Participants/Project Abstracts
Summer 2007 Bioanalytical Science REU Participants
DEVELOPMENT OF CITP-NMR: ANALYSIS OF TRACE COMPOUNDS
Layne Higgins, Stacie Eldridge, Albert Korir, and Cynthia Larive
Department of Chemistry, University of California-Riverside, UCR 92521 and California State University San Bernardino, San Bernardino, CA, 92407
Abstract
This
research focuses on the development and application of capillary
isotachophoresis coupled with NMR detection (cITP-NMR) for the analysis of
trace and mass-limited samples. Microcoil NMR is used as the method of detection and provides greater
mass sensitivity. Trace impurity
analysis in the presence of a large excess of parent compound is an analytical
challenge in pharmaceutical applications. cITP-NMR can selectively concentrate and detect charged impurities and
prove to be an effective method in overcoming this challenge. The cosmetic preservatives, parabens
will serve as a model for developing and testing cITP-NMR for this application. The charged compound 4-hydroxybenzoic
acid, at a concentration of 300 μM, is focused and detected by
cITP-NMR. Then 4-hydroxybenzoic
acid is tested in the presence of methyl paraben at a concentration of 1.0 mM
and no focusing was detected. Further optimization of the parabens experimental procedure is required
to achieve adequate separation. For mass-limited samples, 4 μg of porcine heparin oligosaccharides,
produced by enzymatic depolymerization, were analyzed by cITP-NMR. The compounds IS and IIS were
concentrated and detected by cITP-NMR, proving it’s effectiveness as applied to
mass-limited samples.
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