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Updated: Aug 11, 2026

Phase Diagram Characterization Using Magnetic Beads as Liquid Carriers
Published on: September 4, 2015
1H NMR characterization of the product from single solid-phase resin beads using capillary NMR flow probes
M E Lacey1, J V Sweedler, C K Larive
1Department of Chemistry and Beckman Institute, University of Illinois, Urbana, Illinois 61801, USA.
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.
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