with the same tunability of ionic liquids.  Several publications in key chemistry journals (e.g. JACS, Nano Letters, ACS Nano, Analytical Chemistry, Chemical Communications, and Langmuir) and pending patents have resulted from this new area of research.
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November Meeting
Wednesday, November 13, 2013
6:00 pm - 8:00 pm
U.S. Pharmacopeia

Speaker:  Tony Brand, Ph.D., Agilent Technologies
Title:  Do we really know what the left and right are up to? Supercritical Fluid Chromatography is now the tool to tell, with some help from an MS

Abstract:   Chiral drugs are important in medicine and SFC has earned its place as a preferred chromatographic analysis tool for separating enantiomers, etc.  With the new generation of instruments, SFC is now poised to take a bigger role in the laboratory.  This talk will introduce the basic theory of SFC and contrast its application to reverse phase and normal phase LC and GC.  A number of re-discovered SFC and SFC/MS applications will be discussed, highlighting the advantages of using liquid carbon dioxide as a chromatographic solvent.

Speaker Bio:  Dr. Tony Brand obtained his Ph.D. in Physical Organic Chemistry at the University of California.  He came to HP/Agilent in 1994 and hasn’t left yet.  Tony started as a LIMS specialist, then joined the newly formed LC/MS team in 1997.  More recently, he has been working on ultra-high throughput LC and LC/MS applications as well as process automation, as well as being a leader in the SFC team.
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October Meeting
Wednesday, October 23, 2013
6:00 pm - 8:00 pm
U.S. Pharmacopeia

Speaker:  Benjamin Place, Ph.D., NIST
Title:  Multi-Dimensional Chromatography as a Quantitative Tool

Abstract:   Comprehensive, two-dimensional liquid chromatography (LCxLC) and gas chromatography (GCxGC) are emerging techniques that increase the chromatographic peak capacity of a single analytical run through the use of orthogonal separation mechanisms. These techniques are excellent for the separation of species of interest from other compounds (e.g., isomeric separation and/or sample matrix interferences). Early studies with both GCxGC and LCxLC have mainly focused on qualitative efforts, such as increasing peak capacity. Quantitative efforts have been made with both techniques, although the methods are less developed due to a lack of data processing tools. This presentation will focus on the efforts at the National Institute of Standards and Technology (NIST) to better understand GCxGC-TOF-MS and LCxLC-UV/Vis analyses, as well as determine the quantitative performance of these tools. Quantitative analysis by LCxLC-UV/Vis is still in its infant stage and multiple studies were performed to understand the data-processing. A program was developed in-house using R statistical software, an open-source program, for the transparent examination of various peak description and integration approaches and its impact on the quantitative performance of LCxLC-UV/Vis determination of four polycyclic aromatic hydrocarbons (PAHs). Also, various commercially-available software programs were evaluated for quantitative performance by the same LCxLC-UV/Vis analysis. Quantitative GCxGC-TOF-MS analysis has been much more rigorously studied, although analytical method development for specific analytes is still being studied. At NIST, multiple analytical methods were developed for GCxGC-TOF-MS for the detection of PAHs in available NIST Standard Reference Materials (SRMs). The quantitative performance of these GCxGC methods will be presented, along with future goals of NIST multidimensional chromatography program.

Speaker Bio:  Dr. Benjamin Place is currently an NRC Postdoctoral Fellow at the National Institute of Standards and Technology (NIST) and has been working with his mentor Dr. Catherine Rimmer in the Chemical Sciences Division since October 2012. Ben received his B.S. in Chemistry from Alma College, Alma, MI in 2008 and his Ph.D. in Analytical Chemistry from Oregon State University while working with Dr. Jennifer Field developing analytical methods for the identification, detection, and quantification of emerging contaminants in environmentally-relevant matrices. His Ph.D. work covered a wide range of compounds, including carbon nanomaterials, per- and polyfluorinated surfactants, and oil dispersant surfactants. Ben’s NRC fellowship work at NIST is focused on the development of LCxLC-MS methods for the non-targeted screening of Standard Reference Materials (SRMs) for novel environmental compounds.
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Open House and Poster Session
Wednesday, September 18, 2013
6:00 pm - 8:00 pm
Bethesda North Marriott Hotel & Conference Center   
5701 Marinelli RdNorth Bethesda, MD 20852


