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LeClaire-Dow Instrumentation Facility critical to researchers

Nestled on the first floor of Kolthoff Hall is one of the most sophisticated, specialized instrumentation facilities on the University of Minnesota campus.

The LeClaire-Dow Instrumentation Facility houses the Mass Spectrometry Laboratory (MSL), the Nuclear Magnetic Resonance (NMR) laboratory, and the X-Ray Crystallographic Laboratory (XCL). These laboratories annually support hundreds of researchers in the Department of Chemistry, across the university, and from other institutions and industries. Most of the equipment is state-of-the-art and some recent infrastructure grants will replace aging equipment.

Each of these facilities are directed by highly trained, doctorate-holding chemists who are specialists in their fields. Joseph Dalluge is director of the MSL, Letitia Yao is director of the NMR lab, and Victor Young Jr. is director of the XCL.

Mass Spectrometry Laboratory
The Mass Spectrometry Laboratory is highly used by faculty and student researchers at the university and from other colleges and universities, and by industrial researchers. Forty Department of Chemistry faculty members and their research groups use the facility, and 50 researchers from other departments such as Biochemistry, Molecular Biology and Biophysics, Food Science and Nutrition, Biomedical Engineering, Chemical Engineering & Materials Science, Medicinal Chemistry, Pharmaceutics, and Veterinary Medicine, and the Medical School employ the facility for analysis or research collaboration.

Working with Dalluge, these research collaborations have resulted in eight peer-reviewed articles published the past year. In addition, more than 20 industrial clients use the instrumentation.

Since Dalluge started with the department in 2009, he has expanded the breadth of equipment and services provided by the MSL, making it one of the premier facilities of its kind in the country. Its capabilities range from classical chemical characterization techniques to leading edge MS and 2D imaging and advanced metabolite profiling.  

The recent acquisition of two mass spectrometers was made possible through grants awarded in 2013. The first is an Applied Biosystems-Sciex 5800 MALDI-TOF/TOF mass spectrometer funded by a National Science Foundation Major Research Instrumentation grant awarded to Professor Michael Bowser, principal investigator, and Dalluge, co-principal investigator. MALDI-MS is a powerful tool for analyzing a variety of different analytes including small molecules (metabolites), lipids, nucleic acids, peptides, proteins, and polymers. The second is a Fluidigm CyTOF2 Mass Cytometer funded through a University of Minnesota Office of the Vice President for Research Infrastructure Grant awarded to Professor Edgar Arriaga, principal investigator. Mass cytometry combines the advantages of single cell high speed analysis common to conventional flow cytometry with the ability to resolve more than 100 metal probes with minimal signal overlap common to atomic mass spectroscopy. This provides researchers with an unparalleled ability to phenotypically and functionally profile cells from normal and disease states.

Nuclear Magnetic Resonance Laboratory
For Yao, NMR spectroscopy is an invaluable tool for researchers who make or structurally characterize new organic, organometallic, medicinal, and polymeric compounds. Essential to the productivity of these researchers is modern, sophisticated instrumentation capable of providing high quality data in a user-friendly, walk-up or open-access environment, which is offered in her laboratory.

Approximately 300 researchers from 42 different research groups on campus, spanning 10 different departments, including Chemistry, Chemical Engineering and Materials Science, the Masonic Cancer Center, Medicinal Chemistry, and Bioproducts and Biosystems Engineering, are trained operators of the spectrometers in the NMR laboratory. Together, they collect more than 40,000 spectra annually. These instruments also service the needs of about a dozen industrial clients, several local colleges and community colleges, and the Department of Chemistry’s undergraduate teaching mission. A critical distinction of the Department of Chemistry’s laboratory is the diversity of experiments required by its users. Thousands of new compounds are produced at the University of Minnesota each year.

“Letitia Yao is the person that I absolutely admire for her outstanding NMR service and attentive help at all times,” wrote Son Nguyen in his student dissertation, Synthesis of the ABCD and FGHI Domains of Azaspiracid.

The NMR laboratory houses three vintage Varian spectrometers at 300 MHz and 500 MHz, which were acquired in the late 1980s, and two modern 500 MHz spectrometers, which were acquired in the 2010s. One of the Bruker 500 MHz instruments, which sits on a vibration isolation table, was purchased by the university so at least one spectrometer is protected from the vibrations and electromagnetic interference generated by the nearby light rail trains. The second Bruker 500 MHz instrument was purchased with a National Institutes of Health instrumentation grant with matched funding from the university and Department of Chemistry. Professor William Pomerantz contributed a portion of his start-up funds to equip one of the Brukers with a liquid-nitrogen cooled Prodigy cryoprobe with enhanced sensitivity for F19 nuclei (and H1 and C13).

