1 H 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

Fingerprint

beads
resins
solid phases
Resins
Nuclear magnetic resonance
nuclear magnetic resonance
Electrospray Ionization Mass Spectrometry
probes
products
Dimethyl Sulfoxide
Capillary flow
Electrospray ionization
Fluidics
capillary flow
organic liquids
Dilution
fluidics
Mass spectrometry
Spectrometers
dilution

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

Cite this

1 H NMR characterization of the product from single solid-phase resin beads using capillary NMR flow probes . / Lacey, Michael E.; Sweedler, Jonathan V; Larive, Cynthia K.; Pipe, Adrian J.; Farrant, R. Duncan.

In: Journal of Magnetic Resonance, Vol. 153, No. 2, 01.01.2001, p. 215-222.

Research output: Contribution to journalArticle

Lacey, Michael E. ; Sweedler, Jonathan V ; Larive, Cynthia K. ; Pipe, Adrian J. ; Farrant, R. Duncan. / 1 H NMR characterization of the product from single solid-phase resin beads using capillary NMR flow probes In: Journal of Magnetic Resonance. 2001 ; Vol. 153, No. 2. pp. 215-222.
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