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May Meeting
Wednesday, May 22, 2013
6:00 pm - 8:00 pm
U.S. Pharmacopeia

Speaker:  Dr. Christopher Okunji, USP
Title:  High Speed Counter-Current Chromatography: An Efficient Technique for Large-Scale Isolation of Pharmacopeia Reference Standards

Abstract:  High-speed counter-current chromatography (HSCCC) is an all-liquid chromatographic system that uses a support-free liquid stationary phase.  HSCCC is winning wide applications in the preparative separation of various natural and synthetic products.  Compared to preparative HPLC, HCCCC offers several advantages including significantly higher sample load requiring only cheap solvents instead of expensive solid phase columns for the separation.  Many medicinal plants have been studied and more than 1000 compounds have been successfully prepared by HSCCC for both commercial and research purposes.  HPLC purities of separated compounds are all above 90-98%.  The major classes of natural products that have been separated using HSCCC include alkaloids, flavonoids, phenolics, terpenoids, saponins, phenylpropanoids, quinones, stilbenes, sterols, peptides, anthraquinones and organic acids.  Among these constituents the more noteworthy representatives of dietary supplement reference standards are tanshinones from Salvia miltiorrhiza, monoterpene glycosides (Rosavin) from Rhodiola rosea, cichoric acid from Echinacea purpurea root, ganoderic acids from Ganoderma lucidum fungus, ginsenosides from ginseng, capsaicin and dihydrocapsaicin from Capsicum frutescens, bilobalide and ginkgolides from Ginkgo biloba leaves, lycopene from crude extract of tomato paste, etc.  Recent advances in instrument development as well as application of this technique to scale-up isolation of USP reference standards will be discussed.  The strengths and versatility of HSCCC separations and their ability to increase resolution and throughput and overcome traditional drawbacks of adsorption chromatography will be highlighted.
Speaker Bio: Dr. Chris Okunji is a Scientific Liaison for the Dietary Supplements group at United States Pharmacopeia (USP), Headquarter, Rockville MD., responsible for Dietary Supplement General Chapters and works closely with the USP Dietary Supplements and General Chapters Expert Committee’s where appropriate. Before joining USP in 2011, Dr.Okunji has been an NIH Special Volunteer working with countercurrent chromatography (CCC) to isolate large quantities of natural product constituents, Scientific Review Administrator NIAID-NIH (Contractor) and Senior Research Associate at Walter Reed Army Institute of Research (WRAIR) all in Maryland.  Dr.Okunji's teaching and research experience in the field of natural products/pharmacognosy includes scale-up isolation of natural product compounds using CCC, screening  African medicinal plants for  biological activities such as antimalarial, antileishmanial, antifungal, anticancer, antimicrobial, antitrypanosomiasis and antitrichomonas and Anti-HIV. Dr. Okunji also has Dietary Supplement manufacturing experience and a former Associate Professor of Pharmacognosy, University of Nigeria.  Dr. Okunji holds a M.Sc. and Ph.D. degrees in Pharmacognosy from University of Nigeria. He has more than 30 years of experience in academic, industrial and government settings. Dr. Okunji is a recipient of U.S. National Research Council Fellowship in 1993.
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April Meeting
Monday, April 15, 2013
Co-sponsored with the Washington-Baltimore Mass Spectrometry Discussion Group
6:00 pm - 8:15 pm (Speaker at 7:15 pm)
Shimadzu Training Center

Speaker:  Dr. Michael Boyne, FDA
Title: Modern Analytics for the Analysis of Complex Drug Products:  Physicochemical Characterization using MS

Abstract: Modern analytical methods continue to improve the ability of analysts to sensitively identify and quantify the structure and composition of complex drugs. The increased information content these technologies provide increases the level of assurance of these products' quality. For this reason, the FDA has investigated the use of information rich analytical techniques to assess the quality of complex drug products including therapeutic proteins, monoclonal antibodies, and naturally derived small molecules. I will present examples of these techniques applied to currently marketed products.
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February Meeting
Wednesday, February 20, 2013
6:00 pm - 8:00 pm
U.S. Pharmacopeia

Speaker:  Andrew Alpert, PolyLC
Title: Advantages of HILIC and ERLIC for Proteomics

