The combination of NMR and a separation method provide unmatched structural elucidation capabilities, based primarily on the wealth of chemical information that NMR provides. Unfortunately NMR is an inherently insensitive technique and thus requires large sample masses. The overall goal of this proposal is to improve the mass sensitivity of NMR by two orders of magnitude so that 5-500 nL volumes and picomole masses can be analyzed. The advance that enable such sensitivity improvements is development of miniaturized radiofrequency coils for signal detection in NMR. As the coil diameter is reduced in size it provides much higher signal-to-noise ratios for a given mass of sample. A major portion of this work is the optimization of coil fabrication and design geometry. The nanoliter volume NMR detector cells will be coupled to microseparations. Specifically, optimized flow cells, acquisition parameters, separation modes and preconcentration methods will be developed for capillary electrophoresis and capillary liquid chromatography. In addition to hardware development this proposal seeks to employ to nanoliter NMR method to study the mass limited, but high concentration environment of the interior of a series of peptide containing vesicles from the marine mollusk, Aplysia californica.

Agency
National Institute of Health (NIH)
Institute
National Institute of General Medical Sciences (NIGMS)
Type
Research Project (R01)
Project #
3R01GM053030-03S1
Application #
6133275
Study Section
Metallobiochemistry Study Section (BMT)
Project Start
1996-06-01
Project End
2000-04-30
Budget Start
1999-06-01
Budget End
2000-04-30
Support Year
3
Fiscal Year
1999
Total Cost
Indirect Cost
Name
University of Illinois Urbana-Champaign
Department
Chemistry
Type
Schools of Arts and Sciences
DUNS #
041544081
City
Champaign
State
IL
Country
United States
Zip Code
61820
Sutton, Bradley P; Ciobanu, Luisa; Zhang, Xiaozhong et al. (2005) Parallel imaging for NMR microscopy at 14.1 Tesla. Magn Reson Med 54:9-13
Wang, Han; Ciobanu, Luisa; Webb, Andrew (2005) Reduced data acquisition time in multi-dimensional NMR spectroscopy using multiple-coil probes. J Magn Reson 173:134-9
Wolters, Andrew M; Jayawickrama, Dimuthu A; Sweedler, Jonathan V (2005) Comparative analysis of a neurotoxin from Calliostoma canaliculatum by on-line capillary isotachophoresis/1H NMR and diffusion 1H NMR. J Nat Prod 68:162-7
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Ciobanu, Luisa; Webb, Andrew G; Pennington, Charles H (2004) Signal enhancement by diffusion: experimental observation of the ""DESIRE"" effect. J Magn Reson 170:252-6
Jayawickrama, Dimuthu A; Wolters, Andrew M; Sweedler, Jonathan V (2003) Mobile phase compensation to improve NMR spectral properties during solvent gradients. Analyst 128:421-6
Li, Yu; Lacey, Michael E; Sweedler, Jonathan V et al. (2003) Spectral restoration from low signal-to-noise, distorted NMR signals: application to hyphenated capillary electrophoresis-NMR. J Magn Reson 162:133-40
Kakuta, Masaya; Jayawickrama, Dimuthu A; Wolters, Andrew M et al. (2003) Micromixer-based time-resolved NMR: applications to ubiquitin protein conformation. Anal Chem 75:956-60
Wolters, Andrew M; Jayawickrama, Dimuthu A; Larive, Cynthia K et al. (2002) Insights into the cITP process using on-line NMR spectroscopy. Anal Chem 74:4191-7
Lacey, Michael E; Webb, Andrew G; Sweedler, Jonathan V (2002) On-line temperature monitoring in a capillary electrochromatography frit using microcoil NMR. Anal Chem 74:4583-7

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