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IU Northwest’s new 400Mhz superconducting NMR spectrometer enhances chemistry research and teaching

Powerful tool accelerates groundbreaking research and provides students with advanced experience

Wednesday Oct 25, 2017

As Jennifer Mishevich unlocks the door to Indiana University Northwest’s newest laboratory, the senior chemistry major is greeted with a blast of chilly air, an amenity meant for the well-being of the university’s powerful new 400 MHz research-grade NMR spectrometer.

Mishevich recently learned how to operate the powerful superconducting magnet, prepare it for experimentation, and analyze the samples she’s developing as a research assistant for Assistant Professor of Chemistry Tia Walker.

Zipping up her sweater, Mishevich prepares to fill the instrument with liquid nitrogen. The room temperature helps minimize cryogen loss; in addition to offsetting the heat generated by the magnet and two computer systems.

NMR stands for nuclear magnetic resonance. Most understand the technology as it is applied in the medical field. An MRI, or magnetic resonance imaging, is a diagnostic test that uses magnetism to create images from the resonance of the water in different tissues of the body.

The NMR works in much the same way, but with more power, and by looking at the hydrogen atoms on organic molecules. It is one of the most powerful tools that research chemists have for the characterization and identification of chemical compounds, including small molecules and peptides.

It enables researchers like Walker, and her colleague, Assistant Professor of Chemistry Ian Taschner, to move faster in their research because they can analyze their samples onsite, for immediate feedback.

For example, Walker, who last year received a prestigious National Institutes of Health (NIH) grant to pursue research that could have implications to treat multiple sclerosis, is working to derivatize the N2S2 ligand, a molecule she needs to produce in order to do further testing. Without the NMR, there would be no way to tell if she and Mishevich had successfully made the molecule.

Now that Mishevich can use the NMR to immediately determine whether she has correctly made the ligand, she can quickly adjust her calculations and accurately produce it in greater quantities.

Perpetual discovery

What Mishevich is doing now, many don’t get to do until graduate school. She is experiencing failures and altering her synthetic plan. For example, Mishevich could not identify why her reaction was not working at first, and could not isolate her product. With the NMR, she was able to identify that the reaction was not finished. With a little more heat, time and a catalyst, she completed the reaction and was ready to move on to the next step in the process.

“Now,” Mishevich said, “we are trying to identify the structural and chemical changes that occur when cuprizone binds to vitamin B6. We have been attempting to grow crystals of the complex but with the NMR we can attack it from a new angle and run several experiments to elucidate the new structure.”

This structure, once identified, will enable Walker’s research to move one step closer to understanding the mechanism associated with cuprizone toxicity and demyelination. Such a discovery could contribute to breakthroughs in treating multiple sclerosis, an unpredicatable, often disabling autoimmune disorder of the central nervous system.

At IU Northwest, this unique opportunity to work with the NMR, though atypical for most undergraduates in general, is not reserved for ambitious research assistants like Mishevich. The university’s new NMR is already being integrated into advanced chemistry lab courses and undergraduate research this semester so that all chemistry students will get this experience—one that is part of an education endorsed by the American Chemical Society.

Taschner explained that the NMR helps students learn in ways that aren’t always accessible. It helps them brave unknown territory, and experience failures that are common in scientific discovery, and alter their plan.

“If something is off by just a fraction of a percent,” explains Taschner, “the reaction may not work and form something completely different. It’s good to put students in those scenarios.”

Freedom to research

Taschner is using the NMR to analyze the formation of a cyclic peptide used to reduce tumor growth. When produced naturally, it only occurs in small amounts. However, using organic synthetic chemistry, ample quantities can be prepared and studied.

“My goal is to eventually make this compound,” Taschner explained, “and we are very close, but the only way I can tell I made it, is to have a ‘picture’ of the molecule. I need the NMR to prove to the scientific community that I produced it in the lab.”

Once Taschner achieves this, he can produce quantities large enough for researchers to do effective studies on how it inhibits tumor growth. He hopes this research will one day contribute to a breakthrough in cancer and tumor treatment.

Having a 400MHz NMR onsite will enable Taschner to have more freedom with his experimentation and arrive at his desired results much faster. 

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