Abstract:  Hydrophilic interaction chromatography (HILIC) can accomplish some separations that are not easy or possible with alternative modes:
Top-down proteomics:  If a set of proteins can be maintained in the predominantly organic solutions, then top-down analysis of intact proteins can be done with volatile solvents.  This then permits their separation on the basis of differences as minor as a single carbohydrate residue.
Bottom-up proteomics: A HILIC-RP sequence compares favorably with the widely-used SCX-RP sequence for fractionation of complex tryptic digests.  The new ERLIC mode (electrostatic repulsion-hydrophilic interaction chromatography) is even better.  Using volatile solvents, an ERLIC-RP sequence identifies 30-40% more peptides and proteins than does a SCX-RP sequence, with appreciably less effort.  ERLIC separates tryptic peptides in order of decreasing pI value, without ampholines.  ERLIC also affords selective isolation and separation of phosphopeptides and glycopeptides from unmodified peptides.   Finally, a RP-ERLIC sequence permits the identification of proteins that were deamidated in vivo.  This may be a new mechanism for biological control.  The motifs for sites susceptible to deamidation of asparagine matched those in the literature, but sites for deamidation of glutamine were quite different.

Speaker Bio: Andrew Alpert received his B.S. degree in chemistry from Yale College in 1973 and a M.S. in biochemistry from the University of Nebraska Medical Center.  His Ph.D. work was with Fred Regnier at Purdue University, developing the first HPLC packing materials and techniques for protein applications.  Following two post-doctoral fellowships at Baylor College of Medicine (Arthur Beaudet’s group and H. F. Gilbert’s group), he started PolyLC in 1985.  The company manufactures chromatography columns and materials for difficult protein and peptide separations.  Dr. Alpert introduced the technique of Hydrophilic Interaction Chromatography (HILIC) in 1990.  Current interests include:  1) Development of techniques for analysis of particularly difficult proteins, including histone variants and proteomics analysis of both membrane and nonmembrane proteins; 2) Mixed-bed ion-exchange columns for proteins; 3) Multidimensional fractionation of peptides for proteomics applications (e.g., the SCX-RP sequence); 4) HILIC of solutes on columns of the same charge (a variant called ERLIC), which permits isocratic separations of solutes differing greatly in composition such as amino acids and nucleotides.  It also affords selective isolation and resolution of phosphopeptides, glycopeptides, and deamidated peptides for proteomics analyses.
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January Meeting
Wednesday, January 16, 2013
6:00 pm - 8:00 pm
U.S. Pharmacopeia

Speaker:  Kevin Siek, LECO Corporation
Title: "Sharpening Chromatographic and Spectral Resolution to Reveal More in Metabolomic, Food Safety, Environmental, and Pharmaceutical Sciences"

Abstract: The analysis of complex mixtures and characterization of the analytes therein is of fundamental significance to numerous disciplines of study. In modern analytical sciences this requires separation followed by analysis using a diagnostic spectroscopic technique. This is most often achieved using liquid chromatography or gas chromatography interfaced to mass spectrometry. The degree of separation required is related inversely to the “power” (resolution and mass accuracy) of the mass spectrometric technique. An ultra-high resolution mass spectrometer (R > 25,000) requires less chromatographic resolution than a unit mass system and a high capacity (resolution) separation (two dimensional gas chromatography or capillary electrophoresis) does not necessarily require an ultra-high resolution mass spectrometer. In this presentation, examples are provided from numerous fields of analytical study including metabolomics, environmental sciences and food safety, and petroleum analysis which demonstrate utility of high mass resolving power, as well as the utility of GCxGC separation to achieve analyte identification by separation from interfering substances. The capability of ultra high performance mass spectrometry using comprehensive time of flight to provide high-confidence formula and structural identification is leveraged in a variety of matrices and to address numerous analytical issues. Mass resolving powers at 25000 or 50000 or higher and mass errors of approx. 1 ppm provide confident identifications and selective detection. Two dimensional GC in combination with library-searchable EI spectra provide an ability to complement what is detected using the high performance MS analyses.

