SMRL: Stanford NMR Facility and Resource


Emerging Technology and Applications:
NMR Micro-Flow Probes in Studies of Proteins,
Metabolites, and Natural Products

9:30-11:45 a.m., May 6, 2003
M112 Medical School Building (Alway Building) [
Stanford University School of Medicine

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9:30-9:50 a.m. Refreshments
9:50-10 a.m. Welcome: Prof. Joseph Puglisi - Director, SMRL
10-10:45 a.m. Dean Olson, Ph.D - MRM Corporation [Bio]
Capillary NMR: Capabilities and Applications of the Microflow Approach [Abstract]
10:45-11 a.m. Intermission and Refreshments
11-11:45 a.m. Mark O'Neil Johnson - Sequoia Sciences [Bio]
Can I Get a Structure on 50 Micrograms? Proteins, Metabolites and Natural Products Using a CapNMR Probe [Abstract]
11:45 a.m. Conclusion

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Dean Olson - MRM Corporation, Saoy, IL

Capillary NMR: Capabilities and Applications of the Microflow Approach

CapNMR Probe. A new, capillary-based probe offers a unique approach to performing high-sensitivity NMR spectroscopy. The flow cell of the CapNMR probe has a volume of just 5 microL, and the entire probe has an inlet-to-outlet volume of only 10 microL. Mass sensitivity is about 10 times more than a conventional-scale 5 mm tube probe, and nearly the same as NMR cryoprobes. A typical figure of merit is that an injection of 1 nmol of sample dissolved in 3 microL of solvent yields a high-resolution, stopped-flow, proton spectrum in about 10 minutes on a 500 MHz spectrometer, with a S/N greater than 10. For a compound of 500 MW, this is 0.5 microg of sample at 0.33 mM. Capillary fluidic design throughout greatly reduces the rate of deuterated solvent consumption and expense.

Sample Injection Options. Manual sample injection is performed with a hand-held syringe connected directly to the probe. Assisted flow injection is performed by loading a valve-mounted sample loop with a hand-held syringe followed by delivery to the NMR flow cell by a micropump. Automated flow injection consists of the Gilson Micro 215, which loads the sample loop of the micropump.

Capillary LC-NMR. The CapLC offers non-split flow, three-channel programmable solvent gradients, a very sensitive, photo-diode array UV-Vis detector, and peak-parking and resume-flow capability for seamless interruption of separation runs, including during solvent gradients. Sample loading volumes for the CapLC are as low at 0.2 microL and total sample volumes as low as 1 microL.

Mark O'Neil Johnson - Sequoia Sciences, San Diego, CA

Can I Get a Structure on 50 Micrograms? Proteins, Metabolites and Natural Products Using a CapNMR Probe

From structural biology and proteomics to metabolite identification and natural products discovery, the amounts of material necessary to do structure elucidation has always been the slow process in moving research forward. With NMR being a pivotal tool in this process, substantial amounts of material are necessary relative to other analytical techniques.

Recent technological advancements in NMR has alleviated some of these problems. With the introduction of very high field NMR spectrometers and the increased sensitivity from cryoprobe technology along with new NMR acquisition techniques, the needs for larger quantities of small molecules or proteins has not been less of a problem. Only a limited budget has been the limiting factor. The latest introduction of the CapNMR(tm) probe technology has made another significant reduction in the necessary quantities of sample needed and softened the budgetary impact.

With the CapNMR(tm) probe, scientists can now very easily acquire complete NMR data sets on as little as 50 micrograms of small molecule unknowns and routine proton spectra on 5 micrograms or less. Preliminary results on proteins has also shown that with less than 10 micrograms of material one can acquire fabulous data. Without the need for NMR tubes and requiring minimal solvent consumption, the CapNMR(tm) probe will pave the way for the future of NMR sample submission and data acquisition.

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Dean Olson - Dean Olson completed a Ph.D. in analytical chemistry from the University of Illinois in 1994. He then joined the academic research group of Professor Jonathan Sweedler performing the first high-resolution NMR studies with nanoliter-volume microcoils. .He also did the first experiments using high-resolution NMR as a detector for capillary electrophoresis and mass-limited samples. He is now employed at MRM Corporation conducting research toward the commercial development and applications of capillary-based NMR probes.

Mark O'Neil-Johnson - Mark O'Neil-Johnson has twenty years experience in the field of NMR and application development of NMR to chemical characterization. Mark started as a natural products chemist performing total synthesis of natural products under John McMurry at UC Santa Cruz. He started his industrial work at IBM Research doing synthetic chemistry at the IBM San Jose site. Mark joined IBM Instruments in its inception, starting up the San Jose NMR Demo Lab under the direction of Charles Wade. IBM Instruments left the instruments business in 1987 and Mark joined Bruker, setting up the NMR Demo Lab in the San Jose area. While at Bruker, Mark has performed NMR demonstrations at 300, 400 and 500 MHz, on-site user training at over 250 customer sites, conducted in-house NMR training courses, development and demonstrations of flow NMR and LC-NMR-MS capabilities and NMR applications development with scientific collaborators.

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This symposium is made possible in part through the generous sponsorship of Protasis Corporation, and by funding through the SMRL Industrial Affiliate Program provided by Varian, Incorporated.

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Please contact:

Manolia Margaris
SMRL Administrative Associate

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2002 Stanford University, All Rights Reserved.
Last Modified: Apr 9 02:51:10 2003