title: 1H NMR characterization of the product from single solid-phase resin beads using capillary NMR flow probes.
abstract: A capillary NMR flow probe was designed to generate high-resolution (1)H NMR spectra at 600 MHz from the cleaved product of individual 160-microm Tentagel combinatorial chemistry beads. By injecting a dissolved sample sandwiched between an immiscible, perfluorinated organic liquid directly into the probe, NMR spectra of the product cleaved from single beads were acquired in just 1 h of spectrometer time without diffusional dilution. Sample handling efficiency on the single bead scale was comparable to that obtained with a bulk sample. Using the relative intensity of the DMSO-d(5)H versus the analyte signals in a fully relaxed CPMG spectrum, the amount of product cleaved from a single bead was determined to be 540+/-170 pmol in one of the samples. Following the NMR data collection, the samples were examined with electrospray ionization mass spectrometry to provide additional structural information. By coupling with microliter-volume fluidic capabilities, the capillary flow probe described here will enable multidimensional characterization of single solid-phase resin products in an online manner.
authors.affiliation: Department of Chemistry and Beckman Institute, University of Illinois, Urbana, Illinois 61801, USA.
authors.forename: M E
authors.initials: ME
authors.lastname: Lacey
authors.forename: J V
authors.initials: JV
authors.lastname: Sweedler
authors.forename: C K
authors.initials: CK
authors.lastname: Larive
authors.forename: A J
authors.initials: AJ
authors.lastname: Pipe
authors.forename: R D
authors.initials: RD
authors.lastname: Farrant