Speaker Bio: Kevin Siek is the Technical Product Specialist for High Resolution TOFMS Technology for LECO Corporation, a position he has held for three years.  Prior to his position at LECO, Kevin was in pharmaceutical research and development at Sanofi-Aventis for about fifteen years, where he gained experience in molecular characterization, quantitative method development for putatively genotoxic impurities and other assays, metabolite identification, finished product characterization, and other duties as needed, including but not limited to improvisatorial plumbing and sweeping up much shattered glassware.  His greatest single accomplishment has been persuading his wife to stay married to him through all this.  Anyone living with someone who finds chemistry jokes funny deserves admiration.  Kevin received his BS in Chemistry from Valparaiso Univeristy.
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December Meeting
Wednesday, December 12, 2012
6:00 pm - 8:00 pm
U.S. Pharmacopeia

Speaker:  Jeff Rohrer, Ph.D., Director, Applications Development, Dionex Products, Thermo Fisher Scientific
Title: Ion Chromatography for Pharmaceuticals

Abstract:  The last decade has witnessed a significant increase in the number of ion chromatography (IC) based methods in the United States Pharmacopeia National Formulary (USP-NF).  The methods include assays of drug substances and drug products, and the determination of related substances and impurities in drug substances and drug products.  IC is also commonly used in the pharmaceutical industry to assay for excipients and active pharmaceutical ingredient (API) counterions.  Compared to reversed-phase HPLC, IC offers a different and often superior approach to determining ionic compounds, especially those lacking a strong chromophore.  Most IC assays feature an ion-exchange separation followed by suppressed conductivity detection, but there are IC methods for pharmaceuticals that use other detection techniques.  This talk will review the general principles of IC including separation and detection strategies, as well as briefly discuss newer develops including capillary IC and the charge detector.  The majority of the presentation will describe the development of IC assays for drug substances and products, related substances and impurities in drug substances and products, and API counterions.  The assays presented will demonstrate the different IC separation and detection strategies that can be employed to meet the specificity and sensitivity needs of the application.

Speaker Bio:   Dr. Jeffrey S. Rohrer is the Director of Applications Development, Dionex Products for Thermo Fisher Scientific.  In this position he directs the work of three corporate applications laboratories in California, China, and Thailand.  These labs develop HPLC, IC, HPAE-PAD, and other LC-based assays.  Dr. Rohrer is an author of over 50 peer-reviewed publications and is a member of the United States Pharmacopeia (USP) Expert Committee on Monograph Development for Small Molecules #1, a member of the USP Expert Panel on Glycoprotein and Glycan Analysis, and a member of the USP Expert Panel on Modernization of Identification Tests.  Between 2005 and 2010 he was a member of the USP Expert Committee for Antibiotics Monograph Development.  He is also the coeditor or a recently published book: Applications of Ion Chromatography for Pharmaceutical and Biological Products (Wiley).  Dr. Rohrer joined Thermo Fisher (then Dionex) in 1989 and has held positions that include, Marketing Field Chemist, Senior Biochemist in R&D, Sales Support Manager, and Applications Lab Manager.  Prior to joining Thermo Fisher Scientific he spent two years as a post-doctoral associate in Dr. Elizabeth Theil's lab at North Carolina State University studying the mechanism of iron deposition into the protein ferritin.  Jeff received his BS in Chemistry from Franklin and Marshall College in 1981 and his Ph.D. in Chemistry from the University of Delaware working with Dr. Harold White III studying the role of glycosylation in the transport of chicken serum riboflavin-binding protein across the oocyte membrane.
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November Meeting
Tuesday, November 13, 2012
6:00 pm - 8:00 pm
U.S. Pharmacopeia

Speaker: Len Sidisky, R&D Manager, Gas Separations, Supelco
Title: Advances in Ionic Liquid Stationary Phases for Capillary Gas Chromatography

Abstract: Ionic liquids have received considerable interest as new green solvent systems in the areas of organic reactions and separation technologies along with a number of other areas. These materials are a class of non-molecular solvents that consist of essentially organic cations and anions. They have been found to possess negligible volatility, non-flammability, high thermal stability, and low melting points. There are numerous combinations of cations and anions possible, so tailoring the material to a specific application or function is a potential benefit of these materials.
Recently, a series of geminal dicationic and polyionic ionic liquids have been prepared for use as stationary phases in capillary gas chromatography. These materials are known to provide higher thermal stability for gas chromatography, broader liquid working ranges and broader selectivity ranges than monocationic ionic liquids. This study will examine the selectivity of newly developed ionic liquid phases along with comparing their thermal stability and durability. A variety of Petrochemical, Food & Beverage and Environmental samples will be evaluated for the comparisons.

