This webpage contains all the information, presentations and other useful materials pertaining to the NMR workshop organized at the American Society of Pharmacognosy ASP2017 meeting in Portland, Oregon. The workshop will be dedicated to understanding the principle of quantitative NMR (qNMR), and discovering its multiple applications in different research settings (Academia, Industry, and Government). Attendees will have the great opportunity to network with our invited speakers Dr. Art Edison (University of Georgia), Dr. Joe Ray (Baxter), and Dr. Charlotte Corbett (DEA). There will be plenty of time for questions and discussions (see schedule here)…. don’t be shy!
Dr. Joe Ray received his BS in Chemistry from Loyola University of Maryland in 1964, his PhD from Carnegie-Melon University in organic chemistry in 1968, and, after a post-doctoral position at The Ohio State University, joined Amoco the NMR lab in 1970. After 29 years and many name changes, when Amoco became British Petroleum, Joe took early retirement in 1999. In 2000, Joe joined the NMR group at Baxter Healthcare where he is currently the Senior Subject Matter Expert in the NMR lab. During his career, Joe has used multinuclear, multidimensional, high-resolution, and solid-state NMR to characterize petroleum, polymers, catalyst, other organics and, most recently, biologically important systems. Emphasis was on the quantitative and qualitative analysis of gases, liquids and solids. Both 1D and 2D techniques have been developed and used to solve structure - property relationships for diverse business groups.
Presentation: NMR at Baxter: Quantitative Applications to Products at Different Stages of their Life Cycle. There are many phases in the life cycle of a given product in industry, and NMR has applications in all of them. This presentation will discuss the Exploratory phase of the cycle by showing how NMR was used to assess and select a polysaccharide from various algae candidates for use as an procoagulant. The Process Development phase of the cycle will be discussed using an example of a polysaccharide that was designed to attach to a drug to extend the life of a Factor VIII drug used to treat deficiency in hemophiliacs. The Manufacturing phase will be illustrated by showing how NMR determines Total Organic Carbon using 1H NMR data. Finally, for the Post-Manufacturing phase we will show how NMR determined the source and identity of an adulterant intentionally added to a Baxter product.☝︎
see also anecdotal qNMR
Dr. Charlotte Corbett has worked as a forensic drug chemist for 15 years. She has specialized in nuclear magnetic resonance (NMR) for the past five years. The Drug Enforcement Administration (DEA) utilizes NMR for purity determination, structure differentiation, identification, and structure elucidation. DEA continues to simplify quantitation through automation. New compounds are identified on a weekly basis. DEA also strives to assist forensic laboratories with new technology, such as low resolution NMR, comparison spectra, and expert analysis.
Presentation: qHNMR at the DEA. Quantitation at the Drug Enforcement Administration informs intelligence as well as criminal sentencingProton NMR is one of many quantitation methods; however, NMR provides some key advantages, such as not requiring a known purity of the analyte of interest and simple method validation. Almost all samples are mixtures, and current processing requires at least one signal region to be free of interferences, so some mixtures are not amenable to qHNMR. Peak height quantitation can be used to corroborate integral results.☝︎
Dr. Art Edison completed his Ph.D. in biophysics from the University of Wisconsin-Madison, where he developed and applied NMR methods for protein structural studies under the supervision of John Markley and Frank Weinhold. He joined the faculty at the University of Florida in 1996, where he became a full professor and Co-PI of the National High Magnetic Field Laboratory. In 2013, he was the founding PI and Director of the NIH-funded (U24) Southeast Center for Integrated Metabolomics (SECIM), one of 6 NIH metabolomics centers. He moved to the University of Georgia as a Professor and GRA Eminent Scholar in NMR Spectroscopy in 2015.
Presentation: The Power of Statistical Correlation Spectroscopy. Because NMR is quantitative, it is possible to obtain a great deal of information through statistical correlations. Statistical Total Correlation Spectroscopy (STOCSY) was first introduced by the Nicholson laboratory as a tool in complex mixtures to group resonances in 1D 1H NMR data that are in the same molecule.1 Essentially the same approach can be applied to integrating 1D 1H NMR data with other datasets, such as mass spectrometry (Statistical Heterospectroscopy—SHY2) or 13C NMR.3 I will introduce STOCSY and show how it can be used in metabolomics and natural products applications.☝︎
☞ You can access Dr. Edison’s presentation here
References:  Cloarec, O., Dumas, M. E., Craig, A., Barton, R. H., Trygg, J., Hudson, J., Blancher, C., Gauguier, D., Lindon, J. C., Holmes, E., and Nicholson, J. (2005) Statistical total correlation spectroscopy: an exploratory approach for latent biomarker identification from metabolic 1H NMR data sets, Analytical Chemistry 77, 1282-1289.  Crockford, D. J., Holmes, E., Lindon, J. C., Plumb, R. S., Zirah, S., Bruce, S. J., Rainville, P., Stumpf, C. L., and Nicholson, J. K. (2006) Statistical heterospectroscopy, an approach to the integrated analysis of NMR and UPLC-MS data sets: Application in metabonomic toxicology studies, Analytical Chemistry 78, 363-371.  Clendinen, C. S., Lee-McMullen, B., Williams, C. M., Stupp, G. S., Vandenborne, K., Hahn, D. A., Walter, G. A., and Edison, A. S. (2014) 13-C NMR metabolomics: applications at natural abundance, Anal Chem 86, 9242-9250.
☞ See also Edison Lab
Workshop Group Photo
Prepared and presented by Drs. Guido Pauli & Charlotte Simmler. Send us an email at firstname.lastname@example.org for any comments you may have.
The raw NMR data and calculation spreadsheet presented herein are made freely available at doi:10.7910/DVN/UZM3NV(Harvard Dataverse).
Useful Links and Educative Websites
* Practical aspects of qNMR from Dr. Larive
* Parameters of NMR acquisition
* Instruction for purity determination from the Journal of Medicinal Chemisitry
* Ottawa University NMR blog
* Links from the University of California Davis
* MestReNova related blog
* Calibration of 90 degree pulse (Bruker)
* the qNMR webpage of Northwestern University where our review on the applications of qNMR for the analysis of complex natural products has been cited.