The NMR laboratory was recently awarded a $329,600 Research Infrastructure Reinvestment Program grant from the Office of the Vice President for Research, which will be matched with funds from the College of Science & Engineering and the Department of Chemistry. This will enable the laboratory to purchase two new 400 MHz spectrometers to replace the vintage ones, which require frequent repairs, once they reach the end of their useful lifetimes. The new machines also will lower the use of non-renewable consumables like liquid helium, and will be fully shielded from vibrations and electronic fields generated by the light rail line.

X-Ray Crystallographic Laboratory
The X-Ray Crystallographic Facility is nationally recognized, providing its users with a variety of crystallographic instrumentation, expertise in crystallographic techniques, computers, and crystallographic software. The mission of this facility it to provide the best molecular structure elucidation services to University of Minnesota researchers and collaborators at other institutions and industries. While the laboratory primarily offers single crystal diffraction services, expertise in most areas of crystallography is available.

About 300 projects were studied in 2013, and most of those provided researchers with publication-ready crystallographic results.

Frequently, the research projects present obstacles that require expertise and innovation to overcome such as twinning, small crystal sizes, or solvent loss, said Young. “For instance, our laboratory is recognized as being expert in the solution and refinement of non-merohedrally twinned materials,” he said.

In 2012, the XCL was awarded a National Science Foundation Major Research Instrumentation Grant to purchase a Bruker-AXS D8 Venture single crystal diffractometer with Cu-KαIμS microfocus source, PHOTON-100 CMOS detector, and an Oxford Cryostream 700-Plus Cryostat. This joined an existing Bruker-AXS APEX-II CCD diffractometer. Additional equipment includes two area-detector single-crystal instruments, plus access to the Cambridge Structural Database and the APEX-II software suite.

Since 1999, Young has taught the graduate course CHEM 5755, which blends a traditional theory curriculum with a laboratory experience where the students learn to operate modern single crystal diffractometers.

Joseph Dalluge, Ph.D.

Education: Doctorate in biochemistry from the University of Utah, bachelor’s degree from Gustavus Adolphus College
Post-Doctoral Research: National Research Council Post-Doctoral Associate, National Institute of Standards and Technology, Gaithersburg, MD
Employment: Research Chemist at the National Institute of Standards and Technology; Senior Chemist with Cargill Incorporated; Director of Department of Chemistry Mass Spectrometry Laboratory since 2009
Professional affiliations: Editorial Board, Current Protein and Peptide Science, American Chemical Society, American Society for Mass Spectrometry, Past-President and Board Member of the Minnesota Mass Spectrometry Discussion Group
Publications/Presentations/Patents: 37 publications, four abstracts, one patent, and seven invited presentations

Letitia Johnson Yao, Ph.D.
Education: Doctorate from the University of Minnesota, bachelor’s degree from the College of Wooster in Ohio
Post-Doctoral Research: University of California in San Francisco
Employment: Temporary Department of Chemistry faculty, and NMR Research Associate since 1997, and now Laboratory Director
Professional affiliations: American Chemical Society, Minnesota Section of the American Chemical Society, Association of Managers of Magnetic Resonance Laboratories, Sigma XI, Phi Beta Kappa, Graduate Women in Science, Department of Chemistry Women in Science & Engineering (WISE) team, Minnesota NMR Users Group, National Academy of Sciences Committee on Science, Engineering and Public Policy
Publications/Presentations/Patents: 18 publications, six presentations

Victor Young Jr., Ph.D.
Education: Doctorate from Arizona State University, bachelor’s degree from Spring Arbor College in Michigan
Post-Doctoral Research: Arizona State University
Employment: Development and Testing Engineer II for Chrysler Corporation; Visiting Scientist at the Los Alamos National Laboratory; Staff Crystallographer in the Department of Chemistry at Iowa State University; and Research Associate, Senior Research Associate and, since 1995, Director of the X-Ray Crystallographic Laboratory since 1995
Professional affiliations: American Crystallographic Association, and Neutron Scattering Society of America
Publications/Presentations/Patents: More than 40 presentations and 257 publications, workshops for local university and college faculty members and their students to introduce them to crystallographic theory and the modern instrumentation, and part of the Inter-national Year of Crystallography 2014 Task Force that is organizing numerous educational and outreach activities through this year of celebration.