Speaker Bio: Leonard M. Sidisky is Research & Development Manager for Gas Separations at Supelco, Division of Sigma-Aldrich. He received his B.S. degree in Biology (1980) and an M.S. in Food Science (1997) from The Pennsylvania State University. He has been working at Supelco since 1982 and is responsible for the research and development of new novel technologies related to gas chromatography, sample preparation, air sampling, solid phase microextraction and high performance carbon adsorbents. His analytical background includes expertise in Gas Chromatography, Liquid Chromatography, Sample Preparation devices such as Solid Phase Extraction (SPE), and Solid Phase Microextraction (SPME). He is a member of the American Oil Chemist’s Society (AOCS), AOCS Analytical Division, AOCS Northeast Section, AOCS Chromatography Committee Chairperson 2000-2009, AOCS Governing Board Technical Steering Committee Chairperson 2010-present, AOCS Northeast Section president 2000-2001, vice president 1998-1999, Hans Kaunitz Award Chairman 2000-2001, Supelco/Nicholas Pelick AOCS Lipid Award Representative 1994-present, 1992 Ralph H. Potts Memorial Fellowship Award Winner. He is also a member of the Institute of Food Technologists (IFT) professional member 1992-present, American Chemical Society (ACS) member 1982-present; ASTM D16 (Aromatic Hydrocarbons) 1990-present, D16.OE.09 Task Group (Capillary Applications) chairman 1995-present and ASTM E13 Committee His research interests are in the development of Gas Chromatographic products for wide range of industrial applications, capillary columns for lipid sample analyses,  theory and practical application of Capillary Gas Chromatography and Solid Phase Micro Extraction (SPME) product development and applications. He has presented numerous papers and seminars worldwide and has published over 25 journals articles.
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October Meeting

Thursday, October 11, 2012
Chemical Society of Washington Dinner Meeting
6:00 pm - 9:00 pm
Far East Restaurant, Rockville, MD
6:00 pm - Social Hour and Poster Session by Project SEED Students
7:00 pm - Dinner
8:00 pm - Speaker Presentation
 
Speaker: Jessica Reiner, Ph.D., National Institute of Standards and Technology
Title: Temporal and Spatial Trends of Current-use and Legacy Persistent Organic Pollutants in Marine Mammals

Abstract: The Arctic is considered a major sink for persistent organic pollutants (POPs) that are capable of long range atmospheric or oceanic transport.  Once in the arctic biosphere, cold temperatures reduce their degradation and facilitate transport from air to water, enhancing bioconcentration into aquatic food webs.   Consequently there have been numerous studies assessing time and location trends of POPs in arctic regions including regions in Canada, Greenland, and northern Europe.  There are comparatively fewer time trend descriptions of POPs in arctic fauna from other locations particularly from the northern Bering Sea and Chukchi Sea regions of the Arctic.
The Alaska Marine Mammal Tissue Archival Project (AMMTAP) was established in 1987 through an agreement between the National Oceanic and Atmospheric Administration (NOAA), the National Institute of Standards and Technology (NIST), and the Minerals Management Service (MMS) to help determine contaminant levels in marine mammal samples that were taken primarily during native subsistence hunts in Alaska. Tissues were collected and banked at the National Marine Mammal Tissue Bank (NMMTB) for long-term archival using NIST standardized protocols. Archived samples from the NMMTB were provided for this retrospective analysis of contaminants.
From 1989 to 2006 liver (n=68) and blubber samples (n=72) were collected from beluga whales (Delphinapterus leucas) from both the Cook Inlet and the eastern Chukchi Sea beluga whale stocks and analyzed for a variety of current-use and legacy POPs, in order to provide more information on the status of POPs in the Alaskan region.  From 1987 to 2007, liver (n=49) and blubber samples (n=50) were collected from northern fur seals (Callorhinus ursinus) from St. Paul Island in the Bering Sea and analyzed for the POPs.  This presentation will discuss measurements of POPs from these two arctic species and demonstrate the importance of a long term archival program as a source of samples for monitoring time trends.

