1H NMR characterization of the product from single solid-phase resin beads using capillary NMR flow probes

Michael E. Lacey, Jonathan V. Sweedler, Cynthia K. Larive, Adrian J. Pipe, R. Duncan Farrant

Research output: Contribution to journalArticle

Abstract

A capillary NMR flow probe was designed to generate high-resolution 1H NMR spectra at 600 MHz from the cleaved product of individual 160-μm 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-d5H 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.

Original languageEnglish (US)
Pages (from-to)215-222
Number of pages8
JournalJournal of Magnetic Resonance
Volume153
Issue number2
DOIs
StatePublished - Jan 1 2001

Keywords

  • Mass spectrometry
  • Microcoil
  • Nanoliter
  • Nuclear magnetic resonance
  • Tentagel beads

ASJC Scopus subject areas

  • Molecular Biology
  • Physical and Theoretical Chemistry
  • Spectroscopy
  • Radiology Nuclear Medicine and imaging
  • Condensed Matter Physics

Fingerprint Dive into the research topics of '<sup>1</sup>H NMR characterization of the product from single solid-phase resin beads using capillary NMR flow probes'. Together they form a unique fingerprint.

  • Cite this