Speaker Bio: Dr. Jessica Reiner received a B.S. degree in Chemistry and Chemical Oceanography at the University of Rhode Island in 2001 and a Ph.D. degree in Environmental Chemistry at University at Albany, State University of New York in 2007. Dr. Reiner’s research interests are focused in the area of chemicals of emerging concern in environmental and human samples. She has worked in determining contaminant concentrations in sediment, water, food, biota, and humans, as well as establishing baseline information on potential exposure pathways. Presently, her research goals are to improve analytical measurements of chemicals of emerging concern, mainly perfluorinated alky acids, through the certification of reference materials, methods development, and other quality assurance activities. She has worked as part of the NIST staff at the Hollings Marine Laboratory in Charleston, SC; a multidisciplinary research location that focuses on solving marine and human health problems. She has authored and co-authored several peer-reviewed publications and presented at many national and international conferences.
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Open House & Poster Session
Wednesday, September 12, 2012
Click here to download a PDF of the program.
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May Meeting

Wednesday, May 16, 2012
6:00 pm - 8:00 pm
US Pharmacopeia, Rockville, MD
Speaker: Pierluigi DelMonte, Ph.D., Office of Regulatory Science Center for Food Safety and Applied Nutrition, FDA
Title: Investigation of comprehensive LCxLC for the separation of phytochemicals in dietary supplements

Abstract:  Botanical dietary supplements are most often complex mixtures of phytochemicals characterized by markedly different chemical properties. Often a single dimension liquid chromatographic separation does not provide the theoretical plates or the selectivity needed for the separation of such complex mixtures. While reversed phase chromatography (RP) is the most widely applied approach for the separation of phytochemicals, normal phase and HILIC chromatography are often used to separate compounds containing sugar moieties. The combination of these separation mechanisms in a comprehensive LCxLC system using a HILIC column for the first dimension separation (D1) and an RP column for the second dimension (D2) proved to be a suitable platform for the separation of phytochemicals in dietary supplements.
Comprehensive LCxLC was tested for the separation of the polyphenolic compounds and steviol glycosides in extracts of Stevia rebaudiana. The tested platform consisted of a capillary WAX column for D1 separation and a C18 UHPLC column (2.1 mm x 30 mm, 1.8 micron) maintained at 60 °C for the D2 separation, with a modulation time of 15 sec.

Speaker Bio:  Pierluigi Delmonte received his Master Degree in Chemistry from the University of Parma (Parma, Italy) in 1996 and the Doctorate Degree in Food Biotechnology from the University of Bologna (Bologna, Italy) in 2001.  His Ph.D. research focused on the analysis of conjugated linoleic acid (CLA) in dairy products. In 2001, Dr. Delmonte joined the Center for Food Safety and Applied Nutrition of the U.S. Food and Drug Administration. His research focuses primarily on the development of HPLC and gas chromatography methods for the analysis of CLA and trans fatty acids in foods, and of active components in dietary supplements.
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April Meeting

Wednesday, April 18, 2012
6:00 pm - 8:00 pm
US Pharmacopeia, Rockville, MD

Speaker: Mark Lowenthal, Ph.D., National Institute of Standards and Technology
Title: Developing LC-MS methods for qualitative characterization of NIST Standard Reference Materials

Abstract:  Standard Reference Materials (SRMs) offer the scientific community a stable source of biomaterials boasting broad application possibilities.  Traditionally, SRMs provide quantitative information for only a few targeted analytes in buffered solutions, or complex matrices.  Current efforts attempt to broaden the scope of how and what information is offered to the SRM community by providing qualitative information about biomaterials, such as chromatographic profiles and untargeted identifications.  In order to more fully characterize these biomaterials, metabolomic and proteomic profiles were applied to a suite of Vaccinium berry dietary supplement SRMs.  An unbounded set of qualitative data about a biomaterial is a valuable resource intended to complement quantitative information traditionally provided in NIST Certificates of Analysis. Metabolites and proteins were separately enriched from a suite of Vaccinium-based biomaterials.  Untargeted metabolite discovery was performed using mass spectral matching of tandem MS data to the NIST MS/MS library.  Validation of metabolite IDs was achieved using multiple reaction monitoring MS analysis on a triple quadrupole MS with authentic standards.  The use of prior probabilities for metabolite identification is discussed.  Proteins were analyzed using typical bottom-up proteomics approaches. A protein database was created from Vaccinium and citrus-based expressed sequence tags (ESTs) and used for novel protein identifications. Definitive IDs are reported for metabolites and novel protein identifications.  Over 50 putative identifications were determined among the biomaterials based on reporting guidelines set forth by the Metabolomics Standards Initiative.  A large subset of identifications consisted of anthocyanins, organic acids, flavan-3-ols, and other flavanoids typically found from fruit extracts.  Chromatographic profiling of these berry materials will provide valuable qualitative information for users of an SRM material.  Using MS library matching to discriminate biomolecules or biomolecular classes in complex materials is discussed in regards to the structural similarity among many small organic molecules.

Speaker Bio:  Mark Lowenthal is a research chemist at the National Institute of Standards and Technology in the Material Measurement Lab (Analytical Chemistry Division).  He has been at NIST for over four years working on qualitative and quantitative measurements of metabolites and proteins in biomaterials and SRMs.  Prior to joining NIST, Mark worked on molecular profiles of cellular lipid droplets at the University of Colorado Health Sciences Center, and for three years in a proteomics lab at NIH (NCI).  Mark got a PhD from the University of Maryland in Analytical Chemistry.  
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March Meeting

Wednesday, March 21, 2012
6:00 pm - 8:00 pm
US Pharmacopeia, Rockville, MD
Speaker: John Van Antwerp, Waters Corporation
Title: Fundamentals and Advancements in Analytical SFC

Abstract:  In the past decade, Supercritical Fluid Chromatography (SFC) has demonstrated great promise as the choice of chromatography for chiral compounds, and as a general replacement technique for normal phase liquid chromatography (NPLC).  Compared to traditional normal phase HPLC, SFC is on average 3 to 10 times faster.  Using inexpensive CO2 and a polar modifier such as methanol, SFC is more cost-effective and environmentally friendly by reducing the consumption and disposal of organic solvents.  Widespread adoption of analytical SFC has been hampered by instrumentation which does not perform to the standards established by modern HPLC systems.  Poor signal to noise ratio, poor retention time and injector reproducibility, and overall lower reliability, as compared to HPLC, are often described as major limitations. In order to bring this separation technique to a performance level desired by today’s modern laboratory, a holistic system must be designed from the ground up.  The majority of system components of an analytical SFC system are the same as any LC system, pump, autosampler, detector, software solutions, along with some components unique to SFC.  Although similar to LC, the design challenges for each component must be considered and each component must be designed so that the system as a whole performs at a high level.  We present here some of the design challenges along with their solutions and a basic evaluation of instrument performance, at a system level.  This talk will describe the advances made to the hardware and chemistries and will have examples of increases in efficiencies and throughput as well as return on investment.

Speaker Bio:  John Van Antwerp is the Waters Corporation Americas Business Manager for quadrupole MS products and SFC/SFE.  He has been at Waters for 24 years in various roles from regional technical support up through his current role as business manager.  Over the past 15 years he has been involved in new technologies at waters including LC/MS, SFC, SFE and SFC/MS.  Prior to joining Waters , John spent 15 years developing analytical HPLC methods for a major Pharmaceutical Company.
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February Meeting
Wednesday, February 15, 2012
6:00 pm - 8:00 pm
US Pharmacopeia, Rockville, MD

Speaker: Rick Lake and Ty Kahler, Restek Corporation
Title: Characterizing Stationary Phase Selectivity - A Practical Look at Column Selection

Abstract:  In this presentation, we will review the popular Hydrophobic Subtraction Model and present an extended characterization for modern non-alkyl phases.  We will then discuss the dominant reversed phase separation mechanisms involved with common stationary phase types.  Lastly, we will provide a practical approach to stationary phase selection, including a brief discussion on applying scouting gradients.

Speaker Bios:  As a Product Line Manager, Rick Lake oversees the development and application of Restek’s LC products.  He previously served as our Pharmaceutical Market Development Manager and Pharmaceutical Innovations Chemist, developing GC and LC applications and assisting in new product development. Before coming on board in 2005, he worked for 7 years as a study director and principal investigator for a contract research lab, where he developed and validated GC and LC methods while also managing the stability testing department. Prior to shifting his focus to pharmaceuticals, he spent 4 years performing pesticide residue and volatile/semivolatile analysis.
Ty Kahler joined Restek as a Senior Innovations Chemist in 2008 where his responsibilities include liquid chromatographic methods development, standard methods testing, and phase design/research.  Prior to joining Restek, he worked as a manager, study director, and principal investigator for a contract pharmaceutical research laboratory conducting method development, validation, and analysis of pre-clinical and clinical pharmaceuticals.  He has been in the fields of pharmaceuticals and liquid chromatography development and analysis for over 14 years, including time as a quality chemist and instrumentation metrologist.  In addition to time spent in the pharmaceutical industry, he has worked as the lead chemist on studies involving agrochemicals and pesticide manufacturing.
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January Meeting
Wednesday, January 18, 2012
6:00 pm - 8:00 pm
US Pharmacopeia, Rockville, MD

Speaker: Ruin Moaddel, Ph.D., National Institute on Aging, National Institutes of Health
Title: Bioaffinity Chromatography:  The Study of Drug-Protein and Protein-Protein Interactions

Abstract: Protein-based liquid chromatography stationary phases are used in bioaffinity chromatography for studying drug-protein interactions including the determination of binding affinities and competitive and allosteric interactions, as well as for studying protein-protein interactions.  The development and characterization of protein-based stationary phase, and the application of these phases using frontal and zonal chromatography techniques will be discussed. More recently, the use of the protein-coated magnetic beads for ligand and protein fishing has also been carried out, demonstrating the versatility of protein-based stationary phases for the identification of unknown ligands from cellular or botanical extracts.

Speaker Bio:  Ruin Moaddel earned his Ph.D. from Northeastern University in 1999, followed by post-doctoral studies at Georgetown University.  He is currently a Staff Scientist at the National Institute on Aging, NIH.  Currently at the NIA, Ruin’s main research interests are in the creation of cellular membrane affinity chromatography columns on multiple formats and their use in online drug screening in complex matrices and ligand binding studies for multiple proteins.  This is carried out by frontal affinity chromatography, non-linear chromatography, missing peak chromatography and/or ligand fishing in complex matrices.
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November Meeting
Wednesday, November 16, 2011
6:00 pm - 8:00 pm
Shimadzu Scientific Instruments, Inc. Training Center
7100 Riverwood Drive, Columbia, MD 21046
 
Speaker: Cynthia Tyburczy, Ph.D., FDA-CFSAN
Title: Covalent Adduct Chemical Ionization Mass Spectrometry for the Identification of Fatty Acid Methyl Ester Double Bond Configuration

Abstract: Covalent adduct chemical ionization (CACI) mass spectrometry (MS) was developed as a convenient and rapid tool for the unequivocal identification of double bond configuration in most fatty acid methyl esters (FAME).  Acetonitrile maintained under CI conditions yields ions at m/z 40 and 42, and an ion at m/z 54 which was identified as 1-methyleneimino-1-ethenylium, the decomposition product of the reaction of acetonitrile with itself.  The m/z 54 ion selectively reacts with the double bonds of FAME, resulting in predictable fragmentation about the double bonds.  Single-stage CACI-MS provides structural information related to FAME chain length, degree of unsaturation and, in some cases, double bond geometry.  In CACI MS/MS, fragmentation of the preselected parent ions yields a small number of predictable peaks that are indicative of FAME double bond location.  Key practical advantages of CACI MS and MS/MS over re-derivatization methods involving 4,4 dimethyloxazoline (DMOX) or picolinyl esters include the fact that FAME are analyzed directly with no additional chemical treatment and that similar gas chromatography (GC) conditions (column, temperature program, sample concentration) are used, thus enabling direct comparisons between GC and GC-MS chromatograms.  This method is applicable to the identification of homoallylic and conjugated linoleic acid FAME and to the quantitation of cis and trans monoenoic FAME through selected ion monitoring.  In recent years, CACI-MS and MS/MS have been used for the identification of unique partially conjugated and non methylene interrupted polyenoic FAME.

Speaker Bio: Cynthia Tyburczy earned her B.S. (2006) and M.S. (2008) degrees in Animal Science from Cornell University working with Dr. Dale E. Bauman. Her M.S. research focused on the biological activity of individual trans 18:1 fatty acids with regard to milk fat synthesis and as biomarkers for coronary heart disease risk. She earned her Ph.D. (2011) in Molecular Nutrition from the Division of Nutritional Sciences at Cornell University working with Dr. J. Thomas Brenna. Cynthia’s Ph.D. research focused on the effect of dietary arachidonic acid level and source on neonatal piglet development. She joined the U.S. Food and Drug Administration’s Center for Food Safety and Applied Nutrition in April 2011 as a postdoctoral research fellow. She currently investigates gas chromatography and infrared spectroscopy methods for quantifying trans fat in food.
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Open House & Poster Session

Wednesday, September 28, 2011
Click here for a copy of the program